MultiMode SPM

Instruction Manual
Version 4.31ce

Copyright 1996-99 Digital Instruments Veeco Metrology Group

All rights reserved.

Document Revision History: MultiMode SPM Instruction Manual

Revision

Date

Ref.
DCR

Section(s) Affected

4.31ce

27OCT97

Chapters 3, 5 and 8

168, 185,
189

4.22ce

14FEB97

TOC, TOW, Chapters 2, 5, 7, 11, 12, 13, 15 and

Index

139

4.22

15JUL96

Released

Approval

VERSION 4.31ce27OCT97

MultiMode SPM Instruction Manual

Table of Contents
Table of Warnings
Chapter 1

Introduction to the MultiMode SPM

Introduction 1-2
Microscope Specifications 1-4
Image size and resolution. 1-4
Scanning techniques with the MultiMode SPM. 1-5
Controller Electronics and Auxiliary Channels 1-6

Chapter 2

SPM Fundamentals for the MultiMode

Chapter Table of Contents 2-1
Hardware 2-2
MultiMode SPM 2-3
SPM Head 2-4
Scanners 2-5
Tipholders 2-9
Probes 2-10

Control Mechanisms and Feedback 2-13

A brief history of SPM control mechanisms. 2-13

Feedback Gains 2-15

Proportional and Integral GainAn Analogy 2-15
Proportional Gain 2-16
Integral Gain 2-18
LookAhead Gain 2-19
Completing the AnalogyFeedback Gains in SPM 2-19
Setpoint 2-19
The SPM Electronic Feedback Loop 2-20
More about Feedback and Images 2-21
What Data Type of image? 2-24

MultiModeSPM Instruction Manual

Chapter 2 Cont...

Control Parameters and Feedback 2-26

Reexamining the Control Loop 2-26
General Description of Main Menu Items 2-26
User Example 2-28
Review of General Operating Concepts 2-28

Review of TappingMode AFM 2-32

General Operating Concepts 2-32
Optimizing the TappingMode AFM signal after engagement. 2-34

Terms and Abbreviations 2-35

Chapter 3

Setup & Installation

Installing the MultiMode SPM 3-1
Component List 3-1
Component List (cont.) 3-2
Unpack The System 3-3
Vibration isolation 3-8
System Power Up & DOS Start-Up 3-9

Chapter 4

Cantilever Preparation for the MultiMode SPM

Silicon Cantilever Substrates 4-1
Tip Shape of Etched Silicon Probes 4-2

Silicon Nitride Cantilever Substrates 4-8

Tip Shape of Silicon Nitride Probes 4-10

Chapter 5

Head, Probe and Sample Preparation

Preparing to Image with the MultiMode SPM 5-1
Initial Preparation for Contact AFM Imaging 5-2
Prepare the sample. 5-2
Load the sample. 5-4
Load a probe into the tipholder. 5-6
Install the tipholder. 5-9

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Chapter 5 Cont...

Laser Alignment 5-10

Method 1: the magnifier method 5-10
Method 2: The "paper" method 5-13
Maximize the SUM Signal 5-21

Start the Microscope Program 5-22

MultiMode SPM Voltage Meters 5-23

Chapter 6

Contact AFM
Introduction to Contact AFM 6-1
Preparation Prior to Imaging 6-1
Adjust the Detector Offsets 6-1
Signal settings 6-3
Adjust tip height above sample surface 6-4

Suggested Initial Control Settings 6-4

Initial Settings: Scan, Feedback and Other Controls panels 6-4
Other Controls Panel 6-5
Interleave Controls panel 6-5
Channel 1, 2 and 3 6-6

Initiate the Engage Command 6-6

Adjust Setpoint with Force Calibration 6-7
Adjust Sensitivity (if required). 6-10

Beyond the Basics of AFM Operation 6-11

Cantilever selection 6-11

Optimization of Scanning Parameters 6-12

Data type 6-13
Gain settings 6-13
Scan size and Scan rate 6-14
Setpoint 6-14
Lowpass filter 6-15
Highpass filter 6-15

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iii

Chapter 7

Contact AFM in Fluids

Fluid OperationOverview
Fluid OperationHardware
Notes on Sample Mounting
Fluid OperationProcedure

7-1
7-2
7-3
7-5

Load the Fluid Tipholder with a Cantilever Substrate 7-5

Install the Tipholder on the Microscope Head 7-5
Align the laser 7-6
Watch Out for False Reflections 7-6
Align the Laser on the Cantilever 7-7
Install the Protective O-ring and Flood the Fluid Chamber 7-7
Lower Tipholder into Fluid 7-7
Readjust Laser Aiming (If Required) 7-7
Adjust the Detector Offsets and Setpoint 7-7
Check Scan Parameters 7-8
Engage the Surface 7-8
Adjust Scan Parameters 7-8
Clean and Dry Parts When Done 7-9

Chapter 8

TappingMode AFM
Introduction to TappingMode AFM 8-1
Basic Principle of TappingMode 8-1
Preparation Prior to Imaging 8-3
Switch to TappingMode and check parameters 8-3
Adjust laser and photodetector 8-4
Additional preparations 8-7
Tune the cantilever 8-8
Setting the Drive amplitude and Setpoint 8-11

Engaging The Microscope 8-13

Withdrawing the Tip 8-15
Beyond Basics with Resonating Techniques 8-15
Subtleties of Cantilever Oscillation 8-15
Tuning the cantilever Drive frequency 8-18
Optimization of scanning parameters 8-18

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Chapter 8 Cont...

Force Calibration (Z Scan Controls) Mode 8-21

The Force Calibration plot 8-22
The Force Calibration control paneladditional features 8-23
Examples of amplitude calibration plots 8-25

TappingMode in FluidsIntroduction 8-26

Acknowledgments 8-26
Overview 8-26
Fluid cell preparation 8-27
TappingMode operation in fluid. 8-31
Troubleshooting tips. 8-35
Model sample preparations. 8-37

Lysozyme on micaA model procedure for protein binding 8-38

Dissolve protein. 8-39
Prepare fluid cell. 8-39
Prepare mica. 8-39
Deposit protein solution on mica. 8-40
Allow protein to bind to substrate. 8-40
Rinse unbound proteins from fluid cell. 8-40
Assemble fluid cell. 8-40
Clamp fluid drain line. 8-40

Binding DNA to Mica 8-41

Dilute DNA in buffer 8-42
Deposit drop on freshly cleaved mica. 8-42
Rinse unbound DNA if desired. 8-42
Vacuum dry sample. 8-42
Prepare AFM and fluid cell 8-43
Fill fluid cell with buffer. 8-43
Acknowledgments 8-43

Troubleshooting Tips 8-43

Cantilever Tune plot looks badloose fluid cell or tip 8-43
8O-ring slides across sample surface, causing drift 8-43
Laser Sum Signal absent or weakair bubbles 8-44
Poor image qualitycontaminated tip 8-44
Unable to locate particulate samplesattraction to cantilever 8-44

MultiModeSPM Instruction Manual

Chapter 9

Scanning Tunneling Microscopy (STM)

Introduction 9-1
Overview of STM 9-2
STM hardware 9-3
Fine points of STM operation 9-4

Basic STM Operation 9-9

Imaging samples 9-9

Spectroscopy with the STM 9-13

STS plot modes 9-13
Operation of STS 9-14
Continuous Imaging Tunneling Spectroscopy (CITS) 9-15

Obtaining Images with STM 9-15

Imaging highly ordered pyrolytic graphite (HOPG) 9-16
Imaging a gold calibration ruling. 9-21

Troubleshooting for STM 9-23

9.5.1. Head and microscope-related problems 9-23
9.5.2. Head engages immediately 9-23
Tip never engages 9-24
Tip crashes 9-24
Problems during Real Time operation 9-25
Image goes out of range 9-26
Z drift 9-26
Real Time image hides features 9-27
Image is streaky or wavy 9-27
Image is triangular over step-like features 9-27
Image goes white ("A" scanners) 9-28

Etching Tungsten Tips 9-28

Procedure 9-29

Chapter 10

Lateral Force Mode

Introduction 10-1
LFM Mode in More Detail 10-2
Optimal Setup for Frictional Measurements 10-2
Determination of friction 10-3
Identification of Forces other than Friction 10-5
Example of frictional data 10-6

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Chapter 11

Force Imaging
Introduction 11-1
Plotting Force in Contact AFM 11-1
The Force Curve and Piezo Extension-Retraction Cycle 11-4

Contact AFM Force Plots 11-5

Contact AFM Force Plots 11-7
Sensitivity Determination 11-9
Force Minimization 11-10
Calculating Contact Force 11-11
Interpreting Force Curves 11-13

Force Imaging in TappingMode 11-13

Force Plots 11-14
Obtaining a Force Plot of a Calibration Reference in TappingMode 11-16
Very High Contact Force 11-18
Triggering 11-20

Force Plot Control Panels 11-21

Force Plot Control Panel Parameters 11-22

Imaging Local Elasticity with Force Modulation 11-25

Introduction 11-25
Selecting a Force Modulation Tip 11-27
Force modulationOperating Principle 11-28
Force modulationProcedure 11-29

Force Modulation with Negative LiftMode 11-39

Find Resonance of the Bimorph 11-39
Set Interleave Controls 11-40
Obtain a TappingMode Image 11-40
Obtain a Negative LiftMode Force Modulation Image 11-40
Final Comments 11-41

Force Volume Imaging 11-42

Description 11-42
Setting Up for Force Volume 11-43
Obtaining Force Volume Images Using Contact AFM 11-44

MultiModeSPM Instruction Manual

vii

Chapter 12

Interleave Scanning and LiftMode

Preface: Interleave Scanning & LiftMode 12-1
Interleave Mode Description 12-2
Lift Mode Description 12-3
Operation of Interleave Scanning / Lift Mode 12-4
Use of LiftMode with TappingMode 12-5
Main Drive Amplitude and Frequency selection 12-5
Setpoint Selection 12-5
Interleave Drive Amplitude and Frequency Selection 12-6
Amplitude Data Interpretation 12-7
Cantilever Oscillation Amplitude 12-7

Chapter 13

Magnetic Force (MFM) Imaging

Magnetic Force Imaging Overview 13-1
MFM Using Interleave Scanning and LiftMode 13-3
Procedure 13-4
Frequency modulation. 13-8

Troubleshooting Suggestions 13-9

MFM image verification. 13-9
Saturation in amplitude detection 13-9
Optical interference. 13-9

Advanced Topics 13-10

Lift scan height and magnetic imaging resolution. 13-10
Fine Tuning Interleave Controls 13-11

Installation of Extender Electronics Module 13-13

Setting the Extender Electronics for Dimension or MultiMode 13-14
Microscope parameter files. 13-14
Important points. 13-16

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MultiModeSPM Instruction Manual

Chapter 14

Electric Force (EFM) Imaging

Chapter Table of Contents 14-1
Electric Force Microscopy Overview 14-2
Electric field gradient imaging overview. 14-3
Surface Potential Imaging Overview 14-4

Electric Field Gradient DetectionTheory 14-4

Electric Field Gradient DetectionPreparation 14-7
Jumper configurations for systems without the Extender Electronics Module 14-9
Jumper Configurations For Microscopes With the Extender Electronics Module 14-14

Electric Field Gradient DetectionProcedures 14-19

Amplitude Detection 14-23

Surface Potential DetectionTheory 14-25

Surface Potential DetectionPreparation 14-27
Applying Voltage to the Sample Directly 14-28
Applying Voltage to the Sample Through Piezo Cap 14-29

Surface Potential ImagingProcedure

14-30

Troubleshooting the surface potential feedback loop. 14-34

Chapter 15

Calibration Procedures, Troubleshooting and Maintenance

SPM Calibration TheoryOverview 15-1
Theory behind calibration 15-2

Sensitivity and Scanner Calibration

Background Information 15-4
Calibration References 15-6
Linearity Correction Procedure 15-7
Check scanner parameter values 15-7
Align calibration reference 15-7
Set Real Time parameters 15-8
Set up SPM for contact AFM. 15-8
Check sample orthogonality. 15-8
Adjust sample orthogonality. 15-9
Adjust mag0 and arg0 15-9

X-Y Calibration using Capture Calibration 15-13

Off-line / Utility / Autocalibration 15-16

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ix

Chapter 15 Cont...

Fine-tuning for X-Y Measuring Accuracy 15-18

Prepare system for fine-tuning. 15-18
Measure horizontally at 440 V scan size. 15-19
Measure vertically at 440 V scan size 15-20
Measure horizontally at 150 V scan size 15-21
Measure vertically at 150 V scan size 15-22
Change Scan angle and repeat calibration routines 15-23

Fine-tuning for Z Measuring Accuracy 15-23

Engage surface and begin imaging 15-23
Adjust Scan size 15-24
Capture and correct an image 15-24
Measure vertical features 15-26
Correct Z sensitivity 15-28
Recheck Z-axis measuring accuracy and correct 15-28
Calculate Retracted and Extended offset deratings 15-29

Calibration of A Scanners for Atomic-scale Measurement 15-30

Prepare sample. 15-30

Troubleshooting the MultiMode SPM 15-33

Contact AFM: False engagement 15-33
Contact AFM: Head appears engaged but does not track surface features 15-34
Contact AFM: Head does not engage 15-35
Contact AFM: Head engages immediately 15-35
Contact AFM: Displacement of material 15-35
Contact AFM: Lines in the image 15-36
Contact AFM: Problems with silicon nitride cantilevers 15-36
Contact AFM: Image vertical dimensions are not correct 15-37
Contact AFM: Z Center Position goes out of range 15-37
Contact AFM: Poor image quality 15-38
Contact AFM: Force Calibration command does not seem to work 15-39
Contact AFM: Image vertical dimensions are not correct 15-39
Contact AFM: Z Center Position goes out of range 15-39
Contact AFM: Image goes white 15-39
TappingMode: Streaks on the trailing edge of surface features 15-40
TappingMode: Lines across the image 15-40
TappingMode: Rings around features on the surface. 15-41
TappingMode: Multiple or repeating patterns 15-41
TappingMode: Image goes white or black 15-41
Fluid Imaging: Image drifts. 15-41

MultiModeSPM Instruction Manual

Chapter 15 Cont...

MultiMode SPM Adjustment Screw Maintenance Procedure 15-43

Inspection 15-43
Remove adjustment screws. 15-44
Inspect for physical damage. 15-45
Clean guide bushings. 15-45
Lubricate. 15-46
Reinstall. 15-46

Index

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MultiMode SPM Instruction Manual

Table of Warnings

CAUTION: Some early-model AFM tipholders may short out power supplies when used with
MM-SPMs. If you suspect your tipholder is from an older AFM, check with Digital
Instruments or your international representative before using.
2-9
ATTENTION: Certains modles de support de bras de leviers pour AFM de contact peuvent
endommager les alimentations lectriques quand ils sont utiliss avec un MultiMode (MMSPMs). En cas de doute, contacter Digital Instruments ou son reprsentant lgal pour verification.
2-9
WARNHINWEIS: Einige ltere Ausfhrungen des AFM-Spitzenhalters knnen einen
Kurzschlu verursachen falls sie mit einem MultiMode-AFM verwendet
werden. Bitte wenden Sie sich im Zweifelsfall an Digital Instruments bzw. an die fr Sie
zustndige DI-Vertretung.
2-9
WARNING! During and prior to set up of the laser, it is especially important to avoid looking
directly at the laser beam or at the laser spot. The laser head should never be plugged into the
microscope control electronics unless the head is installed in the Z-stage mount. Care should
be taken when highly reflective samples are inserted onto the chuck. Avoid looking at all
reflected laser light. Operators should use care to avoid staring into beams that may be
reflected from sample surfaces.
5-2

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ATTENTION! Avant dutiliser le laser, et durant tout le temps pendant lequel il

fonctionne, il est impratif de ne pas regarder directement le faisceau. La sonde laser
ne doit jamais tre branche sur llectronique de contrle du microscope, tant que la
tte de mesure nest pas installe dans son support. Il est impratif de faire trs
attention lorsque des chantillons trs rflchissants sont dposs sur la platine. Eviter
toute exposition la lumire laser. Durant lutilisation, ne pas fixer les faisceaux laser
rflchis par les surfaces dchantillons.
5-2
WARNUNG! Es ist sehr wichtig, vor und whrend der Laserjustierung nicht in den
Laserstrahl oder auf den Laserpunkt zu schauen. Der Laser sollte niemals an die
Mikroskopelektronik angeschlossen werden, wenn er nicht in der Halterung der ZVerschiebeeinheit installiert ist. Seien Sie bitte sehr vorsichtig, wenn stark
reflektierende Proben auf dem Probenteller liegen. Vermeiden Sie unter allen
Umstnden, in das reflektierte Laserlicht zu schauen. Alle Bediener des Mikroskops
sollten grte Vorsicht walten lassen um zu vermeiden, in den von der
Probenoberflche reflektierten Laserstrahl zu schauen.
5-2
WARNING! Staring at a bright beam or reflection can result in eye damage. Be sure
that you are using a magnifier with a laser filter installed.
5-10
AVERTISSEMENT! Fixer un faisceau lumineux puissant ou sa rflexion peuvent
entrainer des dommages au niveau des yeux. Il est impratif dutiliser un filtre laser.
5-10
WARNUNG! Der direkte Blick in den Laserstrahl oder dessen Reflektion kann
Augenschdigungen hervorrufen. Bitte stellen Sie auf jeden Fall sicher, da ein
optisches Gert, mit dem Sie in den Laserstrahl schauen, mit einem Laserschutzfilter
ausgestattet ist.
5-10
WARNING! To avoid eye damage due to high-level laser light, do not place highly
reflective or metallized objects into the head area while the laser is on.
5-13
AVERTISSEMENT! Pour prvenir tout accident au niveau des yeux, d la lumire
du laser, il est recommand de ne pas placer dobjet trs rflchissant ou mtallique
sous le faisceau laser lorsque celui-ci est allum.
5-13

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WARNUNG! Um Augenschdigungen aufgrund von Laserlicht zu vermeiden achten

Sie bitte darauf, da keine reflektierenden oder mit Metall beschichteten Gegenstnde
im Bereich des AFM-Kopfes benutzt werden, solange der Laser eingeschaltet ist. 5-13
CAUTION! When imaging fluid samples, use extraordinary precautions against
spillage. Fluids must NOT be spilled on or around the sample stage, electronic boxes,
or other components containing electronic parts. Avoid spilling all corrosive fluids on
exposed surfaces; otherwise, damage may result! In the case of a spill, immediately
clean and dry all affected surfaces carefully.
7-1
ATTENTION! En milieu liquide, prendre toutes les prcautions pour viter une fuite
qui pourrait atteindre la platine porte -chantillon, le boitier lectronique ou tout autre
partie lectronique du microscope. Eviter tout contact avec un liquide corrosif. 7-1
WARHINWEISS! Falls Sie Proben in Flssigkeiten abbilden, lassen Sie uerste
Vorsicht walten, damit keine Flssigkeit verspritzt wird. Flssigkeiten drfen nicht auf
die oder nahe der Probenhalterung, der Elektronikbox oder anderen Komponenten, die
elektronische Bauteile enthalten, verspritzt werden. Vermeiden Sie bitte, korrosive
Flssigkeiten auf freiliegende Oberflchen zu verspritzen; andernfalls wren
Beschdigungen die Folge! Falls Sie Flssigkeit verspritzt haben, subern und
trocknen Sie alle betroffenen Flchen sorgfltig.
7-1
IMPORTANT: Do not attempt to operate the standard air tipholder in a fluid
environment. Standard tipholders have exposed electrical signal lines that could short
circuit if exposed to a conducting fluid.
7-2
ATTENTION: En milieu liquide, ne pas utiliser le support de bras de levier standard
prvu pour une utilisation lair. Le support de bras de levier standard comporte des
fils lectroniques non protgs qui peuvent provoquer un court-circuit en cas de
contact avec un liquide conducteur.
7-2
WARNHINWEISS: Versuchen Sie nicht, den Standard-Luft-Cantileverhalter in
Flssigkeiten zu betreiben. Am Standard-Cantileverhalter liegen elektrische Leitungen
frei, die in leitfhigen Flssigkeiten kurzgeschlossen werden knnten.
7-2

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CAUTION! When imaging fluid samples, use extraordinary precautions against

spillage. Fluids must NOT be spilled on or around the sample stage, electronic boxes,
or other components containing electronic parts. Avoid spilling all corrosive fluids on
exposed surfaces; otherwise, damage may result! In the case of a spill, immediately
clean and dry all affected surfaces carefully.
7-4
ATTENTION! Lors dun travail en milieu liquide, prendre toute prcaution pour viter
des fuites. Les liquides ne doivent pas se rpandre sur la platine porte chantillons, le
botier lectronique ou toute autre partie du microscope contenant de llectronique.
Eviter toute fuite de liquide corrosif sur les surfaces exposes. Le non respect de cette
recommandation peut entraner des dommages. En cas de fuite, nettoyer et scher
immdiatement les surfaces touches.
7-4
WARHINWEISS! Falls Sie Proben in Flssigkeiten abbilden, lassen Sie uerste
Vorsicht walten, damit keine Flssigkeit verspritzt wird. Flssigkeiten drfen nicht auf
die oder nahe der Probenhalterung, der Elektronikbox oder anderen Komponenten, die
elektronische Bauteile enthalten, verspritzt werden. Vermeiden Sie bitte, korrosive
Flssigkeiten auf freiliegende Oberflchen zu verspritzen; andernfalls wren
Beschdigungen die Folge! Falls Sie Flssigkeit verspritzt haben, subern und
trocknen Sie alle betroffenen Flchen sorgfltig.
7-4
CAUTION! When imaging fluid samples, use extraordinary precautions against
spillage. Fluids must NOT be spilled on or around the sample stage, electronics boxes,
or other components containing electronic parts. Avoid spilling all corrosive fluids on
exposed surfaces; otherwise, damage may result! In the case of a spill, immediately
clean and dry all affected surfaces carefully
8-26
ATTENTION! Lors dun travail en milieu liquide, prendre toute prcaution pour viter
des fuites. Les liquides ne doivent pas se rpandre sur la platine porte chantillons, le
botier lectronique ou toute autre partie du microscope contenant de llectronique.
Eviter toute fuite de liquide corrosif sur les surfaces exposes. Le non respect de cette
recommandation peut entraner des dommages. En cas de fuite, nettoyer et scher
immdiatement les surfaces touches.
8-26
CAUTION! Do not add excessive amounts of fluid or the cell will overflow and
damage the piezo tube scanner.
8-29
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MultiModeSPM Instruction Manual

ATTENTION! N'ajoutez pas trop de fluide. Sinon, la cellule dbordera et

endommagera le scanner du tube piezo.

8-29

CAUTION! When imaging fluid samples, use extraordinary precautions against

spillage. Fluids must NOT be spilled on or around the sample stage, electronics boxes,
or other components containing electronic parts. Avoid spilling all corrosive fluids on
exposed surfaces; otherwise, damage may result! In the case of a spill, immediately
clean and dry all affected surfaces carefully.
8-29
ATTENTION! Lors dun travail en milieu liquide, prendre toute prcaution pour viter
des fuites. Les liquides ne doivent pas se rpandre sur la platine porte chantillons, le
botier lectronique ou toute autre partie du microscope contenant de llectronique.
Eviter toute fuite de liquide corrosif sur les surfaces exposes. Le non respect de cette
recommandation peut entraner des dommages. En cas de fuite, nettoyer et scher
immdiatement les surfaces touches.
8-29
WARHINWEISS! Falls Sie Proben in Flssigkeiten abbilden, lassen Sie uerste
Vorsicht walten, damit keine Flssigkeit verspritzt wird. Flssigkeiten drfen nicht auf
die oder nahe der Probenhalterung, der Elektronikbox oder anderen Komponenten, die
elektronische Bauteile enthalten, verspritzt werden. Vermeiden Sie bitte, korrosive
Flssigkeiten auf freiliegende Oberflchen zu verspritzen; andernfalls wren
Beschdigungen die Folge! Falls Sie Flssigkeit verspritzt haben, subern und
trocknen Sie alle betroffenen Flchen sorgfltig.
8-30
CAUTION: Because TappingMode cantilevers are relatively stiff, Force Mode can
potentially damage the tip and/or surface. DI recommends using Force Plot only with
extreme caution.
11-13
ATTENTION: Les bras de leviers pour TappingMode tant relativement rigides,
lutilisation du mode Force peut endommager la pointe ou lchantillon. Digital
Instruments recommande dutiliser le mode Force Plot avec une extrme prcaution.
11-13
WARNHINWEIS: Da TappingMode-Mespitzen relativ steif sind, kann im Force
Mode unter Umstnden die Mespitze oder die Oberflche beschdigt werden. DI
empfiehlt, den Force Plot nur unter grter Vorsicht anzuwenden.
11-13
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CAUTION: Because TappingMode cantilevers are relatively stiff, Force Mode can
potentially damage the tip and/or surface. DI recommends using Force Plot only with
extreme caution.
11-16
ATTENTION: Le pointes Tapping tant relativement raides, lutilisation du mode
Force peut endommager la pointe ou lchantillon. Digital Instruments recommande
dutiliser le mode Force Plot avec une extrme prcaution.
11-16
WARNHINWEIS: Da TappingMode-Mespitzen relativ steif sind, kann im Force
Mode unter Umstnden die Mespitze oder die Oberflche beschdigt werden. DI
empfiehlt, den Force Plot nur unter grter Vorsicht anzuwenden.
11-16
CAUTION: If employing stiffer cantilevers than those normally used, the sample may
be damaged by the cantilever tip. To minimize this damage, make the Setpoint as low
as possible.
11-34
ATTENTION! Lutilisation dun levier plus rigide que ceux utiliss habituellement
peut entraner un endommagement de lchantillon par la pointe. Afin de rduire les
risques dendommagement, ajuster la valeur cible du rtro-contrle (Setpoint) sa
valeur la plus faible possible.
11-35
WARNHINWEIS! Falls Sie mit Cantilevern hherer Federkonstanten arbeiten, als
normal blich, kann die Probe durch die Spitze beschdigt werden.. Um eine evtl.
Beschdigung zu minimieren bzw. zu vermeiden, benutzen Sie bitte einen
Arbeitspunkt (Setpoint), der nur geringfgig ber der freien Deflektion des Cantilevers
liegt. Die Differenz zwischen Setpoint im Feedback-Men und der freien Deflektion
des Cantilevers (Photodetektorsignal A-B) sollte minimal sein.
11-35
CAUTION: Before enabling the Interleave Drive Amplitude, check that its value is not
much larger than the main Drive Amplitude value to prevent possible damage to the tip.
12-6
ATTENTION: Lors dun travail en mode intercal (Interleave Mode), vrifier que la
tension applique pour osciller le bras de levier lorsquil est en positon haute nest pas
beaucoup plus importante que la tension applique lorsque ce mme bras de levier est
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MultiModeSPM Instruction Manual

en position basse (Main Drive Amplitude). Le non respect de cette procdure peut
entraner la destruction de la pointe.
12-6
WARNHINWEIS: Bevor Sie im Interleave-Mode die Interleave Drive-Amplitude
einschalten, vergewissern Sie sich bitte, da der dort eingetragene Wert nicht
wesentlich grer ist, als der Wert der Main Drive-Amplitude, um evtl.
Beschdigungen der Spitze vorzubeugen.
12-6
CAUTION: Before enabling the Interleave Drive Amplitude, check that its value is
not much larger than the main Drive Amplitude value to prevent possible damage to
the tip.
13-12
ATTENTION: Lors dun travail en mode intercal (Interleave Mode), vrifier que la
valeur de tension applique loscillateur pizo-lectrique est infrieure celle
applique loscillateur en mode imagerie (Main Drive Amplitude). Le non respect
de cette procdure peut entraner la destruction de la pointe.
13-12
WARNHINWEIS: Bevor Sie im Interleave-Mode die Interleave Drive-Amplitude
einschalten, vergewissern Sie sich bitte, da der dort eingetragene Wert nicht
wesentlich grer ist, als der Wert der Main Drive-Amplitude, um evtl.
Beschdigungen der Spitze vorzubeugen.
13-12
WARNING: Do not insert a conducting object (e.g., screwdriver) into the Phase
Extender box while it is engergized.
13-14
ATTENTION: Ne pas insrer d objet conducteur (par exemple: un tournevis) dans le
botier dextension de phase (Phase Box) quand celui-ci est sous tension.
13-14
WARNUNG: Stecken Sie keine leitfhigen Teile (zum Beispiel Schraubenzieher) in
die Phase Extender Box, whrend diese eingeschaltet ist.
13-14
CAUTION: When closing the System.par file after viewing it, if you are asked to
SAVE the file or to SAVE CHANGES, be sure to say No.
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ATTENTION: Si vous avez besoin de consulter le fichier "System.par," sa fermeture

lorsque lordinateur demande SAUVEGARDER (SAVE) ou SAUVEGARDER LES
CHANGEMENTS (SAVE CHANGES), rpondre toujours NON.
13-15
WARNHINWEIS: Falls Sie sich mit einem Editor die Datei system.par anschauen
und beim Verlassen des Editors gefragt werden, ob Sie die Datei speichern (SAVE)
bzw. die nderungen speichern wollen (SAVE CHANGES), antworten Sie bitte mit
Nein (No).
13-15
CAUTION! Do NOT splash solvent on the scanner tube or wiring at the center of the
scanner bodycertain components (e.g., wiring insulation) may be dissolved, causing
scanner failure!
15-45
ATTENTION! Ne pas clabousser le tube en cramique pizo-lectrique ou le
montage lintrieur du tube avec un solvant. Certains composants pourraient tre
dissous, entranant une dfaillance du tube.
15-45
WARHINWEIS! Verwenden Sie keine Lsungsmittel auf dem Scanner-Rhrchen oder
den Kabelanschlssen am Piezo - manche Komponenten (z.B. Isolation der
Anschludrhte)knntensichauflsenundeineFehlfunktiondesScannersnachsichziehen.
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Introduction to the MultiMode SPM

Control monitor

Display monitor

Computer

NanoScope Controller

Mouse
Keyboard

MultiMode SPM

Figure 1.1. MultiModeSPM system components.

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Part I: Introduction

1.1. Introduction
The MultiMode scanning probe microscope (MM-SPM) is one of Digital Instruments original, mainstay designs and remains a highly dependable unit; several
hundred MultiModes have been shipped to laboratories and businesses worldwide.
The unit is designed for imaging small (approx. 1.5 cm dia.) samples using a series
of interchangeable scanners and is able to provide images from the atomic scale to
175 m in size. This manual is designed to assist operators with using the MMSPM and has been rewritten from earlier editions. The reader is also referred to the
Command Reference Manual.
The MM-SPM is designed around a stationary probe. That is, samples are scanned
back and forth beneath the probe. (This is opposite to other of Digital Instruments
designse.g., Dimension Series SPMswhich mount samples stationary while
scanning the probe back and forth above them.) Typically, samples are fixed to
round 1.5 cm metal disks (pucks), then magnetically attached to the top of the
scanner tube. As the scanner moves back and forth, the sample moves with it,
allowing the probe to extract information from the sample surface much like a phonograph needle plays a vinyl record.
Because the size of features imaged with SPM is often below the visible wavelength of light, all information gathered from sample surfaces is electronically
derived and rendered. Electronic controls have evolved through the years from an
early array of switches and knobs to the present software control system, designated NanoScope, version 4.x. Digital Instruments has divided its SPM software
into a two-function architecture: Real Time and Off-line. The Real Time software
functions are dedicated to running the actual microscope, changing the size and
location of scans, controlling gains, etc. Images produced from scans may be analyzed and/or modified using the microscopes Off-line functions. These yield sectional profiles, correct for noise and artifacts, analyze for depth, roughness, grain
size and power spectral density, among many other things. One major advantage to
the NanoScope design is that both modes may be run simultaneously. That is, the
microscope can save (capture) images in Real Time mode while the operator is
busy analyzing earlier images in the Off-line mode, making the MM-SPM a maximum-productivity tool.

How does it work?

This manual is designed to assist users of the MM-SPM in obtaining microscopic
images by leading them through the most basic steps. No previous knowledge is
assumed, and the reader is encouraged to forge ahead, even when full understanding of the microscopes workings may seem out of reach. Initially, the microscope
may be treated as a black box by following instructions in this manual; however,

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Introduction to the MultiMode SPM

a deeper understanding of how SPM works will prove invaluable to the operator.
Our advice: experiment! Consult the Command Reference Manual for more information regarding software controls.

Six Rules of Safety

Here is a summary of precautions to follow during your learning phase. If you follow the six rules below, the MM-SPM can come to little harm and you may feel free
to experiment boldly.

1. Read the manuals!

Even if you have prior experience with the MM-SPM, be sure to read chapters
1-5 in this manual before doing any imaging work. Each of the remaining chapters are dedicated to specific types of imaging. Chapter 6 provides an introduction to contact AFM, which is a good place for beginners to start. Other chapters
may be read as required. Also consult the Command Reference Manual for a
complete explanation of software controls.

2. Follow good rules of engagement.

Engagement refers to the process of bringing the tip and surface together. This
is harder than it sounds, and the software routine for controlling the process is
complex. Some probes (especially crystal silicon TappingMode probes) are
prone to breakage if engaged too quickly or too hard. Ensure that engagement
settings never exceed the limits of safety (see Chapter 5) and never attempt to
engage manually using coarse adjustment screws.

3. Never move the head while imaging.

The head contains the tipholder, laser and photodiode array. An X-Y translation
stage is provided for moving the head and tip several millimeters across the
sample for coarse adjustment. Even for relatively smooth samples, the head
should NEVER be moved with the tip engaged. This almost always results in tip
breakage. Always disengage first before using the X-Y stage to move the tip.

4. Never leave your controller ON while the computer is turned OFF.

Operators are advised to turn OFF their controller and computer when finished
with imaging. If the controller is left ON for an extended period without an
energized computer, damage to the scanner may result. (This is especially true if
the scan has been heavily offset in X and Y.)

5. Do not unplug cables to/from energized hardware. Turn OFF first.

Unplugging energized hardware is not recommended and may result in damage
to the MM-SPM. Always turn OFF hardware before making connections.

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6. Check all connections before hardwiring external equipment.

External equipment which is hardwired into the MM-SPM, such as for EFM
and ECSTM imaging, requires special cautions. To prevent damage to your
microscope, always check connections carefully against documentation before
energizing the system. For more information, see Support Note 210.
The first step to gaining a working knowledge of your microscope is to learn about
its various parts and what they do. Chapter 2 provides a quick tour of the MM-SPM
hardware and principles of operation.

1.2. Microscope Specifications

The MultiMode SPM, proven in over 500 installations, is the highest resolving
SPM in the world. The microscope can be fitted with any of several scanners,
depending upon the imaging requirements. Generally, the smaller the scan, the
smaller the scanner used. This is especially true of atomic-scale scans, which are
most often conducted with A or E scanners. Larger scans are normally performed using J scanners. Following is a list of basic specifications:

1.2.1. Image size and resolution.

Images consist of raster-scanned, electronic renderings of sample surfaces. There
are three default sizes: 128 x 128 pixels, 256 x 256 pixels, and 512 x 512 pixels. In
addition, six width-to-height aspect ratios may be specified by the user: 1:1, 2:1,
4:1, 8:1, 16:1, and 32:1. Thus, it is possible to obtain strip scans which require
less time to capture.
The controller provides 16-bit resolution on all three axes, with three independent
16-bit digital-to-analog converters (DACs) in X and Y for control of the scan pattern, scaling and offset. This configuration provides 16-bit resolution of the lateral
scanning motion at any scan size, and the ability to perform atomic resolution
imaging throughout the full lateral range of the scanner. The patented digital feedback is governed by integral and proportional gain controls, providing immediate
response to scanning parameter changes.
The MultiMode can scan up to 200 m laterally (in X and Y) and 10 m vertically
(Z axis). A table summarizing each scanners capabilities is provided in Chapter 2.

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Introduction to the MultiMode SPM

1.2.2. Scanning techniques with the MultiMode SPM.

The MultiMode is so called because it offers multiple SPM modes, including AFM,
ECAFM, ECSTM, STM and TappingMode. While many early SPMs offered only
one dedicated operating mode (e.g., STM), the MultiMode was the worlds first
multiple-use SPM. It remains one of Digital Instruments most versatile instruments. A complete range of Atomic Force Microscopy (AFM) and Scanning Tunneling Microscopy (STM) techniques is available with the MultiMode SPM. Some
of these techniques are available only through Digital Instruments.

Contact AFM Measures topography by sliding the probes tip across the
sample surface. Operates in both air and fluids. See Chapter 6.

TappingMode AFM Measures topography by tapping the surface with an

oscillating tip. This eliminates shear forces which can damage soft samples and
reduce image resolution. TappingMode is available in air and fluids (patented).
This is now the technique of choice for most AFM work. See Chapter 8.

Phase Imaging Provides image contrast caused by differences in surface

adhesion and viscoelasticity. Requires an Extender Electronics Module
(patent pending). See Chapters 8 and 13.

Non-contact AFM Measures topography by sensing Van der Waals attractive

forces between the surface and the probe tip held above the surface. Provides
lower resolution than either contact AFM or TappingMode.

Magnetic Force Microscope (MFM) Measures magnetic force gradient

distribution above the sample surface. Performed using LiftMode to track
topography (Extender Electronics Module recommended). See Chapter 13.

Electric Force Microscope (EFM) Measures electric field gradient

distribution above sample surfaces. Performed using LiftMode to track
topography (Extender Electronics Module recommended). See Chapter 13.

Surface Potential Microscopy Measures differences in local surface

potential across the sample surface. Performed using LiftMode to track
topography (Extender Electronics Module only). See Chapter 13.

LiftMode A combined, two-pass technique that separately measures

topography (using TappingMode) and another selected property (e.g., magnetic
or electric force), using the topographical information to track the probe tip at a
constant height above the surface (patented). See Chapter 12.

Force Modulation Measures relative elasticity/stiffness of surface features

(patented). Force modulation is only one of several types of force imaging
which are possible. See Chapter 11.

Lateral Force Microscopy (LFM) Measures frictional forces between the

probe tip and sample surface. See Chapter 10.

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Scanning Tunneling Microscopy (STM) Measures topography of surface

electronic states using a tunneling current which is dependent on the separation
between the probe tip and a conductive sample surface. An optional LowCurrent STM Converter allows operation in the subpicoamp tunneling current
region which can be useful when scanning poorly conductive samples.
Tunneling spectroscopy may also be performed. See Chapter 9.

Electrochemical Microscopy (ECSTM and ECAFM) Measures the surface

structure and properties of conducting materials immersed in electrolyte
solutions with or without potential control. See ECSTM/ECAFM manuals.

Lithography Use of a probe tip to mechanically scribe or indent a sample

surface. May be used to generate patterns, test surfaces for microhardness, etc.
Performed using AFM and STM. See the Command Reference Manual and
Support Note 225.
Most of these imaging techniques are discussed in this manual. If you do not find
sufficient information here, refer to Digital Instruments World Wide Web site (http:/
/www.di.com) to order the necessary support notes or obtain technical support.

1.2.3. Controller Electronics and Auxiliary Channels

The MultiMode utilizes a NanoScope IIIa Controller having a digital signal processor (DSP) with a 20 MHz peak rate for arithmetic operations. The MultiMode is
equipped with four auxiliary digital-to-analog converters (DACs). Three DACs
have 10 V outputs, and one DAC has a 12 V and 220 V outputs; all four channels have 16-bit resolution.
In addition, there are two 10 V analog-to-digital converters (ADCs) having 14-bit
resolution and software-selectable filters. One ADC has four-way mutliplexing.
All Digital Instruments SPMs may be attached to an optional Signal Access Module (SAM), which provides direct access (via BNC connectors) to all input and output signals between the controller and the microscope. Generally, the SAM is
useful for customized use or modification of the SPM.

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Chapter 2

SPM Fundamentals for the

MultiMode

Chapter Table of Contents

2.1.

2.2.
2.3.

2.4.

2.5.
2.6.

Hardware 2
2.1.1. MultiMode SPM 3
2.1.2. SPM Head 4
2.1.3. Scanners 5
2.1.4. Tipholders 9
2.1.5. Probes 9
Control Mechanisms and Feedback 12
2.2.1. A Brief History of SPM Control Mechanisms 12
Feedback Gains 15
2.3.1. Proportional and Integral GainAn Analogy 15
2.3.2. Proportional Gain 16
2.3.3. Integral Gain 18
2.3.4. LookAhead Gain 19
2.3.5. Completing the Analogy 19
2.3.6. Setpoint 20
2.3.7. The SPM Electronic Feedback Loop 20
2.3.8. More about Feedback and Images 21
2.3.9. What Data Type of Image? 24
Control Parameters and Feedback 26
2.4.1. Reexamining the Control Loop 26
2.4.2. General Description of Main Menu Items 26
2.4.3. User Example 28
2.4.4. Review of General Operating Concepts 28
Review of TappingMode AFM 32
2.5.1. General Operating Concepts 32
2.5.2. Optimizing the TappingMode AFM Signal After Engagement 34
Terms and Abbreviations 35

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Part I: Introduction

2.1. Hardware
This section provides a quick tour of the MultiMode SPM and its hardware. The
MultiMode SPM consists of seven major components: SPM, controller, computer,
keyboard, mouse, display monitor and control monitor. Mouse movements automatically transfer the cursor between monitors, enabling the operator to seamlessly
switch between control and display functions.
Control monitor

Display monitor

Mouse moves cursor

between monitors

Computer

Keyboard

Controller

Mouse

SPM

Figure 2.1. MultiMode SPM system hardware.

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2.1.1. MultiMode SPM

The heart of the system is the SPM itself, shown below in figure 2.2.
Photodiode
adjustment knob

Laser adjustment knobs

SPM tip
Head
Tipholder
X-Y head translator

Sample
Scanner
(Shown: A)

Retaining springs

Coarse adjustment
screws

Scanner support ring

Motor control
switch

Mode selector
switch

A-B
A+B
display
Base
(A+C)-(B+D)
A+B+C+D
display

Signal sum display

(elliptical)
Figure 2.2. MultiMode SPM.

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2.1.2. SPM Head

Figure 2.3 below shows a MM-SPM head with various adjustment knobs. The head
and attached X-Y stage are kinematically mated to the scanner via three contact
points. A pair of retaining springs hold down the head, allowing it to be raised and
lowered using adjustment screws threaded through the scanner body. On older
models, two screws are manually adjusted by the operator; the rearmost screw is
motorized and under computer control. Newer, vertical scanners use single-screw
adjustment.
Laser Y-axis adjust
Photodiode adjust
Laser X-axis adjust

Head X-axis stage adjust

Head Y-axis stage adjust

Figure 2.3. MultiMode SPM head and major components: laser (1);
mirror (2); cantilever (3); tilt mirror (4); photodetector (5).
Photodiode array The four elements of the quad photodiode (position sensitive
detector) are combined to provide different information depending on the operating
mode. In all modes the four elements combine to form the SUM signal. The amplified differential signal between the top two elements and the two bottom elements
provides a measure of the deflection of the cantilever. This differential signal is
used directly in the contact AFM. It is fed into an RMS converter (or phase module
if attached) for Tapping mode operation. Similarly, the amplified differential signal
between the sum of two left photodiodes and the sum of the two right photodiodes
provides a measure of the torsion in the cantilever and is used in Lateral Force
Microscopy (Image data type: Friction). Figure 2.4 shows the arrangement of the
photodiode elements in the MultiMode head.

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Laser
LFM

Photodetector segments

Photodetector

Mirror

AFM

Cantilever

Figure 2.4. Quad photodetector arrangement. Different segments of the

photodetector are used for generating AFM and LFM signals.

2.1.3. Scanners
Figure 2.5 below shows the various, interchangeable scanners. The maximum scan
size and resolution of images depend upon the choice of scanner (see chart). Longer
scanners, e.g., type J, yield larger scan sizes; shorter scanners, e.g., type A,
offer smaller images down to the atomic-scale. Smaller scanners tend to be more
noise-free at acoustic frequencies because of their compact size and rigidity. Larger
scanner offer wider scans, while requiring extra noise dampening precautions at
smaller scan sizes of high resolution.

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Figure 2.5. Various scanners available with the MultiMode SPM.

Left-to-right: AS-130V (vertical J); AS-200 (K); AS-130 (J);
AS-0.5 (A). Not shown: AS-12 (E) All scanners are interchangeable.
Because each scanner exhibits its own unique piezo properties, each has its own
parameter file. When scanners are changed, the parameter file for the new scanner is
changed along with it, ensuring maximum accuracy at any scan size. Loading new
parameter files requires only a few seconds. The chart below describes the range
capabilities of each MultiMode SPM scanner.

Model

Scan Size

Vertical Range

AS-0.5 (A)

0.4m x 0.4m

0.4m

AS-12 (E)

10m x 10m

2.5m

AS-12V (E vertical)

10m x 10m

2.5m

AS-130 (J)

125m x 125m

5.0m

AS-130V (J vertical)

125m x 125m

5.0m

AS-200

200m x 200m

8.0m

Figure 2.6 depicts the electrode configuration used on one type of scanner piezo
tube. Electrodes are oriented as shown when the MultiMode is viewed from the
front. With the Scan angle parameter in the control panel set to 0.00, the fast-scan
direction is in the direction of the X-axis.

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~
Z

~
Y
Y

~
X

Figure 2.6. Typical scanner piezo tube and X-Y-Z electrical configurations.
AC signals applied to conductive areas of the tube create
piezo movement along the three major axes.
AC voltages applied to the scanner crystals X-Y axes produce a raster-type scan
motion as represented in figure 2.7. The horizontal axis presented on the display
monitor is referred to as the fast axis (in this example, the X-axis) and scans at a
Scan rate entered by the user. The orthogonal axis is known as the slow axis (in
this example, the Y-axis).

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Figure 2.7. Voltages applied to the X- and Y-axes produce a raster scan
pattern. Either axis may be designated as the fast axis.

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SPM Fundamentals for the MultiMode

2.1.4. Tipholders
The sample and mode of SPM to be performed dictate the choice of tip and
tipholder. For example, if contact AFM is to be used for imaging, a silicon nitride
cantilever mounted in a standard tipholder is the usual choice. If TappingMode is to
be used for imaging a biological specimen in fluid, a special fluid cell is employed.
STM utilizes a special tipholder, having a tiny tube holder adapted for holding wire
tips. Examples of each tipholder are shown below in figure 2.8.
Top view

Bottom view
Figure 2.8. Various tipholders utilized with the MultiMode SPM.Left-toright: contact AFM and TappingMode; EFM; force modulation;STM.

Notes

STM tipholder shown now superceded by model MMSTMC.

CAUTION: Some early-model AFM tipholders may short out power supplies
when used with MM-SPMs. If you suspect your tipholder is from an older AFM,
check with Digital Instruments or your international representative before using.
ATTENTION: Certains modles de support de bras de leviers pour AFM de contact peuvent endommager les alimentations lectriques quand ils sont utiliss avec
un MultiMode (MM-SPMs). En cas de doute, contacter Digital Instruments ou son
reprsentant lgal pour verification.
WARNHINWEIS: Einige ltere Ausfhrungen des AFM-Spitzenhalters knnen
einen Kurzschlu verursachen falls sie mit einem MultiMode-AFM verwendet
werden. Bitte wenden Sie sich im Zweifelsfall an Digital Instruments bzw. an die
fr Sie zustndige DI-Vertretung.
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2.1.5. Probes
Probes come in a variety of sizes, shapes and materials and are chosen according to
the type of imaging to be done.

Wire Probes
STM probes usually consist of wire, cut and/or etched to produce atomically sharp
tips at one end. Usually these are made from tungsten or platinum-iridium alloy
wires. A potential is established so that electrons flow between the tip and sample.
A similar type of wire probe is used for lithography. These often consist of ordinary
tungsten STM tips and/or a wire with a tiny diamond fixed to its end. Lithography
tips are used for mechanically deforming sample surfaces in the form of controlled
dents and scratches. Essentially, the tip serves as a scribe or punch. It may be used
to test surfaces for microhardness, etch patterns or explore material characteristics.

Figure 2.9. Diamond tip mounted on wire for

microhardness testing and lithography work.

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Cantilevered Probes
Most SPM work is done using cantilevered probes. These consist of a flexible cantilever extending from a rigid substrate, to which a tip has been attached. In contact
AFM, the cantilevers flexibility acts as a nanometric spring, allowing the tip to
measure surface forces. In TappingMode, the probe is oscillated up and down at its
resonant frequency while its amplitude and phase are monitored.

Figure 2.10. Two types of cantilevered probes: silicon nitride (left), and
crystal silicon (right).

Cantilevered Probessilicon nitride

Most contact AFM is conducted with silicon nitride tips. These tips exhibit excellent flexibility, making them easier to use and more forgiving than stiffer crystal
silicon cantilevers. They are offered in a variety of sizes and coatings, allowing the
user to match them to the sample being imaged. One characteristic of silicon nitride
tips is that they are easily captured by the samples surface tension (capillary) properties; that is, trapped within a microscopic layer of condensed atmospheric water
vapor on the sample surface. This surface tension effect exerts considerable force at
the probes atomically sharp tip. Although this may prove unproblematic on harder
samples, it is frequently enough to deform softer samples. Adjustment to the SPMs
Setpoint parameter can offset much of this force; however, it may still prove troublesome on delicate samples. Silicon nitride tips may also be operated in TappingMode, although they are not optimal for this purpose.

Cantilevered ProbesTappingMode
Digital Instruments answer to minimizing contact AFM forces is TappingMode, a
proprietary form of AFM. In this instance, a stiff crystal silicon probe is oscillated
to its resonant frequency. Because the tip describes a high-frequency (e.g., 100-plus
KHz), oscillating arc, it possesses sufficient energy to break free of surface tension

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forces. The probe is considerably stiffer than silicon nitride, making it more brittle
and less forgiving. Thus, the operator must be more cautious while setting up the tip
and sample.

Cantilevered ProbesMFM
Another variation of the TappingMode tip is the MFM probe. This is basically a
crystal silicon TappingMode probe having a magnetic coating on the tip. (Such tips
are sold by Digital Instruments under the name NanoProbe.) As the magnetized
tip oscillates through magnetic fields on the sample surface, it modulates the cantilevers phase and frequency. These are monitored, providing a measure of magnetic
field strength and providing images of magnetic domains.

Cantilevered ProbesEFM
Similar to MFM (see above), EFM is also conducted using NanoProbe tips. Tips
may be electrically connected to the microscopes circuitry to obtain surface potential maps of the surface, or oscillated while monitoring phase changes due to electrostatic forces. These techniques yield images of the samples electrical domains.

Notes

Both MFM and EFM may be conducted using the MM-SPM alone; however,
best results are obtained with an Extender Electronics Module attached. For
more information regarding this attachment, contact Digital Instruments.

Specialized Probes
As the field of SPM continues its explosive growth, new probes are constantly
introduced. Here are a few examples of specialized probes:

Scanning capacitance microscopy (SCM) Tip acts as an RF antennae to

image microcapacitance phenomena. MFM tips may be used for SCM.

Chemical doped tips Tips doped with a chemical species of interest to the
investigator. The chemically doped tip measures chemical bonding forces on
sample surface, images receptor sites on biological membranes, etc.

Thermal imaging Tip incorporates a tiny thermocouple to image heat.

Focused ion beam (FIB) TappingMode tips up to 6 m in length cut from
crystaline silicon with a focused ion beam. Improved aspect ratio gives them
improved angular resolution on steep side walls.

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2.2. Control Mechanisms and Feedback

To produce quality images, the SPM must be capable of controlling the tip-sample
interaction with great precision. This is accomplished with the use of an electronic
feedback loop, which safeguards the tip and sample by keeping forces between
them at a user-specified Setpoint level. Although signal processing varies according to the image mode used, the feedback loop performs essentially the same function.

2.2.1. A brief history of SPM control mechanisms.

The first SPMs were scanning tunneling microscopes (STMs), which use tunneling
current to monitor tip-sample separation. By monitoring the flow of electrons from
tip to sample (or vice versa), the tips height above the surface can be precisely
maintained. The tip-sample separation is typically maintained at several atomic
diameters, or about 10 angstroms. As tip-sample separation decreases and increases
due to feature height, the tunneling current increases and decreases respectively,
obeying an exponential relationship.
A diagram portraying the tunneling effect during STM is shown in figure 2.11. In
this example, electron activity describes a zone several angstroms wide. Because
electrons flow exponentially across the gap, depending upon tip-sample separation,
dramatic differences in current are shown as the tip-sample distance is varied
slightly. This monitoring mechanism remains the most sensitive used in SPM,
achieving greater resolution than any other method.

Tip
Tunneling electrons

Surface

Figure 2.11. Tunneling phenomenon between tip and sample.

Electron flow varies exponentially with tip-sample distance.
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STMs biggest difficulty is that it requires electrically conductive samples. Soon

after its introduction, a method was sought which would allow non-conducting
samples to be imaged. Efforts lead to the first contact AFMs, which continued using
tunneling current as the monitoring mechanism. Figure 2.12 portrays an early contact AFM scheme. In this scheme, a contact probe was scanned over the surface. As
the tip encountered features, it moved up and down. Positioned directly above the
surface of the contacting probes cantilever was an STM probe. Fluctuations in current between the STM tip and contact probe were used as the feedback mechanism
and to render an electronic image. The main disadvantage of this method was difficulty in aligning the contacting tips cantilever and the STM tip directly above it.

STM tip

Flexible cantilever

Sample
AFM tip
Figure 2.12. Early contact AFM which allowed imaging non-conductive
samples. In this scheme, a contact AFM tip was monitored
using the STM tip directly above it.
Preceding the first SPMs, some profilometers had relied upon optical methods to
monitor the rise and fall of a sharp stylus over sample surfaces. This approach
offered good sensitivity by reflecting a laser beam off the end of the stylus and into
a photodetector to obtain an optical lever capable of detecting even the smallest

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movements (figure 2.13). This approach was then applied to SPMs. A related
method utilized interference to detect shifts in interference fringes.
Laser
Photodetector

Cantilever and tip

Scanner

Figure 2.13. Optical lever for monitoring tip movement.

Laser beam movement is monitored over two axes: vertically and horizontally. As
the tip traces various surface features, its upward and downward movement shifts
the beam between upper and lower photodiode components, creating voltage differences which are electronically rendered into height information. Lateral movements
of the beam are also monitored, corresponding to frictional phenomena on the surface.

2.3. Feedback Gains

The feedback system used to control tip-sample interactions and render images
must be optimized for each new sample. This is accomplished by adjusting various
gains in the SPMs feedback circuit. This section discusses gains and how they are
used to obtain images.

2.3.1. Proportional and Integral GainAn Analogy

To better understand gains and how they control SPM probes, consider the analogy
of a hot air balloon carrying three balloonists. Each rider controls a separate valve
on the balloons gas burner. The valves are mounted in parallel, such that if any one
valve is open, gas flows to the burners, causing the balloon to rise. Similarly, each
balloonist may turn their burner off to reduce altitude. Mounted beneath the balloons gondola is a camera, which automatically takes a photograph of the ground
below. The balloons objective is to obtain detailed photographs of the surface. To

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obtain the highest resolution images, the balloon must track the surface as closely
as possible without crashing into it. This poses a dilemma to the balloonists: how to
tightly control the balloons position relative to the ground.

setpoint altitude
100 meters

Because the balloon will drift slightly up and down due to the effects of wind and
temperature, the balloonists must establish some minimum altitude as a safety zone.
Let us call this the setpoint altitude, and let us assume that it is set at an altitude of
100 meters.1
When the terrain is flat, the problem is simplified. The balloonists need only ensure
a constant supply of gas is supplied to the balloons burners to keep the balloon
aloft. As the terrain becomes hilly, the task becomes more complex. If the terrain
rises, the balloonists must respond by firing the burners to lift the balloon. As the
balloon clears the hill and terrain drops away, the balloonists must turn the burners
off to reduce height and continue tracking the terrain. The type and intensity of the
balloonists responses to terrain can be modeled in terms of three types of feedback:
proportional, integral and LookAhead.

2.3.2. Proportional Gain

Proportional gain means that something is done proportionally in response to
something else. In the case of our first balloonist, Peter, this means producing hot
air in proportion to the balloons altitude above the terrain: where the terrain rises

1. For the sake of simplicity, setpoint in this analogy applies to the balloons altitude;
however, setpoint in SPM is applied to tip-sample forces, not the tips height above the
surface.

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sharply, Peter uses large amounts of gas to lift the balloon; where the terrain is relatively flat, Peter supplies a small, steady amount of gas to maintain the setpoint altitude above the surface.

If altitude > 100 meters,

turn burners off.

range finder
If altitude < 100 meters,
fire burners.

A simple feedback loop emerges in this analogy: let us say Peter uses a range finder
every 30 seconds to determine the distance between the balloon and ground. If the
balloon is below its setpoint altitude, he fires the burners. If the balloon is above its
setpoint altitude, he turns off the burners to lower the balloon. The higher the proportional gain, the more Peter reacts to changes in altitude. For example, at a proportional gain of 1, if the balloon is 25 meters too low, he opens his valve at 10
liters per second; if the balloon is 50 meters too low, he opens his valve at 20 liters
per second. The proportional gain value serves as a multiplier such that at a proportional gain of 2, the gas flow rates are doubled from a proportional gain of 1, and so
on. Although this sort of feedback gain works well for simple, linear models, it does
not function as well for nonlinear models. There remains always some residual
error which causes the system to approach, but not quite reach, the target state.
Assuming that the balloonists wants to get as close as possible without crashing, the
response will depend upon, among other things, the balloons speed over the terrain. When the balloon is being carried swiftly, it is necessary to apply feedback
earlier to compensate. (That is, more gas must be used earlier.) On the other hand, if
there is little or no wind, the balloon may achieve a closer tracking of the terrain.
There may also be sufficient knowledge of the terrain to anticipate its rises and
falls. In order to compensate for these effects, integral and LookAhead gain feedbacks may also be employed. These are discussed next.

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2.3.3. Integral Gain

Integral gain is used to correct the cumulative error between a system and its target
state. In the case of the balloon, it is not enough to use only proportional gain. As
we have seen, the balloon will maintain a constant error around the setpoint altitude
if it relies on proportional gain alone. It is also necessary to consider whether the
total error between the balloons actual altitude and its setpoint altitude is increasing or decreasing over some interval of time. To correct for cumulative error, our
second balloonist, Irene, utilizes integral gain.
Let us assume that Peter announces the balloons altitude every 30 seconds from his
range finder. Irene uses a stopwatch and clipboard to record the amount of error at
each measuring interval, averaging the error over a preceding interval of time (e.g.,
3 minutes). Irene fires the burners based upon her observations: if she notices that
the running average error puts the balloon below the setpoint altitude, she fires the
balloons burners, if she notices that the average error puts the balloon above the
setpoint, she turns the burners off. The effect of integral gain feedback is to reduce
total error by addressing error over a longer period of time. This tends to smooth
out the short-term, fluctuating effects of proportional gain while narrowing the error
closer to the setpoint value. Unfortunately, if the integral gain is set too high, there
is a tendency to overshoot the setpoint. Therefore, integral gain is highly sensitive
and must be used carefully.

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2.3.4. LookAhead Gain

Finally, the third balloonist, Larry, employs yet another type of gain to ensure optimal tracking over the terrain: LookAhead gain. For our example, Larry uses a map
to anticipate the rise and fall of the terrain. When his map indicates a mountain, he
opens his valve to fire the burners and lift the balloon. When a valley is indicated on
the map, he turns his burner off to lower the balloon. The effect of LookAhead gain
is to keep the balloon within the proper altitude zone so that proportional and integral gains will perform better by maintaining the balloon closer to its proper setpoint altitude. When the terrain is comprised of regular rises and falls, the
LookAhead balloonist is at his best, easily anticipating rises and falls. In these
instances, LookAhead gain can be maximized. Conversely, when the terrain is
rough and broken, the LookAhead balloonist must struggle with the balloons sluggish response to anticipate every irregular rise and fall, and may actually make control of the balloon more difficult. In these instances, LookAhead gain should be
minimized or turned off.

2.3.5. Completing the AnalogyFeedback Gains in SPM

Feedback gains used to control an SPMs probe tip are not far removed from those
controlling a hot air balloon. In the case of a probe tip, the objective is quite similar:
the operator assigns a setpoint value corresponding to a certain amount of tip-sample force, then adjusts gains to track the surface as closely as possible while maintaining the setpoint. Instead of gas-fired burners, however, the Z-axis piezo crystal
uses voltage to retract and lower the probe. In addition, such parameters as Scan
rate must be figured in. Just as a balloonist would find it difficult to closely track
rough terrain in a fast-moving balloon, the microscopist must frequently adjust
Scan rate and Setpoint to track samples successfully.

2.3.6. Setpoint
In our ballooning example, setpoint referred to the target altitude to be maintained. In scanning probe microscopy, setpoint refers to how much tip-sample
force is maintained. There are two ways of defining setpoint, depending upon
whether one is referring to contact AFM or TappingMode. In contact AFM, setpoint
is determined by the amount of cantilever flexionas the setpoint increases, the
cantilever flexes more and tip-sample forces increase. In TappingMode, setpoint is
determined by the RMS amplitude of the oscillating tipas setpoint decreases,
RMS amplitude decreases, but tip-sample forces increase1.

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2.3.7. The SPM Electronic Feedback Loop

Just as the balloonists in the example above want to get close to the ground without
crashing into it, the SPM is designed to tightly control the tips position relative to
the sample surface. In the case of contact AFM, this usually means applying a very
light force to the tipjust enough to trace surface features, but not so much force
that the tip is broken off or the surface damaged. In the case of TappingMode, it
means holding the tapping force (measured in terms of the oscillating probes
amplitude) to the setpoint level.
In the earliest SPMs (which were scanning tunneling microscopes), the tip was
scanned at a constant height above a very flat sample surface (e.g., cleaved graphite) while the tips current was monitored. Because tunneling current flows exponentially as a function of tip-sample distance, the image was rendered from mapped
current values at X-Y coordinates. This gave a height rendering of features based
upon current flow. As long as the sample was atomically flat, the tip could be
scanned safely above it and an image produced. Unfortunately, this arrangement
did not work well for rougher surfaces: the tip would crash into raised features,
damaging itself and/or the surface.
The next generation of SPMs added a Z-axis piezo crystal to the arrangement and
used a feedback loop to profile the samples features. Now, instead of using tipsample current flow to produce an image directly, the current was used instead as
the feedback signal to activate the Z-axis piezo. This allowed the tip to be lifted and
lowered, keeping tip height constant over surface features and accommodating
rougher samples. But how were images produced? Instead of using the tip-sample
current directly to render an image, the feedback loop was monitored indirectly.
This process allowed the feedback loop to protect the tip and sample while giving
quality images. In addition, the feedback circuit could be monitored at various
points to access new types of information about the tip-sample interaction.
As SPM evolved beyond its scanning tunneling roots, the feedback circuit was
modified to accommodate new types of imaging. The first major change arrived
with contact AFM, which permitted non-conducting surfaces to be imaged. Tunneling current was now used indirectly to monitor a cantilevered tip as it profiled sam-

1. At first glance, this may seem counterintuitive. However, recall that an oscillating tip in
TappingMode attains its fullest amplitude when it is in free air and not interacting with a
sample. As the oscillating tip is brought against the sample, its RMS amplitude decreases
due to damping effects. The harder the tip is pressed into the sample, the more RMS
oscillation is reduced. Thus, requesting a Setpoint of 0.00 in TappingMode commands
the system to press the tip against the sample so hard that the cantilever cannot oscillate at
all. In TappingMode, reducing setpoint increases tip-sample forces...the opposite of contact AFM.

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ples. Although this method allowed imaging of non-conducting samples, it was

unreliable due to adjustment difficulties with the STM probe and cantilever flexion.
The next great leap in SPM design which presaged the present state of the art was
the introduction of light beam deflection. In one design, a laser is employed to configure a light lever similar to those used with surface profilometers in industry. As
the tip encounters surface features it flexes, causing the incident laser beam to move
across a photodiode detector. Another design relies upon interferometric measurements; however, this design has been superceded by the light levers simpler, more
reliable design.
As new modes of SPM have been added to the field, the analysis of feedback signals has evolved to keep up with changes. The next section discusses how signals
are actually processed inside the NanoScope to render images.

2.3.8. More about Feedback and Images

Digital Instruments unique digital signal feedback architecture is described in
numerous patents filed with the US Patent Office. In summary, the basic feedback
processes may be broken down as follows:
LookAhead gain
In the example above, having a record of previous flights over terrain enabled three
balloonists to better anticipate the rises and falls of the terrain below them. Similarly, the feedback controller relies upon data from the previous (immediately adjacent) scan line to anticipate local features. It is easier to image samples which
contain regular, periodic features (e.g., gratings) since scan lines change relatively
little from scan-to-scan. Consider, for example, scan lines tracing the surface of a
penny.

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Although this scan is much larger than normally found in SPM, it illustrates how an
adjacent, lagging scan line can be used to determine local scan lines on regular surfaces. In most places (e.g., the forehead), each scan line changes little from the line
next to it. In some local areas (such as under the nose) there are small, sudden
changes; however, these are relatively isolated. In contrast, a similar trace of an
irregular, random surface would reveal that each scan line bears little resemblance
to its adjacent line.
The entire purpose of LookAhead gain is to take full advantage of regular features
by using every line to anticipate the next one. In NanoScope software, the LookAhead gain value may be adjusted between a range of 0 (off) to 16 (maximum). As
values are adjusted upward from 0, the LookAhead gain is weighted to apply more
data from the adjacent (lagging) line. Although LookAhead gain is relatively useless for random surfaces, it is a tremendous help on regular surfaces.
When LookAhead gain is switched on ( > 0), it is the first gain calculated in the
feedback process and is used to weight the integral gain as follows:
LA

G int

= z x + ( z (x), (y-1) z ( x+1 ),(y-1) )G LA

LA

That is, the LookAhead-weighted integral gain, G int , is calculated by subtracting

the adjacent pixels Z-axis value from the one immediately next to it, then multiplying this difference by the LookAhead gain value1 and summing the product with
the current data value. A diagram of the affected pixels appears as shown here:
z(x),(y-1)
z(x+1),(y-1)
Previous scan line
Direction of scan

zx

Local scan line

Next scan line

At start-up, there is no information yet recorded from an adjacent scan line; therefore, the LookAhead gain is effectively 0 until three lines have been scanned. This
allows the system to settle down and record data.
Integral gain and average error

1. Although the LookAhead gain value can be set by the operator to values between 0 and
16, these are not the values plugged into the equation. This is a digital signal feedback
process and the actual value multiplied varies between 0 and 224. A similar rule holds also
for both Integral and Proportional gain.

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The second step in the feedback process uses integral gain to correct for error by
averaging (integrating) the total error. In the ballooning example, Irene kept a running average of the balloons altitude error, then responded by firing the burners or
turning them off to bring the balloon closer to the setpoint altitude. Similarly, the
SPMs feedback process maintains a running average of the error and responds to it.
As we have seen, enabling the LookAhead gain by setting it > 0 conditions the
Integral gain entered by the operator. If LookAhead gain is turned off (= 0), integral gain enters the feedback process unchanged. The integral gain is then used to
calculate a running average of error as follows:
new

z acc

LA

= error G int

old

+ z acc

new

old

where z acc is the new average error calculated by adding the old average error z acc
to the product of the integral gain times the error. The running average represented
new

by z acc maintains itself continually until one or more of the major scanning parameters is changed by the operator. Whenever major scan parameters are changed
(e.g., Setpoint), the error accumulator is dumped and begins a new running average. With the average error calculated, the feedback system is prepared to make its
final error correction based upon proportional gain.
Proportional gain
The third and final step in the feedback process uses proportional gain to complete
error correction. Recall that proportional gain responds to error in proportion to
how much it differs from the setpoint. Proportional gain is used to calculate the
final correction voltage sent to the Z-axis piezo according to the relation
new

z voltage = z acc

+ error G prop

As suggested in the equation, by the time proportional gain is figured in, the bulk of
error correction has already been completed. This tends to make Proportional gain
a less touchy control when compared to Integral and LookAhead gain. Nevertheless, the system can be driven into oscillation whenever gains are excessive,
including Proportional gain.
REMINDER: Gain values entered on the Real Time / Feedback Controls panel
do not directly translate to any real quantity, but are merely self-referencing; e.g., a
Proportional gain value of 2.0 is not the same as Integral or LookAhead gain
values of 2.0.

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2.3.9. What Data Type of image?

SPM technology at Digital Instruments has rapidly grown beyond its scanning tunneling roots to encompass numerous types of microscopy. This includes: ECSTM,
contact AFM, ECAFM, TappingMode in air, TappingMode in fluids, amplitude and
phase magnetic force microscopy (MFM), surface potential and field gradient electric force microscopy (EFM), lateral force microscopy (LFM), force modulation
imaging, scanning capacitance microscopy (SCM), thermal imaging, and force volume imaging. In addition, there are numerous variations and combinations of the
above; new types of SPM are added continually as the field expands. Each of these
variations reveals something unique by using Digital Instruments feedback system
to process and extract signals in slightly different ways.
The NanoScope system allows up to three simultaneous image channels, plus auxiliary channels. Each of the image Channel control panels (Channel 1, 2, and 3)
contains a Data type parameter specifying the type of image to be shown on that
channel. The Data type, in turn, is determined by the currently selected microscope
(Real Time / Microscope / Select) and AFM mode shown on the Other Controls
panel. For example, although Height data can be displayed for most types of imagery, only TappingMode displays Amplitude data. Similarly, only contact AFM displays Friction data. Whenever the AFM mode and Data type parameters are
changed, some new portion of the feedback signal is utilized and/or processed differently. Some users tap the NanoScopes auxiliary channels to generate new type
of images from the feedback system.
To better understand what is being viewed when selecting different Data types,
consider the diagram below:
height

Signal out (to Z piezo)

Feedback Controller

Signal in (Inaux)
Signal in (In0)
Microscope

deflection, amplitude, current

auxiliary: phase, frequency, deflection during
TappingMode, friction.
As this diagram shows, different portions of the feedback loop are being accessed,
depending upon what is selected at the AFM mode and Data type parameters. During STM, the signal coming into the feedback controller (at line In0) is Current. In

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contact AFM, the same line now conveys Deflection voltage. In TappingMode, the
same line conveys Amplitude data. In addition, the auxiliary channels utilize line
InA through InD.

Notes

Although there are four separate auxillary lines (InA through InD), the controller
can only access one at a time, plus the In0 line.
The controller is designed to handle two input signals simultaneously (In0 and one
auxiliary line). Because it is extracted from a different (output) portion of the feedback loop, a third channel can be used to simultaneously extract Height data without affecting the input signals. This allows a maximum of three Data types for any
one sample. For example, a sample being imaged with contact AFM can show
Height, Deflection and Friction all at the same time.

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2.4. Control Parameters and Feedback

The feedback scheme described in Section 2.3 above provides a general platform
for imaging sample surfaces; however, vast differences in samples require additional controls to obtain optimal images. The NanoScope imaging system utilizes
over 1000 parameters. The vast majority of these are never seen by users, but those
that are common should be reviewed. This section provides a brief description of
some of the more commonly used parameters.

2.4.1. Reexamining the Control Loop

Recall that the NanoScope control system performs two main functions: 1) it generates drive voltages to control the X-Y scans of the piezoelectric transducer; 2) it
maintains an incoming analog signal from the microscope detection circuitry at a
constant value. This is done by way of a closed-loop feedback control system. The
computer is programmed to read voltage from a comparator circuit through an analog-to-digital (A/D) converter. It is programmed to keep the two inputs of the comparator circuit equal (0 volts). An output voltage generated by the computer
continuously moves the piezoelectric transducer in the Z direction to correct for differences read into the A/D converter. This closed-loop feedback control is the heart
of the imaging portion of the control station.
SPMs are capable of displaying either the input (difference), or output (correction)
applied to the Z-axis piezo. The Nanoscope III control system can also display
information from a second A/D converter. This second input can be friction
between the AFM tip and the sample, data from an electrochemical cell, or one of
four user-selectable inputs.

2.4.2. General Description of Main Menu Items

This section is a general overview of various Real Time menu items. Refer to the
Command Reference Manual for more information about these settings.
Scan size Size of the scan along one side of a square. If the scan is non-square
(as determined by the Aspect ratio parameter), the value entered is the longer of
the two sides.
Aspect ratio Dermines whether the scan is to be square (Aspect ration 1:1), or
non-square (Aspect ratio 2:1, 4:1, 8:1, 16:1 or 32:1). The Aspect ratio parameter
is only displayed if the Non-square scan option is selected in the Scan Controls
panel (upper-left panel button).
X offset; Y offset These controls allow adjustment of the lateral scanned area
and the center of the scanned area.

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Scan angle Combines X-axis and Y-axis drive voltages, causing the piezo to scan
the sample at varying X-Y angles.
Scan rate The number of lines scanned per second in the fast scan (X-axis on
display monitor) direction.
Number of samples Sets the number of pixels displayed per line and the number
of lines scanned per frame.
Slow scan axis Starts and stops the slow scan (Y-axis on display monitor). This
control is used to allow the user to check for lateral mechanical drift in the microscope or assist in tuning the feedback gains. Always set to Enable unless checking
for drift or tuning gains.
Z limit Limits the amount of drive voltage available to the Z piezo circuit. The Z
control system uses a 16-bit D/A converter which drives an amplifier capable of
outputting voltages from +220V to -220V. This means that the resolution of the
control over the Z direction is approximately 6.7mV per bit (440V divided by
65536). This setting defaults to 440V automatically. Reducing the Z limit is useful,
when using a E or J scanner, if scanning samples with relatively small Z features (less than 10 nm peak-to-valley). For example, setting the Z limit to 55V
means that 55 Volts is divided by the same 16-bit digital control. This gives eight
times finer control over the Z direction of the scanner.
Integral gain and Proportional gain Controls the response time of the feedback loop. The feedback loop tries to keep the output of the SPM equal to the setpoint reference chosen. It does this by moving the piezo in Z to keep the SPM's
output on track with the setpoint reference. Piezoelectric transducers have a characteristic response time to the feedback voltage applied. The gains are simply values
that magnify the difference read at the A/D convertor. This causes the computer to
think that the SPM output is further away from the setpoint reference than it really
is. The computer essentially overcompensates for this by sending a larger voltage to
the Z piezo than is truly needed. This causes the piezo scanner to move faster in Z.
This is done to compensate for the mechanical hysteresis of the piezo element. The
effect is smoothed out due to the fact that the piezo is adjusted up to four times the
rate of the display rate.

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2.4.3. User Example

Try this experiment with an easy sample to see how changing parameters influence
an image. A good choice of sample is a diffraction grating or the calibration reference supplied with the system.

Display both the input and the output of the feedback loop. This means setting
the display to show both Height data and the appropriate microscope signal
(STM = Current, contact AFM = Deflection; TappingMode AFM =
Amplitude).

Engage the microscope and reduce the gains until they are close to zero. The
input display data will become larger in Z, and the height data will blur or
become smeared. Raise the gains using the arrow keys until the input voltage is
minimized.

Try increasing and decreasing the scan rate parameter. This will increase or
decrease the traveling velocity of the tip. Note that it will be necessary to
increase the gain settings at faster scan speeds and decrease the gains at slower
scan speeds.

2.4.4. Review of General Operating Concepts

The AFM system is comprised of two main components: 1) the scanner; 2) the
AFM detection system. The scanner houses the piezoelectric transducer. The piezo
element physically moves the sample in the X, Y and Z direction. The detection
system consists of a laser which generates a spot of light that is reflected off of a
microfabricated cantilever onto a mirror and finally into a photodetector (see figure
2.14). The position of the spot is determined by circuitry which generates a voltage
from the difference between the photodiode segments (A - B). The circuit outputs a
voltage ranging from +10V to -10V depending on the position of the spot on the
two photodiodes.

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The AFM system maintains the tip at the end of the cantilever in contact with the
sample surface. The sample is scanned under the tip in X and Y. Features on the
sample surface deflect the cantilever, which in turn change the position of the laser
spot on the photodiodes. This position change is read by the feedback loop. The
feedback loop moves the sample in Z to restore the spot to its original position.
Refer to figure 2.14 (opposite page).
Figure 2.14.A. A flat portion of the sample surface is scanned beneath the tip leftto-right, maintaining the laser beam at the center of the photodiode array.
Figure 2.14.B. As the tip encounters a raised feature, the cantilever is pushed up,
deflecting the laser beam upward onto the "A" portion of the array. With the "A"
photodiode receiving an increased portion of the laser light, its voltage increases
while portion "Bs" decreases (A > B).
Figure 2.14.C. The Vertical Deflection (A-B) voltage differential is sensed by the
feedback electronics, causing a dropped voltage to the Z piezo crystalthe piezo
retracts. As the Z piezo retracts, the cantilever recenters the laser beam onto the
photodiode array (A = B).
Figure 2.14.D. As the tip encounters a decline in the sample topology, the tip drops.
This directs more of the beam onto the "B" portion of the photodiode array. With
the "B" photodiode receiving an increased portion of the laser light, its voltage
increases while portion "As" decreases (A < B).
Figure 2.14.E. Again, the Vertical Deflection (A-B) voltage differential is sensed
by the feedback electronics, increasing voltage to the Z piezo crystalthe piezo
extends. As the Z piezo extends, the tip is pushed down until the laser beam
recenters on the photodiode array (A = B).

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Photodiode Array
Photodiode "B"

Mirror
Laser

Photodiode "A"
Laser beam

Tip

A-B (Vertical Deflection) Reflected

Laser Beam
Voltage
O Volts
Setpoint
Voltage

A/D
Converter

Sample

Z piezo
Scanner
Tube

Computer

B
A

Figure A

Figure D

Figure B

Figure C

Figure E

Figure 2.14. Contact AFM concepts (Figures AE exaggerated.)

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The AFM always first engages in the repulsive region of its operating range. In
other words, the cantilever needs to exert a positive pressure on the sample surface.
The AFM block diagram shows the relationship between the cantilever movement
and the laser spot on the photodiode array. The diagram shows that the spot moves
up (more on "A") when the cantilever is pushed up. The initial setup is to have the
Vertical Deflection (A-B) voltage about 2-3 volts more negative than the Setpoint
voltage. Digital Instruments recommends starting with the Setpoint voltage set to 0
volts and the Vertical Deflection (A-B) set to -2 volts. The reason for this is that 0
volts is the middle of the control range. The indication of a good engagement is a
distinct jump of about 1V from the Vertical Deflection (A-B) voltage to the Setpoint voltage.
The displayed image is an average of the corrections made to Z in a given display
period (number of samples menu item). The two gains are set to values to effectively tune the feedback response to the particular sample topology. This will set
response time of the system so that there is no difference between the SPM's signal
and the setpoint reference during scanning.
Proportional gain The computer multiplies this number times the value read
from the comparison circuit every time the A/D converter is read. It is the high frequency feedback control.
Integral gain This number is multiplied times an accumulated average of A/D
readings. This is the low frequency feedback control.
One of the easiest ways to set the gains properly is to view the input of the feedback
loop. This means displaying the STM current, the AFM deflection, or the TMAFM
amplitude signal. Then raise the gain values until the input of the feedback is minimized. Note that this will result in an image that shows only large transitions in Z;
this is normal. There will always be a time lag between the input and the output
(height data) of the feedback loop. Usually, the Integral gain is the most sensitive
control. Raise the gains together until the input signal (current, deflection or amplitude) is minimum. Don't set them so high as to cause oscillations in the image.
Oscillations are an indication of too much feedback correction voltage sent to Z.
This is generally known as feedback oscillation. The Proportional gain can usually be set about 20 percent higher then the Integral gain, but it is not required.

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2.5. Review of TappingMode AFM

2.5.1. General Operating Concepts
One advantage of TappingMode AFM is an absence of frictional forces which exert
torque on the cantilever. Unlike traditional contact AFM, the feedback loop keeps a
vibrating cantilever at a constant amplitude, rather than keeping a cantilever at a
constant deflection. The tip on the cantilever is modulated through mechanical excitation at its resonance. A laser beam is reflected off of a microfabricated cantilever,
onto a mirror, then reflected onto a photodiode array. The laser spot oscillates vertically across the array as a result of the vibrating cantilever. The signal from the photodiodes is rectified, then lowpass filtered into a DC voltage (RMS Ampl.). The
magnitude of the RMS amplitude is proportional to the amount of cantilever
motion.
The feedback system compares the RMS amplitude to the setpoint voltage. The two
voltages are kept equal by controlling the amount of cantilever movement. The
sample surface is in close proximity to the cantilever. The distance is such that the
tip touches the surface only at the lowest point of its oscillation. The RMS voltage
is reduced to the setpoint voltage by the feedback loop moving the tip into the sample. The sample restricts the cantilever movement until the desired RMS voltage is
reached. The damping of the cantilever is held constant by moving the tip in Z as it
is simultaneously translated in X and Y.
The engagement of TappingMode AFM requires that the setpoint voltage be smaller
than the RMS voltage, which is set automatically by the software. The tip is lowered until the RMS reaches the setpoint.

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Photodiode Array
Photodiode "B"
Mirror
Laser
Photodiode "A"
Laser beam
Reflected Laser
Beam
Oscillating tip

A-B (Vertical Deflection) Reflected

Laser Beam
Voltage
Vx
A/D
O Volts Converter
Vs
Setpoint
Voltage

Figure A

Sample
Z piezo
Scanner
Tube

Computer

Figure B

Figure C
Setpoint Voltage

Figure D
RMS Voltage
Setpoint Voltage

RMS Voltage

RMS Voltage

RMS Voltage

Setpoint Voltage
Setpoint Voltage

0 Volts RMS

0 Volts RMS

0 Volts RMS

0 Volts RMS

Figure 2.15. TappingMode AFM concepts. (See sect. 2.5.2 for explanation.)
Figure 2.15 shows the relationship between the RMS and the setpoint voltage during the engage cycle. The initial setpoint voltage is determined by the computer
rather than the user. The computer sets the setpoint equal to 95 percent of the RMS
amplitude. The tip is then lowered until the RMS matches the setpoint. The computer then tests for true engagement as follows: 1) the motor halts the tips descent;
2) the setpoint is lowered slightly; 3) the feedback control monitors movement of
the Z piezo. Depending upon the tips relationship to the sample, one of the two following conditions will result:
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1. A small Z piezo movement. This indicates that the cantilever is truely engaged
with the sample surface.
2. A large Z piezo movement. This indicates that the cantilever is being damped by
air trapped between the cantilever and sample surface (not in contact with the
actual, solid surface)this is a false engagement condition. The setpoint is readjusted and the engage cycle repeated until the computer reads a small change in Z
when the setpoint voltage is lowered further. One symptom that this condition is
occuring is when the tip travel m display stops momentarily, then starts again.

2.5.2. Optimizing the TappingMode AFM signal after engagement.

The figures on the bottom of figure 2.15 show the relationship between the RMS
and the setpoint voltages.
There are some basic rules to remember:
1. The setpoint voltage is always lower than the RMS voltage (figure A).
2. The difference between the RMS voltage when the tip is off the surface, and the
setpoint voltage dictates the amount of damping or tapping force. The larger the
difference, the greater the tapping force (figs. A, B).
3. The RMS voltage controls the amount of energy that is in the cantilever (figs. A
and D). This is important to note because some samples are stickier than others.
The tip may stick and, therefore, be held to the sample surface if the RMS amplitude is too small.
The initial setup for TappingMode AFM is to:
1. Tune the cantilever at its resonance. Quit out of the View / Cantilever Tune software routine after the resonance is found.
2. Set the desired RMS voltage. This is usually about 1 to 4V.
3. Engage the microscope.

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2.6. Terms and Abbreviations

This section contains a brief list of terms and abbreviations to assist the reader.
Other terms and abbreviations are referenced in the Index at the back of this manual.
AFM Atomic force microscopy; atomic force microscope.
aliasing Electronic image error due to differences in resolution between surface
features and the pixels used to represent them.
bias Electrical potential applied to a tip or sample which causes electron flow to
ensue from one to the other. (STM and EFM only.)
calibration Measurement of known features to ensure accuracy of SPM images.
cantilever Flexible portion of probe extending from the substrate and to which
the tip is attached.
cantilever tune Process of finding a cantilevers natural, resonant frequency by
exciting the cantilever through a range of frequencies until maximum amplitude is
obtained. The frequency at which maximum amplitude is obtained is the resonant
frequency.
DSP Digital signal processor. Computer processor used to control SPM feedback
loop.
drive amplitude Amplitude of the signal used to oscillate a tip in TappingMode.
drive frequency Frequency of the signal used to oscillate a tip in TappingMode.
ECAFM Electrochemical atomic force microscopy; electrochemical atomic
force microscope.
EFM Electric force microscope; electric force microscopy. Method of SPM used
to image electric forces on samples.
engagement Process of bringing a probe tip and sample together in a controlled
manner such that useful information about the surface is obtained without damaging either the tip or the sample.
error Difference between actual tip-sample force measured at the detector and
the setpoint force.

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false engagement Condition due to surface effects or insufficient setpoint (too

low during contact AFM; too high during TappingMode) in which the feedback
controller attempts imaging a sample that is not engaged with the tip.
feedback Process of self-correction between probes actual, real time height-surface force and its intended height-surface force based upon the probes signal.
fluid cell Accessory used for imaging materials in fluid, consisting of a specialized tipholder and o-ring.
force modulation SPM mode used to image visco-elastic properties of materials.
integral gain Amount of correction applied in response to the average error
between setpoint force and actual force measured by the detector.
LFM Lateral force microscopy; lateral force microscope. Frictional measurements of surfaces based upon a tips lateral and torsional response.
LiftMode Two-part, proprietary method of imaging surfaces consisting of a
surface scan to obtain height data, followed by a second scan to extract other information about the surface (such as magnetic force or elasticity) while the tip profiles
the previous Z path at a constant height. The two images are subtracting from each
other to yield an image uninfluenced by topography.
LookAhead gain Amount of correction applied in response to the error signal
between setpoint force and actual force measured by the detector, based upon
recorded information from the adjacent scan line.
MFM Magnetic force microscope; magnetic force microscopy.
NanoScope Trademark name applied to Digital Instruments SPM products.
probe Integrated mechanical device used to image surfaces, including a substrate, cantilever and tip.
proportional gain Correction applied in response to the error signal between
setpoint force and actual force measured by the detector, in direct proportion to the
error.
RMS amplitude Root mean square (RMS) signal measured at the detector. (TappingMode only.)

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SPM Scanning probe microscopy; scanning probe microscope. A general term

encompassing all types of microscopy which utilize a scanned micro-sharpened
probe and feedback circuitry to image nanometric phenomena. Includes AFM,
ECAFM, ECSTM, EFM, MFM, STM, and many others.
STM Scanning tunneling microscopy; scanning tunneling microscope.
sensitivity Amount of movement produced by a scanner piezo for a given
amount of voltage.
setpoint Operator-selected force threshold between tip and sample used as the
feedback control loops target.
spring constant Amount of force required to bend a cantilever some given
amount.
TappingMode Proprietary mode of SPM exclusive to Digital Instruments
which utilizes an oscillating probe to obtain nanometric images. Advantages
include negligible surface impacts, high resolution and sensing of magnetic, electric and chemical forces.
tipholder Removable appliance for mounting SPM probes. On MultiMode
SPMs, the tipholder is installed within the head of the microscope. On Dimension
Series SPMs, the tipholder plugs onto the end of the scanner tube.

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Chapter 3

Setup & Installation

3.1. Installing the MultiMode SPM

Set up the computer, main controller and two monitors as described in this chapter.
If MultiMode software is not already installed on the system, install the software on
the Intel PC using the supplied 3.5" floppy disks. The MultiMode scanning probe
microscope control program should be installed in a special directory (C:\SPM)
which must be entered to run Z.EXE.

3.2. Component List

If this is a first-time installation, verify that you have received all necessary components. The MultiMode SPM system includes the following:

MultiMode SPM base

NanoScope SPM controller
MultiMode SPM Instruction Manual (this document)
Command Reference Manual

MultiMode parameter files on 3 1/2 diskette1

1. NOTE: The calibrated scanners parameter files are located in the hard disks EQUIP
directory.

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Component List (cont.)

NanoScope controller-to-MultiMode SPM cable, 37-to-25 pin, D-type.

Fiber optic illuminator, Fiber-Lite, Model 190
Vibration isolation pad
Scanner calibration reference: XYZ, 10 x 10, 180 nm vertical (all scanners);
Mica sample ("A" scanners); 1 XY grating ("E" scanners)

Package of 10 contact mode cantilevers - silicon nitride type

Package of 10 TappingMode cantilevers - single crystal silicon
MultiMode SPM head

Figure 3.1. MultiMode SPM head.

3-2

MultiMode SPM scanner with retaining springs

Tweezer kit containing: SM3-SA; SA-2A; 88 MM; 7-SA.
45X magnifier with mounting stand
Sample disks (pucks): 20 large, 20 small.
Sample adhesives
Noise reduction hood
Intel computer
Monitors: 14" (NEC XV15) and 17" (NEC XV17)

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Setup & Installation

3.2.1. Unpack The System

The NanoScope system is normally shipped in five separate boxes. Each monitor is
shipped in its own box, the computer and controller are shipped in separate boxes,
and the MultiMode SPM, cables and hardware are shipped in one box.

Figure 3.2. Each monitor is shipped separately (left). The SPM is packed in
a separate box (right). Heavy hardware should be removed carefully from
each box with the help of 2-3 people.
1. Clear a table for the microscope. You will require a table of at least 76 x 152 cm
(30 x 60 inches) size. The table should be level, of sturdy construction, and located
where it will not be vibrated or jarred by foot traffic. It should be located away from
sources of heat and cold; avoid windows, air conditioning and heating ducts, blowers, etc.
2. First remove the computer and controller. The controller may be used to support
the display monitor1 as shown in the setup below.
Extender box
(if supplied)

Control monitor

Printer cable

Display monitor

Computer

NanoScope
controller
SPM
Keyboard
Mouse

1. The display monitor is the larger (17-inch) of the two monitors.

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3. Remove the remaining components and locate them using the layout above as a
guide. Some users find it advantageous to set the SPM on the floor or atop a heavy
concrete cinder block. This will reduce vibrational noise which can affect scans. If
a tripod vibration isolator or similar mount will be used, locate it next to the table.
All units are supplied with a round vibration isolation pad to set the SPM on. This
can be used between the SPM and table top or floor to reduce vibrational noise.
Cabling
4. Before connecting cables, review the following precautions:

DO NOT power anything until all cables are connected and double-checked.
Power cords should be connected to their source of power last.

DO NOT route cables through pinch-points or over sharp edges. The table
should be pulled away from walls so that cables will not be pinched. The cable
between the controller and SPM carries up to 440 volts and must be protected
from chaffing.

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Setup & Installation

5. Connect computer cables (monitors, keyboard, mouse, controller and printer) as

shown below.
*Verify that voltage
selection switch is
set correctly for
your voltage.
Power
Mouse
Keyboard
COM2
(Dimension SPMs only)

Printer (LPT1)

COM1
(Trackball)

Display monitor
Control monitor

NanoScope
controller

Figure 3.3. Rear view of computer on standard MultiMode systems.

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NanoScope
controller

Control monitor
Display monitor

COM1
(Trackball)
Printer (LPT1)
COM2
(Dimension SPMs only)
Mouse
Keyboard
Power

*Verify that voltage

selection switch is
set correctly for
your voltage.

Figure 3.4. Rear view of computer on ce certified (European) MultiMode

systems.
Note that computers are not equipped with network cards from DI, but may be
added by the user. Printers are also user-supplied. Serial ports COM1 and COM2
may be configured by the user for peripheral equipment.
6. Connect cables to the back of the NanoScope controller: the power cable should
be connected to the controllers receptacle on one side, the controller-to-computer
cable on the other. DO NOT connect the power cable to a source of power yet.
7. The SPM is connected to the front of the controller with the 37-pin ribbon connector. Verify that the ribbon cable is securely connected; otherwise, the microscope may not engage or exhibit other problems.

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Notes

If an Extender Electronics Module is included, install it now between the

SPM and controller. Verify that it has been properly configured per instructions
provided in Chapter 13 of this manual BEFORE powering the NanoScope
controller.
8. Install the scanner on the support ring with the scanner cap upright. If the motorized scanner screw will not seat securely into the coupling on the base, use the toggle switch on the SPM base to rotate the screw slightly until it aligns and seats with
the coupling. Attach retaining springs to the support ring by inserting into holes and
securing with screws. Plug the scanner into the receptacle on the support ring as
shown below:
(Shown: "J" scanner)

Plug scanner into

support ring here.

Motorized scanner
screw must seat
with coupling here.

Front View
Rear View

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9. Carefully set the MultiModes head atop the SPM scanner. The head should mate
kinematically with the scanners contact balls. Secure the head using both retaining
springs by stretching the springs up and hooking them over posts located on both
sides of the head. Plug the head into the receptacle on the support ring as shown
below:
(Shown: "A" scanner)

Plug head into

support ring here.
Front View

Rear View
10. Recheck all cable connections. Review the steps above one last time to ensure
that all connections are properly made. Be especially certain that the controller
cable is NOT plugged into the parallel port of the computer or damage to the electronics will result.

3.2.2. Vibration isolation

The microscope must be isolated from sources of vibration in the acoustic and subacoustic frequencies. This requirement can be relaxed somewhat for large-scale
images, but atomic-scale imaging is sensitive to ordinary room vibrations.
Reasonable vibration isolation can be obtained with the black vibration isolation
pad supplied with the system. In many cases, the pad provides enough vibration
isolation to run the microscope on the table, but the pads are especially effective
when placed on a massive object isolated from the fan noise of the computer.
Another effective vibration isolation system consists of a large mass, 20 or more
pounds, suspended from elastic "bungee" cords. The mass should stretch the cords
at least one foot, but not so much that the cords reach their elastic limit. The SPM
should be placed on the large mass having a natural frequency of about 1 Hz or less
both vertically and horizontally. Test this by gently pushing on the mass and measure the rate at which it swings or bounces. A ready-to-use tripod isolation system

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is also available from Digital Instruments (model TRVI). Experience suggests that
air tables often have poor horizontal isolation. If an air table is used, it may require
additional horizontal isolation for atomic-scale images.
As a final note, the best way to reduce coupling from vibrations is to eliminate as
many sources of vibration as possible. Remember that vibrations can be transmitted
to the SPM over the cable. To reduce this phenomenon, prevent tension in the cable
and keep it away from fans and other noise sources. Also, keep the microscope
away from sources of acoustic noise. Loud noises (including conversation) can disrupt atomic images, so it is best to isolate the SPM as much as possible. Use the
noise reduction hood supplied with the system to alleviate acoustic noise.

3.2.3. System Power Up & DOS Start-Up

Verify that all cables are interconnected, especially the SPM controller to the computer. Power up the two monitors, followed by the NanoScope controller, then the
Intel computer using the switch in front. Using a power strip switch allows you to
power up the entire system at the same time.

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MultiMode SPM Instruction Manual

Chapter 4

Cantilever Preparation for the

MultiMode SPM

The MultiMode microscope comes furnished with etched silicon cantilever substrates for TappingMode AFM and silicon nitride cantilevers for contact AFM
modes. In both cases, the cantilever probes should be inspected under the microscope when being used for the first time, to get a better understanding of how the
probes and substrates are connected and taken apart. The procedure for removing
individual substrates from the wafer varies depending on the wafer. It will be easier
to accomplish this task with the aid of a stereo microscope having 5070X magnification.

4.1. Silicon Cantilever Substrates

The silicon cantilever substrates used in TappingMode can be removed from the
wafer with the following procedure. Note that the cantilevers are stored tip-side-up
and that the silicon is very brittle. Contacting the cantilever during this operation
will almost certainly break it off of the substrate.
1. Inspect the wafer with an optical microscope to get a feel for the orientation of
the cantilever substrates and to inspect the cantilevers themselves. (A 10-70X stereo
microscope is useful for this task.) The cantilevers are tip side up as viewed in the
wafer holder. Included with the MultiMode microscope is a wafer tool kit which
contains tweezers and wafer handling tools.
2. Disconnect the substrate from the bulk of the wafer by pressing down gently on
the non-cantilever end of the substrate. Alternatively, using the sharp pointed tweezers, carefully break the 2 substrate supporting arms connecting the substrate to the

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Part II: Pre-Imaging Preparation

silicon wafer frame. The supporting arms connecting the substrate to the bulk of the
wafer will shatter as pressure is applied. See figure 4.1 for clarification.
It may be convenient to break several substrates from the wafer at one time. Extras
may be safely stored in a specially prepared closable container. At the bottom of the
container, place X4-grade, GEL-PAK adhesive strips. Place the substrates, tips
facing up, on the adhesive to permit easy removal of the substrates when needed.
Cover the container when not in use.

Cantilever

Press here
to break out
substrate

Substrate
Supporting
Arm

Cantilever
Substrate

Figure 4.1. Silicon cantilever substrates in wafer.

4. Use the curved, sharp-pointed tweezers to remove the cantilever substrate from
the wafer container. Grasp the sides of the substrate, away from the lever and probe
tip. It may be helpful to tip the substrate to one side to help grasp it in the tweezers.
Be very careful about avoiding any contact with the probe lever, since it will immediately snap off. Silicon is very brittle.

4.1.1. Tip Shape of Etched Silicon Probes

Etched silicon probes provide the highest aspect ratio and most consistent tip sharpness of the probes supplied at present. There are some subtleties in general shape
that should be understood to gain the best advantage from the etched silicon tips
when imaging samples with steep walls over steps of 100 nm to several microns in
height.

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17.0

Cantilever Preparation

17.0

Tip
25.0

10.0

Cantilever

Figure 4.2. Silicon cantilevertheoretical tip shape.

The present process creates a tip which has symmetry from side to side with a 17+
2 half cone angle (refer to top of figure 4.2). Front-to-back, along the length of the
lever, the tip is asymmetric (refer to lower-right of figure 4.2). Another factor affecting the interaction of the tip shape with the surface is the substrate mounting angle.
Along the front edge of the tip, the half angle is nominally 25, and at the back edge
of the tip the half angle is approximately 10, with both of these numbers not
accounting for the tilt of the substrate. With the mounting angle of the substrate
taken into account, the front is 35 and the back is zero degrees. From the tip side,
the cross-section of the tip near the lever is approximated by an inverted kite
shape. All of these subtleties arise from the etching process used to make the tip,
which employs caustic solutions to perform wet anisotropic etching of the silicon.

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Scan line produced using a theoretical

probe tip shape on a 1 - 2 m deep
vertical wall trench
Scan direction = 0 deg.

10
11
55

80

Scan Line Profile

1 m - 2 m Deep Trench

Note: Any wall angle on the left wall that is > 55 deg.
will be shown as 55 deg. in the image.

Figure 4.3. Silicon probe tip profile artifact - front to back

The best orientation of the sample to measure sidewall angles, uses the back edge of
the tip (that which faces back towards the cantilever substrate) to measure step
angles (refer to figure 4.3). Using the back edge, step angles approaching 80
degrees can be measured routinely, depending on the step height. Ensure that the
area of measurement offers sufficient clearance so that other faces and edges of the
tip and lever do not interfere with the measurement. This method does not work
well in small openings of less than 5 microns where, depending on the depth of the
step, other edges of the tip could contact the other faces of the small opening. Wall
angle measurements are best measured in open areas for these reasons.

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Cantilever Preparation

Scan line produced using theoretical

probe tip shape on a 1 - 2 m deep
vertical wall trench
Scan direction = 90 deg.

73 73
Scan Line Profile

1 - 2 m Deep Trench

Note: Any wall angle that is > 73 deg.

will be shown as 73 deg. in the image.

Figure 4.4. Silicon probe tip step profile artifact: side-to-side

Measurements of line pitch are often best measured using the side-to-side faces of
the tip, which exhibits symmetry. Because of the approximate 17 half angle of the
tip, the line or space measurement is best done at the top of the line for simplification of the measurement artifacts (figure 4.4).

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20 - 30

Figure 4.5. Silicon probecommon shape artifact.

Due to the nature of the etching process that shapes the tip, there is often a short
angled ridge near the highest point of the tip. The exact length of the ridge is variable but rarely exceeds 0.5 m in total length. It is inclined steeply, so that for reasonably flat surfaces the highest point is the only one which interacts with the
surface. Depending on the tip in use, sample features of approximately 0.5 m in
height can begin to produce artifacts of an apparent shallow slope over scan fields
of larger than 1-2 m.

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Cantilever Preparation

Subsequent scan line produced by using

the realistic probe tip shape

10
11
55

70 - 80

Scan Line Profile

1 m - 2 m Deep Trench

Note: Any wall angle on the left wall that is > 55 deg.
will be shown as 55 deg. in the image.
Any wall angle on the right wall that is >70-80 deg.
will be shown as 70 -> 80 deg. in the image.

Figure 4.6. Common silicon probe profileresultant scan artifact.

Shown above in figure 4.6 is the resultant effect of the angled back ridge on the step
angle measurement for a deeper trench depth. This will be tip and topography
dependent.
The above discussions for figures 4.24.6 are in relation to microscopic scale shape
characteristics. There is one further detail which can come into play affecting the
wall angle over shorter (nominal 100 nm) step height measurements: the shaped
cusp at the end of the tip.
The shaped cusp at the end of the tip is formed to increase the sharpness of the
point of the tip to a length of 100 nm from the end of the tip. It is formed in such a
manner that the radius of curvature of a silicon tip can be in the range of 510 nm
(on a very good tip).

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4.2. Silicon Nitride Cantilever Substrates

When using the MultiMode microscope for the first time, start with the provided
strip of cantilevers and skip to step 4, which follows. Step 4 provides instructions
on how to separate substrates from strips.
1. Verify that the wafer is oriented with the tips facing upward (gold coated surface
down). Inspect the wafer with an optical microscope. We suggest using a 10 -70X
stereo microscope to become familiar with the styles and orientation of the cantilevers on the probe substrate.
2. Remove the Pyrex strips by resting the silicon ring on a glass slide or ruler, then
applying downward pressure with the tweezers until the strip breaks free from the
silicon ring. While doing this, be very careful to avoid pushing strips together as the
cantilevers are between the strips. (All cantilevers on one side of both strips could
break off, if this occurs accidentally.)

Press here to break out strip.

Position glass slide underneath

for support.

Figure 4.7. Silicon nitride cantilevers in a wafer.

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Cantilever Preparation

3. Place the strip down on a white piece of paper to inspect it under the microscope.
When doing this, be careful that the cantilevers are on the top side of the strip. The
cantilevers are on the same side as the reinforcing ring, while the saw-cuts are on
the opposite side from the cantilevers. Between each one on the down side of the
strip should be a saw-cut almost through the Pyrex.
4. Handling the strip by its ends, place it on a glass slide (taped down to the edge of
a table) with the substrate or spacer piece to be removed, hanging over the edge, as
shown in Figure 4.8. The saw cut should be approximately on the edge of the slide.
While holding down the next substrate on the strip with the wooden end of a cotton
swab, grip the overhanging piece with a pair of wide tweezers and rotate downward. It should pop right off. Repeat this process until as many cantilever substrates
as required have been removed.

Cantilever

Cantilever
Substrate Substrate

Hold down here with

Edge of Glass
end of cotton swab Slide
Edge of Glass Slide

Grip here with wide tweezers.

Rotate downward until
substrate snaps off.

Saw Cuts
Saw-Cuts

Press Here to
Break Off

Figure 4.8. Substrate break-off.

Extra substrates are easily stored in a covered container. The shipped substrates are
held on X0-grade, GEL-PAK adhesive strips. The strips are used to permit easy
removal of the substrates. If GEL-PAK adhesive strips can't be found, a simple substitute is the adhesive area from a Post-it note. When placing the substrates on the
adhesive, be careful that the cantilevers are on the top side of the substrate.
5. Each substrate has two cantilevers on each end of the substrate. Both 100 and
200-micron length cantilevers with two different leg widths are provided. When
ready to use a cantilever substrate, it may be desirable to remove the unused cantilevers from that substrate, but it is not necessary. For most applications, use the 100-

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micron cantilever with the wider legs. For atomic scale images, the 200-micron triangular cantilever with the wider legs can yield good results.

Figure 4.9. Substrate shown with the 100 and 200 m long, wider
cantilevers on top and the 100 and 200 m long, slimer cantilevers on the
bottom.

4.2.1. Tip Shape of Silicon Nitride Probes

Silicon nitride probes provide low cost and durable probes suitable for contact
mode imaging. There are some subtleties in general shape that should be understood to gain the best advantage from the silicon nitride tips when imaging samples
with steps of 0.1 to several microns in height. Bear in mind that the probe tip is
approximated by a pyramid formed by intersecting <111> planes in silicon. The
approximate shape of the tip is shown in the upper right in figure 4.9. In the same
figure are dimensions and approximate values for spring constants and resonant frequencies.

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Cantilever Preparation

45

35

4 m

C
D

Lever Type
100 m Wide
200 m Wide
100 m Narrow
200 m Narrow

A
115
193
115
193

B
122
205
122
205

C
21
36
15
20

D
60
113
69
150

Spring constant
(N/m)
0.58**
0.12**
0.38**
0.06**

Measured Fr
(kHz)
40
12.3-22.1
-

Figure 4.10. Silicon nitride cantileversspecifications and tip shape.

Because the silicon nitride probe tips have lower aspect ratios than single-crystal
etched silicon probes, the steepest measurable step wall angle is appreciably lower.
The highest measurable angle using silicon nitride probes is approximately 65
(figure 4.10) using the inner face of the tip (towards the cantilever holder). The
steepest measurable angle from side to side (parallel to the edge of the probe's substrate) is approximately 55. Both of these figures assume that the measurement
does not have interference from other edges.

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45.0

65.0

11
10.0

Scanning Profile

Figure 4.11. Silicon nitride cantileverssidewall profile effect.

There is one last detail that is useful to know about silicon nitride cantilever probes.
There are two types available: standard and oxide-sharpened tip processes. The
standard devices have the nitride deposited directly into the etched silicon mold pit
formed by the intersecting <111> planes, and have points that are slightly rounded
with respect to the tips produced using the oxidation sharpening process.
The oxide-sharpened silicon nitride probes have a thermally grown silicon dioxide
film deposited in the mold pit used to shape the nitride tip, prior to silicon nitride
film deposition. The oxide has two effects: it shapes the inner contours of the pyramidal pit so that there is a slight cusp formed at the point of the pyramid, and the
oxide protects the tip from excessive exposure to a long duration wet silicon etch
used to free the cantilevers from the silicon substrate. The result is a noticeably
sharper point at the end of the pyramid. Regrettably, along with the increased sharpness of the tip comes a slight increase in double tip effect experienced with the
oxide sharpened process.

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Chapter 5

Head, Probe and Sample

Preparation

Preparing to Image with the MultiMode SPM

This chapter provides instructions for head, probe and sample preparation for imaging with the MultiMode SPM. It describes how to remove and install the microscope head, how to change the probe tipholder, how to mount the probe, load and
position samples, and a general description of how to engage and withdraw the tip.
These procedures are common for most types of MultiMode SPM imaging.
Other chapters in this manual describe how to perform specific types of imagery.
The table below outlines where you will find additional information for each type
of imagery. If you are new to SPM and want to practice, we suggest you begin with
contact AFM in Chapter 6.

For Specific Information Regarding:

See Chapter:

Contact AFM in air

Contact AFM in fluids

TappingMode in air and fluids

Scanning tunneling microscopy (STM)

Lateral force microscopy (friction)

10

Force imaging: force modulation, etc.

11

Interleave scanning

12

Magnetic force microscopy (MFM)

13

Electric force microscopy (EFM)

14

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This instrument uses a semiconductor diode laser emitting a maximum 1.0 mW

beam at 670 nm. The light is emitted downward and normally reflects back into the
systems optics from the back of the cantilever probe. Note that the laser is powered
when the SPM head is plugged into the microscopes support ring and the Mode
switch is set to either AFM & LFM or TM AFM (TappingMode). (As a safety precaution, the MultiMode SPM head features an internal switch to shut power off to
the laser when the head is tilted. Operators should use care, however, to avoid staring into beams reflected from sample surfaces.)
WARNING! During and prior to set up of the laser, it is especially important to
avoid looking directly at the laser beam or at the laser spot. The laser head should
never be plugged into the microscope control electronics unless the head is installed
in the Z-stage mount. Care should be taken when highly reflective samples are
inserted onto the chuck. Avoid looking at all reflected laser light. Operators should
use care to avoid staring into beams that may be reflected from sample surfaces.
AVERTISSEMENT! Avant dutiliser le laser, et durant tout le temps pendant
lequel il fonctionne, il est impratif de ne pas regarder directement le faisceau. La
sonde laser ne doit jamais tre branche sur llectronique de contrle du microscope, tant que la tte de mesure nest pas installe dans son support. Il est impratif de faire trs attention lorsque des chantillons trs rflchissants sont dposs sur
la platine. Eviter toute exposition la lumire laser. Durant lutilisation, ne pas fixer
les faisceaux laser rflchis par les surfaces dchantillons.
WARNUNG! Es ist sehr wichtig, vor und whrend der Laserjustierung nicht in
den Laserstrahl oder auf den Laserpunkt zu schauen. Der Laser sollte niemals an
die Mikroskopelektronik angeschlossen werden, wenn er nicht in der Halterung der
Z-Verschiebeeinheit installiert ist. Seien Sie bitte sehr vorsichtig, wenn stark reflektierende Proben auf dem Probenteller liegen. Vermeiden Sie unter allen Umstnden,
in das reflektierte Laserlicht zu schauen. Alle Bediener des Mikroskops sollten
grte Vorsicht walten lassen um zu vermeiden, in den von der Probenoberflche
reflektierten Laserstrahl zu schauen.

5.1. Initial Preparation for Contact AFM Imaging

5.1.1. Prepare the sample.
Verify that your sample will fit atop the scanner tube and is less than 8 mm thick. If
you already have prior experience with loading samples into the MultiMode SPM
system, load your sample now. Otherwise, read the next section for suggestions on
how to prepare and load small samples.

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Sample Preparation
If it is your first time operating the microscope, we recommend that you image the
calibration sample provided with the instrument (usually a 10m-pitch grid of
180nm step height).
The calibration sample or other small sample should be placed on one of the 15 mm
diameter metal disks used for sample mounting. The MultiMode SPM is provided
with several steel sample disks that can be attached to the magnetic sample holder,
located atop the scanner tube.
Provided with the instrument are red and white colored sticky tabs which are 2
sided adhesive patches. Peel off a sticky tab from the provided sheet, and place it
on the steel small sample puck, then peel off the red-and-white paper. This leaves a
patch of the two-sided adhesive on the steel sample disk, which will hold the sample chip to the disk. Using tweezers, place the small sample to be imaged firmly on
the sticky tab adhesive (figure 5.1). Alternatively, a small sample can be glued
down to the sample puck using cyanoacrylate glue (superglue). Place the small
sample disk atop the scanner.

Figure 5.1. Gently press the sample onto the sticky tab until secured.

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5.1.2. Load the sample.

Remove head and load sample.
If the head is not already removed, do so now by unfastening the retaining springs
on either side and unplugging the heads micro-D connector. Gently lift the head off
and set aside. This will expose the top of the scanner tube. Mount the sample puck
with the calibration standard atop the scanner tube. An internal magnet supplied
with most units holds the puck down.

Top of scanner tube.

Place sample puck here.

Retaining springs

Figure 5.2. MultiMode base with scanner mounted on support ring.

Reinstall the head.
With the sample in place, remount the head by gently lowering it over the scanner
tube while checking for clearance. The top of the sample should protrude no more
than a few millimeters above the top of the heads X-Y translation stage. Secure
both retaining springs and plug the heads connector into the support ring (figure
5.3).

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Reattach retaining
springs (2)

Figure 5.3. The head is held securely using retaining springs.

Check head for free vertical movement.
Verify basic function of the motorized Z-axis by toggling the Up switch on the
MultiMode base (figure 5.4). This activates the leadscrew at the rear of the unit to
lift the head upward. If you are using a standard, three-screw scanner, the two forward screws will also have to be rotated to keep the head level while lifting. (Single-screw, vertical scanners require only that the rear, motorized screw be rotated to
raise and lower the head.) To verify rotation of the motorized screw, feel the flexible
coupling on the base with your finger while the tip Up / Down switch is toggled.

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Tip down

Tip up

Figure 5.4. The tip is quickly raised and lowered using the Up / Down
toggle switch on the MultiMode SPMs base.

5.1.3. Load a probe into the tipholder.

Contact AFM

TappingMode

For contact AFM, install a silicon nitride probe tip in the AFM tipholder. Figure 5.5
shows the AFM tipholder. Detailed procedures for silicon nitride cantilever substrate preparation are given in Chapter 4, including a description of the procedure to
break out substrates from the wafer. Ensure the gold-plated side of the substrate is
placed down towards the substrate mount, with the nitride film side attached to the
cantilever oriented up away from the substrate mount.
The procedure for installation of TappingMode, single crystal silicon probe tips is
essentially the same as for contact AFM (see above paragraph). The substrate
should be face-up, with the probes cantilever pointing away from the AFM
tipholder. This ensures that the cantilever and tip are facing toward the sample once
the tipholder is mounted in the head. Refer to Chapter 4 for a description of the procedure to break out each substrate from the wafer.

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Handle probes with tweezers.

Apply gentle downward pressure to lift spring clip.

Spring clip

Locate probe flush against

inside edges of groove.
Figure 5.5. Slide the probe carefully into the tipholders groove. Gentle
downward pressure against the tipholder will lift the spring clip for probe
insertion.(Shown: underside of AFM tipholder.)

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Probe

Part II: Pre-Imaging Preparation

Wire clip

Lift wire clip by pressing

plunger on opposite side
of tipholder. Insert probe
with tweezers, then release
clip.

Figure 5.6. Fluid cell probe installation is similar to AFM/LFM tipholders.

Lift wire clip by pressing plunger on opposite side to insert probes.
(Shown: underside detail of fluid cell.)
To load a probe into the tipholder.
Refer to figure 5.6. Turn the tipholder upside down with the groove facing up as
shown. Apply gentle upward pressure against the plunger to lift the spring clip.
With the spring clip lifted, carefully slide the probe into the tipholder's groove until
it is located squarely against the innermost edges, then lower the spring clip by
releasing pressure against the plunger. This will hold the probe securely in the
tipholders groove. Check that the probe's substrate is flush with the back of the
groove and flat against one side (this keeps the probe's cantilever oriented in the
correct direction). If identical probes are loaded the same way each time, aiming the
laser onto the cantilever will be much quicker and easier.
CAUTION! The spring clip is extremely fragile and must be handled with great
care to prevent bending.
ATTENTION! Les embouts de ressort sont extrmement fragiles et doivent tre
manipuls avec une extrme prcaution.
WARNHINWEIS! Die Haltefeder ist sehr empfindlich und mu sehr vorsichtig
behandelt werden, um ein Verbiegen zu vermeiden.

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5.1.4. Install the tipholder.

Rotate clamping screw
CW (rear side of head)
to secure tipholder

(Rear view)
Clamping
screw

Figure 5.7. Install tipholder in head without touching the sample.

Secure tipholder using clamping screw at rear of head.
Once the tipholder is loaded with a probe (see Section 5.1.5 above), the tipholder is
placed inside the SPMs head and clamped into position. First, verify that the head
is sufficiently raised to clear the sample with the tip. (The top of the sample should
protrude no more than 1-2 mm above the plane of the heads bottom hole.) Insert
the loaded AFM tipholder into the MultiModes head by lifting the tipholder carefully over the sample. Do not touch the sample with the tipholder. Press gently forward, then lower the tipholder (figure 5.7).
Three precision ball mounts inside the head mate kinematically with the tipholders
underside. If the scanner cap has been properly positioned, the tipholder will come
to rest with the probe just above the sample surface. If the scanner cap is adjusted
too high, the tip will be plunged into the sample surface and broken. If it appears
the probe may crash when the tipholder is installed, remove the tipholder completely and use the tip Up toggle switch to obtain sufficient clearance. It is recommended that beginners practice with scrap probes and samples to learn proper
loading procedures.

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5.2. Laser Alignment

This section describes two methods for aligning the laser, mirror and photodiode
for all modes except STM. (STM does not use a laser.) The first method uses a
high-powered monocular magnifier (supplied with each MultiMode) to observe the
laser spots position on the cantilever. The second method uses a strip of paper to
observe the lasers position. The choice of method is largely a matter of personal
preference. Before beginning, verify that the mode switch on the MultiMode SPMs
base is switched to AFM & LFM or TM AFM. If the switch is toggled to STM,
the laser will be turned off.

5.2.1. Method 1: the magnifier method

This operation is performed using the high-powered monocular magnifier (shipped
with each MultiMode) or a similar magnifying system, under low light conditions.
First, the laser spot is positioned onto the cantilever. The photodiode is then positioned to maximize the signal and the spot is fine-adjusted onto the very tip of the
cantilever.
WARNING! Staring at a bright beam or reflection can result in eye damage. Be
sure that you are using a magnifier with a laser filter installed.
AVERTISSEMENT! Fixer un faisceau lumineux puissant ou sa rflexion peuvent
entrainer des dommages au niveau des yeux. Il est impratif dutiliser un filtre laser.
WARNUNG! Der direkte Blick in den Laserstrahl oder dessen Reflektion kann
Augenschdigungen hervorrufen. Bitte stellen Sie auf jeden Fall sicher, da ein
optisches Gert, mit dem Sie in den Laserstrahl schauen, mit einem Laserschutzfilter ausgestattet ist.
1. Position the magnifier (figure 5.8).
Using the 45X magnifier, focus on the cantilever substrate. There are two ways you
can do this. One way is to view the substrate from the side through the gap between
the cantilever mount and the bottom of the head shell. This is a useful vantage point
with the glass cantilever mount, as the edge of the substrate can be clearly seen.
Also, this is the same position used to view the cantilever-to-sample separation
when the tip is brought close to the surface; therefore the same magnifier position
can be used for both operations. With the metal cantilever mount, it is preferable to
do the alignment by looking down on the substrate from an elevated angle. Whichever viewing angle is used, the alignment process is the same.

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Figure 5.8. Two ways of positioning a magnifier when aligning the laser.
Through the heads front window (left), and overhead (right).
2. Identify the key features.
There are many laser light reflections, particularly from the tipholder, the sample,
and various metal surfaces. It is helpful to identify the key features before starting
the alignment. Make sure that the adjustment screws are positioned such that the
cantilever is well above the sample, so reflections off the sample do not make it
hard to locate the cantilever. Compare the view through the magnifier to the earlier
view of the cantilever.
3. Position the laser spot on the substrate.
The laser spot can be moved around with the two positioning knobs on the top of
the head. With the right-positioning screw, move the spot so it is on the cantilever
substrate. This is easy to see with the silicon nitride cantilevers because the glass
substrate will glow and there will be a lot of diffused red light scattered around the
internal area of the head.

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4. Find the cantilever with the laser spot (figure 5.9).

Y-axis adj.

While observing the substrate through the magnifier, slowly move the laser spot
lengthwise along the substrate with the X-axis positioning screw until the spot is
barely off the edge of the substrate (1). The laser spot may be visible on the sample
just off the substrate edge. With the rear-positioning screw, move the spot along the
edge of the substrate (2). Very small movements of the positioner are enough to
pass over the cantilever, so move slowly with small motions. Since the substrate is
mounted by hand, there is usually a small amount of angle between the substrate
and the axes of the positioners, so the best way to look for the cantilever is to make
small motions along the edge of the substrate and to move the spot back and forth a
little bit lengthwise for each small increment of edgewise motion. This way, it is
possible to stay adjacent to the edge without moving away from the substrate or
back onto it. In this fashion, move along the edge of the substrate. If a corner of the
substrate is reached without finding the cantilever, move back the other way.

1
Laser spot

X-axis adj.

Figure 5.9. Laser spot positioning.

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5. Position the laser spot on the tip of the cantilever.

With the silicon nitride cantilevers and a glass cantilever mount, a small bright red
dot appears to be hanging in mid-air right off the edge of the substrate when the
laser beam is on the cantilever. With the metal mounts with either cantilever, the
cantilever should be visible when the spot is near it. With very small motions of the
positioners, move the spot around on the cantilever until the spot is near the tip.

5.2.2. Method 2: The "paper" method

Some users prefer to align the laser by observing light patterns reflected or diffracted from the surface of the cantilever onto a piece of paper. This is known as the
"paper" method of laser alignment. Interpreting light patterns requires some experience, but is not especially difficult. The paper method can quickly verify with a
high level of confidence whether the laser spot is on the tip of the cantilever.

Figure 5.10. Paper method of laser alignment using

a slip of paper inside SPM head.
WARNING! To avoid eye damage due to high-level laser light, do not place highly
reflective or metallized objects into the head area while the laser is on.
AVERTISSEMENT! Pour prvenir tout accident au niveau des yeux, d la
lumire du laser, il est recommand de ne pas placer dobjet trs rflchissant ou
mtallique sous le faisceau laser lorsque celui-ci est allum.
WARNUNG! Um Augenschdigungen aufgrund von Laserlicht zu vermeiden
achten Sie bitte darauf, da keine reflektierenden oder mit Metall beschichteten
Gegenstnde im Bereich des AFM-Kopfes benutzt werden, solange der Laser
eingeschaltet ist.

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Inside the SPM Head

In this version of the paper method, the user inserts a narrow (1 cm wide) slip of
paper into the head and observes patterns reflected from the top side of the cantilever (figure 5.10). Once learned, this is a very quick method for obtaining laser
alignment. Because the slip of paper prevents light from reaching the photodetector,
the sum signal cannot be monitored while using this method.

Vertical adj.

Images on paper strip

1
Laser spot

Horizontal adj.

Figure 5.11. Directional control of laser spot using adjustment knobs.

Three spot locations are shown along with their resultant reflection
patterns.
1. Position the laser beam off the cantilever substrate (figure 5.12).
Look at the cantilever substrate through the large cutout in the front of the optical
head. Use the laser positioners on the top of the optical head to position the laser
beam off the end of the cantilever substrate. To be certain the beam is off of the substrate, vary the beam position in X until the laser light is reflected brightly from the
substrate, then turn the X-adjustment screw counterclockwise until the bright
reflection disappears. This may be easier to see if the cantilever is one or two millimeters above the sample surface. Insert a 1 cm wide slip of white paper in front of
the photodiode.

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Image on paper

Figure 5.12. Laser spot off probe and resultant reflection pattern.
Intensity may vary according to reflectivity of sample.
2. Position the laser beam in X (figure 5.13).
Position the laser beam so that a small amount of light is reflected from the edge of
the cantilever substrate. The purpose of this step is to position the beam such that
most of the laser light is falling off the end of the substrate; therefore, it is important
that the amount of reflected light be small.

Spot on end
of substrate

NOTE: if beam falls onto

top of cantilever, laser spot
will be intensely bright.

Image on paper

Figure 5.13. Locate the laser spot on the edge of the cantilever.

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3. Position the laser beam in Y.

Using the Y adjustment, move the beam parallel to the edge of the substrate while
looking for a reflection on the paper slip. Typically, the beam will reflect off both of
the legs of the silicon nitride cantilevers, so there will be two spots reflected which
may or may not show on the paper at the same time. In either case, the object is to
position the beam halfway between the two legs. Note that the separation between
the legs will be greater on the 200-m cantilevers than on the 100-m cantilevers.

Spot between
cantilever legs
near tip

Image on paper

Figure 5.14. Position the laser spot between cantilever legs.

Notes

The procedure is similar for the silicon cantilevers but because the cantilever is a
single beam, there will only be one laser spot reflected onto the paper.
4. Align the laser beam with the end of the cantilever (figure 5.15).
For silicon nitride cantilevers: move the laser beam out onto the end of the cantilever by turning the X adjustment counterclockwise while looking at the reflected
spot on the slip of paper. The spots reflected from the legs should merge into a single, well defined, bar-shaped spot. Verify that the laser beam is aligned with the end
of the cantilever by moving the beam back and forth in Y. If more than one reflected
spot is observed, then again position the beam between the two legs and move out
in X. Repeat until only a single, bright, well-defined spot is observed when the
position of the laser beam is varied in Y. If the reflected spot is dim or less well
defined, the laser beam may be improperly aligned. Attempting engagement under
these conditions may result in damage to the cantilever or sample.

Spot on tip
of cantilever

Image on paper

Figure 5.15. Alignment is complete when the laser spot is located

on or near the end of the cantilever.
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Head, Probe and Sample Preparation

Good images can usually be obtained any time there is a good bar-shaped pattern
reflected off the back of the cantilever; however, the following suggestions for finetuning the alignment of the laser spot position may enhance the image quality in
some cases. The position of the laser spot on the cantilever affects the sensitivity of
the cantilever deflection signal. The closer the spot is to the tip, the higher the sensitivity. However, the strength of the deflection signal decreases and optical interference problems increase as the laser spot is moved to the end of the cantilever,
because the cantilever is triangular in shape and the laser beam begins to spill off
the cantilever as the beam is moved towards the tip. This results in a trade-off
between signal strength and sensitivity.
Increased sensitivity is desirable when imaging atoms. So, when imaging atoms,
turn the laser diode X adjustment slightly counterclockwise to move the laser beam
closer to the end of the cantilever. Stop when the reflected bar-shaped pattern on the
piece of paper begins to shorten as the beam spills off the cantilever. It is important
to keep the entire laser beam on the cantilever when imaging samples with tall features. For these and most other samples, a good, solid, bar-shaped reflection on the
piece of paper provides the best results.)
For silicon cantilevers, the paper method will be slightly different because the silicon cantilever is a single beam rather than an open triangle (refer to figure 5.16).
The general method is as follows:
1. Locate the laser spot on the substrate.
2. Move the spot along the Y-axis to locate the center of the cantilever.
3. Move the spot off the substrate and onto the cantilever.
4. Locate the spot on the center of the cantilever.
5. Move the laser spot to the end of the cantilever.
Throughout the procedure, reflections from the cantilever can be interpreted on a
slip of paper. Use figure 5.16 below as a guide.

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5
~ 1/3 turn

Figure 5.16. Procedure for aligning silicon cantilevers using a slip of paper:
1) locate beam on substrate; 2) find center of substrate;
3) move toward cantilever; 4) locate cantilever;
5) find center of cantilever; 6) move to end of cantilever.
6. Align the photodiode with the reflected beam.
Contact AFM
Once the laser beam is aligned with the cantilever, it is necessary to position the
photodiode relative to the reflected spot. This is done by first adjusting the mirror
lever on the rear of the head, then adjusting the photodiode adjustment knob such
that the SUM signal displayed on the elliptical bar graph is maximized. This is a
much less sensitive adjustment than the laser beam alignment, so the maximization
need only be approximate. If the laser beam has been properly aligned, the maximized SUM signal should be over 4 volts with gold-coated silicon nitride cantilevers. If this is not the case, check the alignment of the laser beam.
TappingMode
For TappingMode: with the microscope toggled to TM AFM mode (the LED on the
face of the MultiMode base should be green), use the mirror lever on the rear of the
head and the photodiode adjustment knob to maximize the SUM signal displayed
on the elliptical bar graph, and zero the top/bottom differential signal which is
shown on the lower LCD display. If the range of movement of the photodiode stage
is inadequate to accomplish this, adjust the mirror angle with the lever in the back

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of the head. If the laser beam has been properly aligned, the maximized SUM signal should be 13 volts with a silicon cantilever. If this is not the case, check the
alignment of the laser-beam.
Projecting Diffraction Patterns with Head Removed (Newer Models Only)
Yet another "paper" method of laser alignment consists of removing the head and
interpreting diffraction patterns as light spills around the cantilever (figure 5.17).

Figure 5.17. Projecting diffraction patterns downward with head removed.

NOTE: Microscope shown is a MultiMode AFM, however, procedure
applies to all current models of small sample microscopes.

Notes

As a safety measure, all SPM heads are equipped with a cutout switch that
automatically turns off the laser when the head is moved (to prevent eye
damage). Early model heads feature a magnetic switch which turns off the laser
when the head is removed from the scanner. The method described here will
NOT work with these early model heads. Later models feature a mercury tilt
switch which allows the head to be removed from the scanner without turning
off the laser. Always handle the head with caution. DO NOT DROP!

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The projection method is very similar to the method described above using a slip of
paper. The patterns are also similar, but less distinct.

Figure 5.18. Various diffraction patterns projected on paper for

silicon cantilever. Patterns for silicon nitride cantilevers are similar.

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5.2.3. Maximize the SUM Signal

This section descibes what to do after the laser spot is aligned on the cantilever and
assumes knowledge of how to read voltages from the meters mounted on the front
of the MultiMode base. If you are unfamiliar with reading the MultiModes voltage
meters, skip ahead to section 5.4, then return to this section. Additional information
is provided in each of the various chapters on imaging.
After the laser beam is aligned on the tip of the cantilever using one of the methods
described above, move the mirror lever on the back of the head (figure 5.19) to
maximize the SUM signal. Next, adjust the photodiode positioner to set the output
signal to the desired value.
Photodetector mirror adj.
A-B signal
Y-axis

Tipholder clamping screw

X-axis

Photodetector mirror lever

(Front-Top View)
Photodetector mirror adj.
C-D signal
(Rear View)
Figure 5.19. Signals produced by the photodetector are optimized
using the heads various adjustments.
This adjustment is much less sensitive than the laser position adjustments. The
maximized value should be approximately 5.09.0 Volts for silicon nitride cantilevers. The value of this signal varies with many factors. It is important to note that it
is possible to see a large response on the elliptical bar graph without having the
laser beam on the cantilever, so it is important to visually verify that the laser beam
is on the cantilever and not rely on the elliptical bar graph alone. Attempting to
engage with the laser beam improperly aligned will usually destroy the cantilever.

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5.3. Start the Microscope Program

From the DOS prompt, change to the C:\SPM directory. Start the SPM microscopes Z.EXE program in C:\SPM by entering "Z." To proceed to the Real Time
functions, use the mouse to click on the Real Time icon on the tool bar.

5.3.1. Select microscope and scanner parameters.

This step needs to be completed only when your NanoScope system has more than
one micorscope or more than one scanner. Set the microscope head configuration
by using the mouse in the d / Microscope Select menu.
Microscope Select
AFM

Ok

STM

Edit

MultiMode
Extended MultiMode
EC AFM
EC STM

New
Delete
Cancel

Click on Ok using the mouse to close the Microscope Select dialog box.
Set the scanner configuration by using the mouse to select a scanner in the Microscope / Scanner menu.
Select Scanner
afmj
afmk

Ok

Cancel

TappingMode

For TappingMode, set the Microscope Mode to Tapping. This is done by clicking
on Microscope mode in the Other Controls panel. After this is completed, return
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Head, Probe and Sample Preparation

to the Scan Controls panel to access the most important control settings used for
imaging.
For contact AFM, set the Microscope Mode parameter on the Other Controls
panel to Contact. After this is completed, click on Scan Controls to again bring up
the most important control settings used for imaging.

5.4. MultiMode SPM Voltage Meters

A complete description of the signals coming into and out of the MultiMode SPM
is available in Support Note 210, NanoScope Signal Access Module (SAM)
Description and Use. The SAM is normally used for accessing these signals
directly. A brief description of the SPMs voltages and their interpretation using the
meters on the front of the base is provided here for quick reference.
The MultiMode SPM base is equipped with meters which indicate voltage coming
from the four-segment photodetector. The photodetector array is represented here:
Vertical deflection

B
A

Lateral deflection

Lateral deflection

C D
Vertical deflection

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The MultiMode SPMs bottom, elliptical (SUM) meter 1 indicates the total voltage
generated by the photodetector. That is, the combined voltage of photodetector segments. This is displayed during all modes (except STM when all meters are off).
TAPPING MODE
or CONTACT AFM
OUTPUT
SIGNAL (V)

SUM
1.2

12.0

(V)
10.8

DIFF.

3.6

VERTICAL
or HORIZONTAL
DIFFERENCE

8.4
4.8

6.0

7.2

SUM

The bottom digital meter 2 reads differences in voltage between various segments of
the photodetector. With the mode switch toggled to AFM & LFM, it indicates the
voltage difference (C - D), that is, the left segments minus the right segments. With
the mode switch toggled to TM AFM (TappingMode), it indicates the voltage difference (A - B), that is, the bottom segments minus the top segments.
The topmost digital meter 3 indicates the output signal of the SPM. Depending
upon the mode selected, the topmost meter reads either the (A - B) voltage difference (mode switch toggled to AFM & LFM), or the RMS voltage (mode switch
toggled to TM AFM).

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Chapter 6

Contact AFM

Contact AFM

6.1. Introduction to Contact AFM

This chapter covers procedures for operating the MultiMode SPM in contact AFM
mode. It is assumed the operator has previously prepared a contact AFM probe and
aligned the MultiMode head per instructions provided in Chapter 5 of this manual.
Specific information regarding tip preparation is provided in Chapter 4; Appendix
A of the Command Reference Manual contains further information regarding tips.

6.2. Preparation Prior to Imaging

6.2.1. Adjust the Detector Offsets
Verify that the MultiMode head has been fitted with a contact AFM probe tip per
instructions provided in Chapter 5 of this manual. The laser beam should already be
positioned on the back of the cantilever. This will provide a starting point for
adjusting the laser sum value.
To adjust the detector setting, first review the operation of the various adjustment
screws. The detector adjustment screws are at the left side of the head. The upperleft screw moves the laser spot up and down as shown on the computer screen
detector graphic, and side to side (long axis) on the dark red laser spot screen
directly on the SPM head. The lower-left screw moves the laser spot right-to-left as

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shown on the computer screen detector graphic and top-to-bottom (short axis) on
the dark red laser spot screen mounted into the SPM head.
Photodetector vertical adjustment knob
(A - B)

Tilt mirror lever

Photodetector horizontal adjustment knob

(C-D)
Figure 6.1. Photodetector mirror adjustmentsrear view.
Refer to figure 6.2. For laser aligning screws atop the SPM head, the right-front
screw moves the laser spot left-to-right (horizontally or along the X-axis). Turning
this screw clockwise moves the laser spot to the right. The left-rear laser aligning
screw moves the laser spot top-to-bottom (vertically along the Y-axis). Turning this
screw clockwise moves the laser spot rearward.

Notes

Use of the laser aligning screws to adjust the laser sum signal is NOT advised;
users should adjust the laser sum signal from the photodetector adjustments
only.

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Vertical adj.

For initial adjustment, center the spot on the cantilever as described in Chapter 5.

Horizontal adj.

Laser spot

Figure 6.2. Laser adjustment knobstop view.

6.2.2. Signal settings

In contact AFM mode, the vertical deflection (Vert Defl.) signal is used to provide
the dynamic feedback signal for surface height tracking. The horizontal deflection
(Horiz Defl.) is only used for lateral force measurements in contact mode LFM.
When disengaged in contact AFM mode and preparing for engagement, set the
detector Vert Defl. adjustment to between -3.0 and -2.0 Volts for (SiNi cantilevers)
or -0.5 and -1.0 (Si cantilevers). If performing LFM, set Horiz Defl. to -1.0 to +1.0
Volt. This is recommended for a 0.0 volt Setpoint.

Notes

Large offsets are not recommended between engage and disengage (2 volts)
with etched silicon cantilevers in contact mode (450m long only) because
breakage is likely. With etched silicon contact probes, it may be necessary to
reduce the offset between engage and disengage to a value of 1.01.5 volts.
The large difference is recommended for first-time use of silicon nitride
cantilevers.
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The difference between the vertical deflection before engage and the setpoint is
related to the force. A larger, more positive setpoint voltage results in a larger contact force.

6.2.3. Adjust tip height above sample surface

Next, use the adjustment screws to adjust the tips height just above the sample surface. The magnifier can be used to monitor the tip while this is done. The coarse
adjustment screws (if so equipped) are located in front and may be used to make
gross adjustments. The tip should be positioned just high enough to reach the surface when engaged, but not so low as to risk crashing into it. Use the motorized
screw to ensure the head is reasonably level. (This is not a problem on single-screw
scanners.)
One method employed to adjust the height of silicon nitride tips on noncritical samples is to very slowly lower the tip using the adjustment screws until a sudden
change is noted on the sum display of the MultiMode base. Most silicon nitride
cantilevers are flexible and, if lowered slowly and carefully, may be gently touched
to the surface without damage to either the tip or the surface. Watch for the change
on the elliptical sum signal display! When the sum signal change is noted, stop lowering immediately. The Tip Up switch may then be toggled briefly to lift the tip just
above the surface (the sum signal should resume its normal value). This method
works well on samples which are not delicate and which can be imaged without
concern for damage

6.3. Suggested Initial Control Settings

6.3.1. Initial Settings: Scan, Feedback and Other Controls panels
Before making changes to Scan Controls panel screen parameters, go to the Other
Controls panel (Panels / Other) and verify that the AFM Mode parameter is set to
Contact.
Click on Panels / Scan. Set the Scan size as large as desired (up to approximately
85-100 m with a "J" scanner) and set the X and Y offsets to 0.0. Set the Scan
angle to 0.0 degrees, Scan rate to 2-3 Hz (for single crystal silicon contact cantilevers 450 m long you may want to set this to 1.5-2 Hz). When starting, set the
Number of samples to 256 to expedite setup; later, the value may be increased to
512 for better image clarity. Make sure the Slow scan axis is Enabled. Set the Z
Limit to 440 volts (if not already set)

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Contact AFM

Next, click on Panels / Feedback. Set both Integral and Proportional gain to 2.0
each and the Setpoint to 0.0 Volts. The Feedback Controls screen should appear
as shown below.

Feedback Controls
Integral gain:

2.00

Proportional gain:

2.00

LookAhead gain:

0.00
0.00 V

Deflection Setpoint:

Figure 6.3. Feedback Controls settings for initial setup (contact AFM).

6.3.2. Other Controls Panel

Using the mouse, select Panels / Other. Verify that the AFM mode is set to Contact. Set Units to Metric, Color table to 2, and Input attenuation to 1x. (See
example below.)
Other Controls
Microscope mode:
Z limit:
Units:
Color Table:

Contact
2.000 m
Metric
2

Figure 6.4. Other Controls settings for initial setup (contact AFM).

6.3.3. Interleave Controls panel

Next, go to Interleave Controls by clicking with the mouse on Panels / Interleave. Verify that the Interleave mode field is set to Disabled. (Do not attempt to
set Interleave mode to Enabled at this point.)

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6.3.4. Channel 1, 2 and 3

On the Channel 1 panel, set Data type to Height (see below). Set Z range to a
reasonable value for the sample. (E.g., for the 180 nm step height calibration
sample a reasonable Z range setting would be 300 nm initially). Line direction can
be set to either Trace or Retrace. On the Channel 2 panel, set Data type to Off to
disable the secondary channel.
Channel 1
Data type:

Height

Data scale:

300 nm

Line direction:

Trace

Scan line:

Main

Realtime Planefit:

Line

Offline Planefit:

Full

Highpass filter:

Off

Lowpass filter:

Off

Figure 6.5. Channel 1 panel for initial setup (contact AFM).

6.4. Initiate the Engage Command

Go to the upper menu bar selection Motor, and click on Motor, followed by
Engage (or click on the Engage icon). A pre-engage check, followed by Z-stage
motor sound should be observed. If for any reason the engage aborts because the
SPM head is still too far away from the surface, click on the Abort button and
readjust the screws to start the tip closer to the sample surface. Assuming the tip is
better positioned before engaging again, an image should begin to appear on the
image monitor.
After good engagement is obtained, gradually reduce the setpoint offset (disengageminus-setpoint) to give a smaller contact force. A large offset between the setpoint
and disengaged signal is recommended during a first try, because sometimes there
are difficulties in engagement that can be reduced with a larger offset. On
subsequent engagements, try smaller signal offsets as confidence in use of the
instrument is gained.

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Contact AFM

6.4.1. Adjust Setpoint with Force Calibration

The most accurate way to minimize the Setpoint value is by using Force Calibration (Real Time / View / Force Mode / Plot). This consists of obtaining a force
plot, then adjusting the Setpoint value until the tip almost pulls free of the surface.
In this way, it is possible to minimize tip-sample forces and reduce wear on both the
tip and surface.
Getting a good Force Calibration plot.
Force plots are discussed in detail in Chapter 11 of this manual. For standard force
calibration plots, start with the following parameter values:

Panel
Z Scan Controls

Channel 1

Parameter

Setting

Scan Size

500 nm 1 ma

X offset

0.00 nm

Y offset

0.00 nm

Scan angle

0.00 deg

Scan rate

9.00 Hz

Number of samples

512

Average count

Display mode

Both

Trigger mode

Off

Start mode

Calibrate

Data type

Deflection

Z range

(Set to maximum)

a. A good Z-axis scan size is from 500 nm to 1 m. Scans larger than 1 m

may diminish details and make them hard to see. Scans smaller than 500 nm
may be too small and make it difficult to pull the tip clear of the surface.

What is happening?
The piezo is being retracted from the Z scan start position to the Z scan startplus-Scan size position. The Z scan start point is at the leftmost portion of the plot.
The Z scan start-plus-Scan size point is the rightmost portion of the plot. This corresponds to the Z Center Position that was being used while scanning just before
starting Force Calibration. This means that the Z scan start is recalculated at every
cycle to Force Calibration. The Scan size will be automatically changed if its value
is bigger than the difference between the Z Center Position and the fully retracted
position.

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Procedure
When you first enter forcecal the graph will probably look like this:

The tip is being moved up and down above the surface without touching it. If the
line is railed at the top or bottom of the image click on the Setpoint 0 button in the
Feedback Controls panel. Then you should see the above graph. To get it to touch
the surface you need to increase the Scan start. Doing this with an arrow key works
well. After a few key presses, you should see a graph similar to the one shown here:

If the line slants to the bottom of the graph and stays there, the tip is sticking to the
surface and not popping off the surface when the tip is fully retracted. To get the tip
clear of the surface, increase the Scan size until you can see it come off.

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Contact AFM

Now adjust the Setpoint for imaging. Having the setpoint anywhere above the line
where the tip is off the surface will work. The farther it is above, the more force is
placed onto the sample.

To adjust tip-sample force to the minimum amount, you can run in the area where
the tip is actually pulling up but the liquid layer is holding the tip on the surface.
However, this is not a stable way to image: if the tip pops free of the surface, the
Setpoint must be increased to reattach the tip.

To minimize tip-sample forces, lower the Setpoint until the tip pulls free of the surface and record the Setpoint value: this is the pulloff value. Increase the Setpoint
again to regain the surface, then lower the Setpoint to a point just above the pulloff
value. At this point, tip-sample forces should be at their minimum.
If Setpoint is the only parameter requiring adjustment, skip ahead to section 6.5
below; otherwise, go to the next section to adjust the SPMs Sensitivity parameter.

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6.4.2. Adjust Sensitivity (if required).

If imaging in Deflection mode instead of Height mode, adjust the detectors Sensitivity parameter to the cantilever as described in this section. Use the mouse to
draw a line parallel to the part of the plot where the tip is on the surface. To clear the
screen, click the mouses right button while in the graph.

Click and drag line parallel to sloped portion of plot.

If you want to see more graph range you can change the Input attenuation to 8x.
The graph will not change in appearance until you make the graph range larger. It
can now be made eight times larger. With this you can see the bottom of those big
pulldowns. Be sure to change the Input attenuation back to 1x before imaging.

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If there are periodic waves in the plot of the tip in free air, these are caused by optical interference. Some of this is acceptable but it can be bad enough to be a problem. The only way to fix this without changing tips is to adjust the aim of the laser.
This can be done while in Force Cal.

6.5. Beyond the Basics of AFM Operation

The above section provided a quick introduction to setup of the MultiMode microscope in the contact AFM mode. Although a great deal can be accomplished from
this starting point, there is far more to the operation of the AFM. More regarding
tip-sample interactions can be learned in Chapter 1 of the Command Reference
Manual. Section 11.2 in this instructional manual, "Contact AFM Force Plots,"
contains valuable information regarding the precise measurement of tip-sample
forces.
Cantilever selection is an important area and it will become more important as tip
and cantilever technology continues to develop. A clear understanding of the
parameters in the Real Time control panel allows the user to tune the microscope to
a wide variety of samples. Force mode imaging provides a great deal of information
if the user fully understands its nuances. For more information regarding force
mode imaging, see Chapter 11 in this manual.

6.5.1. Cantilever selection

Two basic cantilever configurations are available for the contact AFM mode. Traditional triangular silicon nitride cantilevers have been used successfully for years.
They are robust and relatively inexpensive. Etched silicon cantilevers with integral
tips provide another scanning option. They have a higher aspect ratio and a smaller
radius of curvature than the silicon nitride cantilevers.

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Silicon nitride cantilevers for this system are available in two process variations:
standard and sharpened. Usually, the standard silicon nitride cantilevers and resonant mode etched silicon probes are shipped with the MultiMode. Sharpened silicon nitride cantilevers have an almost identical appearance, but have slightly
sharper tips. Note that this system does not require the stand-alone type silicon
nitride probes which are used in some older, interferometric microscope heads;
however, they may still be used.
Each silicon nitride cantilever substrate includes four cantilever probes with different sizes and spring-constants. Two of the cantilevers on each substrate measure
115 m from the substrate to the apex of the triangular cantilever (these are referred
to as 100-m cantilevers) while the other two cantilevers measure 193 m from the
substrate to the apex of the triangular cantilever (these are referred to as 200-m
cantilevers). Both cantilever lengths are available with wide legs and narrow legs;
however, thickness of both cantilevers is the same. The calculated spring constants
for common cantilever configurations are listed below and in Appendix A of the
Command Reference Manual. These values are approximate; some variability will
occur. The tabulated values should be used to approximate the contact force unless
more accurate values are measured by the user.

Cantilever Type

k (N/m)
(narrow legs)

k (N/m)
(wide legs)

100 micron (triangular)

.38

.58

200 micron (triangular)

.06

.12

Table 6.1. Cantilever spring constants

The 100 m wide-legged cantilever can be used on most samples. If the image
degrades rapidly because the probe is damaging the sample surface, it may be beneficial to switch to a cantilever with a lower spring-constant. Cantilevers with
smaller spring-constants should be used on softer samples which will be destroyed
by imaging with high-contact forces.

6.6. Optimization of Scanning Parameters

Careful selection of the scan parameters is important to the successful application
of contact AFM. In most cases, the optimal parameter selection depends on the
sample. All parameters in the Real Time control panel are discussed in the NanoScope III Command Reference Manual. The user is encouraged to review these
descriptions carefully. This section analyzes the effects of the most important
parameters.

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Contact AFM

6.6.1. Data type

Data type is the first parameter to set because the settings of other parameters
depend on it. The Data type parameter in the Channel control panels selects the
type of data that is collected by the system. Height data corresponds to the change
in piezo height needed to keep the cantilever deflection constant. Deflection data
comes from the differential signal off of the top and bottom photodiode segments.
The Sensitivity parameter in the Force Mode Calibration panel must be determined, as described in the discussion of Force Calibration mode, before deflection
data is accurate.
The scan parameters required to collect good height data are different from the optimal parameters for deflection data. To collect height data, the feedback gains must
be high so that the tip tracks the sample surface with minimal cantilever deflection.
The position of the piezo during the scan reflects the height of the sample. Deflection data should be collected with low feedback gains so the piezo remains at a constant position relative to the sample. In this case, the tip and cantilever will be
deflected by the features on the sample surface. The output fluctuations in the cantilever deflection voltage from the top and bottom photodiode segments are recorded
as a measure of the variation in the sample surface. To collect accurate topographical data, the Data type parameter should be set to Height in most instances.
Deflection data collected with high feedback gains is essentially the derivative of
the height. This is commonly referred to as the error-signal mode. The error-signal
mode provides a sensitive edge-detection technique. Using dual screen mode, it is
possible to capture both Height and Deflection data simultaneously.

6.6.2. Gain settings

The Integral, Proportional, and LookAhead gains in the Feedback Controls
panel control the feedback on the piezo height. The feedback loop tries to keep the
deflection signal constant by adjusting the height of the piezo tube. If the gains are
high, as they should be for Height data, the piezo height will change to keep the
cantilever deflection nearly constant. If the gains are low, as they should be for
topographical Deflection data, the cantilever will deflect from its nominal position
as features in the sample are encountered. In general, the Integral and Proportional gain can be set to 23 to start scanning. To optimize the gains for height
data, increase the Integral gain until the piezo begins to oscillate, then eliminate
the oscillations by reducing the gain with two or three clicks of the left-arrow key.
Repeat the process for the Proportional gain. Piezo oscillations typically cause
high frequency wavy lines in the Real Time image. For deflection data, engage the
microscope with the gains high, then lower them as much as possible once the system is scanning.

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The LookAhead gain includes information from the previous scan line to determine the current gain setting. It should only be used on samples with step-like features which are oriented perpendicular to the fast scan direction. Otherwise, it
should be left at 0.

Notes

LookAhead gain controls are not implemented on some software releases. For
more information, contact Digital Instruments software department.

6.6.3. Scan size and Scan rate

In general, the Scan rate must be decreased as the Scan size is increased. Scan
rates of 1.52.5 Hz should be used for large scans on samples with tall features.
High scan rates help reduce drift, but they can only be used on very flat samples
with small scan sizes.

6.6.4. Setpoint
The Setpoint parameter defines the desired voltage (and, therefore, the desired
deflection of the cantilever) for the feedback loop. The setpoint voltage is constantly compared to the present photodiode cantilever deflection voltage to calculate the desired change in the piezo position. When the gain values are high, as they
should be when the Data type is set to Height, the Z piezo position changes to keep
the photodiode output signal close to the Setpoint; therefore, the cantilever deflection remains nearly constant. When the gain values are low as they should be when
the Data type is set to Deflection, the piezo height does not change, and the photodiode signal varies around the Setpoint value.
In contact AFM, increased Setpoint yields higher tip-sample forces. The Setpoint
can be adjusted to increase or decrease the cantilever deflection and, therefore, the
contact force of the tip on the sample. The Force Calibration command in the Real
Time / View menu allows the setpoint to be adjusted while viewing a graph of the
tip position versus the deflection voltage. Using this procedure, which is described
in detail in the next portion of this section, the contact force of the tip on the sample
can be minimized. This is especially important on soft materials such as biological
samples.

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6.6.5. Lowpass filter

The Lowpass filter invokes a digital, one-pole, lowpass filter to remove high-frequency noise from the Real Time data. The filter operates on the collected digital
data regardless of the scan direction. Settings for this item range from Off through
9. Off implies no lowpass filtering of the data, while settings of 1 through 9, successively, lower the cut-off frequency of the filter applied to the data stream.

6.6.6. Highpass filter

The Highpass filter parameter invokes a digital, two-pole, highpass filter which
removes low frequency effects, such as ripples caused by torsional forces on the
cantilever when the scan reverses direction. As with the Lowpass filter, it also
operates on the digital data stream regardless of scan direction. This parameter can
be Off or set from 1 through 9. Settings of 1 through 9, successively, lower the cutoff frequency of the filter applied to the data stream. It is important to realize that in
removing low frequency information from the image, the Highpass filter distorts
the height information in the image. As a result, this filter must be Off when accurate height information is desired. The Highpass filter is usually used only for
atomic images.

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Chapter 7

Contact AFM in Fluids

7.1. Fluid OperationOverview

An ever-increasing realm for SPM technology is the imaging of samples in fluid.
This may be prompted from a desire to minimize surface forces on delicate samples, the need to observe biological specimens in their natural, fluid environments,
and/or the necessity to make real time observations of samples undergoing electrochemical reactions (ECAFM). In order to conduct ECAFM observations with electrical potentials, it is necessary to connect an external potentiostat unit. For more
information, contact Digital Instruments.
CAUTION! When imaging fluid samples, use extraordinary precautions against
spillage. Fluids must NOT be spilled on or around the sample stage, electronic
boxes, or other components containing electronic parts. Avoid spilling all corrosive
fluids on exposed surfaces; otherwise, damage may result! In the case of a spill,
immediately clean and dry all affected surfaces carefully.
ATTENTION! En milieu liquide, prendre toutes les prcautions pour viter une
fuite qui pourrait atteindre la platine porte -chantillon, le boitier lectronique ou
tout autre partie lectronique du microscope. Eviter tout contact avec un liquide
corrosif.
WARHINWEISS! Falls Sie Proben in Flssigkeiten abbilden, lassen Sie uerste
Vorsicht walten, damit keine Flssigkeit verspritzt wird. Flssigkeiten drfen nicht
auf die oder nahe der Probenhalterung, der Elektronikbox oder anderen Komponenten, die elektronische Bauteile enthalten, verspritzt werden. Vermeiden Sie bitte,
korrosive Flssigkeiten auf freiliegende Oberflchen zu verspritzen; andernfalls
wren Beschdigungen die Folge! Falls Sie Flssigkeit verspritzt haben, subern
und trocknen Sie alle betroffenen Flchen sorgfltig.

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Essentially, the procedure for observing samples under fluid is the same as that for
contact AFM in air; however, special hardware is utilized to contain the fluid. In
addition, minor adjustments must be made to correct for refractive effects as the
laser beam transits air-fluid boundaries. One feature of imaging samples under fluid
is that attractive forces due to surface tension effects are eliminated. This enables
the sample surface to be imaged with a minimum of cantilever tip forcea decided
advantage when imaging biological specimens and delicate materials.
Images of submerged samples may be obtained in TappingMode; however, the
drive frequency and amplitude of the cantilever must be reduced due to viscous
damping of the fluid. For more information, see Chapter 8. Chapter 8 includes a
procedure (section 8.8.3 ) that should be studied for all types of fluid imaging.
This section describes contact AFM operation of the MultiMode SPM in fluid,
including loading the cantilever into the tipholder, mounting the tipholder into the
head, aligning the laser onto the cantilever and then engaging the tip with the sample. There is also a discussion of methods of preparing the sample for fluid operation. This section assumes familiarity with contact AFM operation of the
MultiMode in air. If you are not familiar with air operation of the MultiMode,
please first follow the procedures outlined in Chapter 6 before attempting to operate
the AFM under fluid.

7.2. Fluid OperationHardware

IMPORTANT: Do not attempt to operate the standard air tipholder in a fluid environment. Standard tipholders have exposed electrical signal lines that could short
circuit if exposed to a conducting fluid.
ATTENTION: En milieu liquide, ne pas utiliser le support de bras de levier standard prvu pour une utilisation lair. Le support de bras de levier standard comporte des fils lectroniques non protgs qui peuvent provoquer un court-circuit en
cas de contact avec un liquide conducteur.
WARNHINWEISS: Versuchen Sie nicht, den Standard-Luft-Cantileverhalter in
Flssigkeiten zu betreiben. Am Standard-Cantileverhalter liegen elektrische Leitungen frei, die in leitfhigen Flssigkeiten kurzgeschlossen werden knnten.

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Fluid imaging requires a special tipholder (Figure 7.1). The fluid tipholder interchanges with the standard tipholder in a matter of a few minutes.

Figure 7.1. Fluid (TappingMode) Tipholder in Case

The fluid tipholder consists of a small glass assembly with a wire clip for holding
an AFM cantilever substrate. The glass surfaces provide a flat, beveled interface so
that the AFM laser beam may pass into the fluid without being distorted by an
unstable fluid surface.

7.3. Notes on Sample Mounting

In many cases, it may be desirable to image a sample under a drop of fluid without
use of a closed fluid cell. Simply attach the sample to a 12 mm puck, then put the
drop of fluid onto the sample and lower the AFM fluid tipholder into the drop.
Without the o-ring, this approach poses a potential spill hazard to the microscopes
electronics and must always be undertaken with extreme caution. To help protect
the scanner, always use the large size (12 mm) puck. If the sample surface is hydro-

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phobic, it should hold a fairly substantial droplet without difficulty. If the sample
surface is hydrophilic and/or porous, it may tend to absorb fluids and wet the scanner. In this case, it will have to be encapsulated within a fluid cell.
Fluid tipholder
Sample
Sample puck
Scanner

Figure 7.2. Imaging a Sample Covered by a Drop of Fluid

Attach the sample rigidly to the puck. Samples may be secured to the puck with
adhesive tape or epoxy. For non-critical applications, Devcon 2-Ton Epoxy works
well. For applications where contamination control is more critical, try a more
inert, solvent-free epoxy like Master Bond EP21LV or EP21AR (phone number
201-343-8983) or various hot melt adhesives. Be sure to follow the manufacturer's
directions for mixing and curing to obtain the best resistance to leaching and chemical attack. For lower-resolution applications where it is also desirable to image a
sample quickly without waiting for an adhesive to cure, you may find it sufficient to
hold the sample to the sample holder using double-sided tape. We recommend
against using any cyanoacrylate glue (like Superglue) for mounting samples in
fluid.
CAUTION! When imaging fluid samples, use extraordinary precautions against
spillage. Fluids must NOT be spilled on or around the sample stage, electronic
boxes, or other components containing electronic parts. Avoid spilling all corrosive
fluids on exposed surfaces; otherwise, damage may result! In the case of a spill,
immediately clean and dry all affected surfaces carefully.
ATTENTION! Lors dun travail en milieu liquide, prendre toute prcaution pour
viter des fuites. Les liquides ne doivent pas se rpandre sur la platine porte chantillons, le botier lectronique ou toute autre partie du microscope contenant de
llectronique. Eviter toute fuite de liquide corrosif sur les surfaces exposes. Le
non respect de cette recommandation peut entraner des dommages. En cas de fuite,
nettoyer et scher immdiatement les surfaces touches.
WARHINWEISS! Falls Sie Proben in Flssigkeiten abbilden, lassen Sie uerste
Vorsicht walten, damit keine Flssigkeit verspritzt wird. Flssigkeiten drfen nicht

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Contact AFM in Fluids

auf die oder nahe der Probenhalterung, der Elektronikbox oder anderen Komponenten, die elektronische Bauteile enthalten, verspritzt werden. Vermeiden Sie bitte,
korrosive Flssigkeiten auf freiliegende Oberflchen zu verspritzen; andernfalls
wren Beschdigungen die Folge! Falls Sie Flssigkeit verspritzt haben, subern
und trocknen Sie alle betroffenen Flchen sorgfltig.

7.4. Fluid OperationProcedure

7.4.1. Load the Fluid Tipholder with a Cantilever Substrate
The cantilever substrate is held in a small pocket on the bottom side of the tipholder
by a gold-plated, stainless steel wire clip. The wire clip is held against the cantilever
substrate by a tiny coil spring mounted on the top of the tipholder. To load a cantilever substrate into the holder, turn the tipholder upside down and gently lift the wire
clip upward by pressing from beneath. With the wire clip raised, slide a cantilever
substrate under the wire and into the pocket. Check that the cantilever substrate is
squarely set against one side of the pocket and flush against the back. Avoid
scratching the tipholder's glass surface with the tweezers or the cantilever substrate,
especially in the area under the cantilever itself. Check that the cantilever substrate
is held firmly by the wire.

7.4.2. Install the Tipholder on the Microscope Head

Verify that the sample is attached firmly to a 12 mm puck and loaded atop the scanner. The head must be raised adequately to clear the sample with the tip. If the head
is positioned too low, toggle the tip Up switch and use coarse adjustment screws to
raise the head adequately. Insert the tipholder carefully into the head, careful not to
contact the sample.

Figure 7.3. Tipholder Inserted into Microscope Head

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7.4.3. Align the laser

Laser alignment is accomplished by either of the procedures described in Chapter 5
in this manual. Note that alignment of an immersed cantilever is slightly different
than in air, since refractive effects cause the beam path to bend slightly. The basic
process is essentially the same, however. The following instructions give an abbreviated procedure, focusing on the differences or additional techniques required for
fluid operation.

7.4.4. Watch Out for False Reflections

The fluid tipholder is constructed such that the cantilever substrate rests flat on an
angled, glass surface. The angled glass surface produces a false laser reflection,
even when the laser is not aimed at the cantilever. This reflection from the glass surface does not affect operation of the MultiMode, but it can be a source of confusion
when aligning the laser on the cantilever. Ignore this fainter reflection and watch
instead for the much brighter reflection from the cantilever.
False reflection from glass (faint)
Reflection from
cantilever (bright)

Laser beam

Fluid tipholder (glass)

O-ring

Sample
Sample puck
Scanner

Figure 7.4. False Reflections from Bottom Surface of Fluid Tipholder

Note that the SUM signal on the display monitor will typically show less than 1 V
when the laser is not yet aligned on the cantilever. The SUM signal should rise well
above 1 V when the laser is reflecting off the cantilever.

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7.4.5. Align the Laser on the Cantilever

Now use either of the techniques for aligning the laser onto the cantilever that are
discussed in Chapter 5 of this manual. Initially, most users find using the optical
magnifier the easiest.

7.4.6. Install the Protective O-ring and Flood the Fluid Chamber
The o-ring is used to protect the SPM scanner tube from spilled liquids. It should be
inserted into the gland (recessed groove) which is ground into the underside of the
tipholder. The o-ring is designed to slide up into the gland as the tipholder is lowered until the tip accesses the sample surface.
Fill a syringe with the fluid to be used for imaging, then chase out all air bubbles.
(Injected air bubbles can become trapped inside the fluid chamber and disrupt
imaging.) Connect the syringe to the inlet tubing on the tipholder. The outlet tube
should be connected to a container where fluid can drain. Push enough fluid
through the fluid chamber to flood it completely, but do not clamp the outlet tube.

7.4.7. Lower Tipholder into Fluid

Carefully tighten the clamping screw to secure the tipholder, making certain that
the o-ring is positioned properly between the sample and tipholder. If the o-ring
attempts to shift off, remove the tipholder and try repositioning the o-ring. If shifting continues, see Chapter 15 in this manual for help. Try clamping the outlet tube.
Clamping is not necessary and may effect noise in the image.

7.4.8. Readjust Laser Aiming (If Required)

The presence of fluid may cause the laser spot to refract slightly, requiring slight
readjust of the laser aiming screw to move the laser spot back onto the end of the
cantilever.
Occasionally, air bubbles will become trapped near the cantilever which interfere
with the laser beam's optical path. If this occurs, it may be impossible to get a good
reflection from the cantilever after flooding the tipholder with fluid. In this case, use
the syringe to force liquid quickly through the cell to try to break the bubbles loose
from the tip.

7.4.9. Adjust the Detector Offsets and Setpoint

Turn the detector mirror adjustment screws to center the laser spot on the laser
detector as described in section 3.3.1. Typical starting conditions might be to set the
vertical deflection signal to roughly -1.0 V and the Setpoint to 0 V. Bear in mind
that the difference between the vertical deflection before engaging and the setpoint
is related to the amount of force that the cantilever probe tip applies to the sample.
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Typically, samples are softer in liquid than in air, so be careful that there is not too
large a difference between the setpoint and the vertical deflection signal before
engaging. Also, it may be desirable to reduce the setpoint once engaged to obtain
minimum tracking force.

7.4.10. Check Scan Parameters

Check that the various scan parameters such as Scan rate, Scan size, Integral gain
and Proportional gain, etc. are reasonable.

7.4.11. Engage the Surface

While monitoring closely through the 25X magnifier, use the coarse adjustment
screws and motor Down switch (on the MultiMode base) to bring the tip just above
the level of the sample surface. Under the Real Time / Motor menu, click on
Engage (or click on the Engage icon). The motor will begin to move the SPM head
and probe down towards the sample. When the cantilever reaches the surface, the
system should automatically stop, beep, and then begin to image the sample. In the
event that the system engages immediately or before the tipholder actually reaches
the surface, try increasing the Setpoint approximately 2.0 Volts, then try again.
If other difficulties are encountered, see the Troubleshooting section of this manual.

7.4.12. Adjust Scan Parameters

Once engaged, adjust the scan parameters to obtain the best image. This procedure
will be similar to operation in air except for the following cautions:
1. Samples are often softer in fluid and so adjusting the applied force can be much
more critical. To avoid sample damage, adjust the Setpoint as low as possible. To
do this reduce the setpoint using the cursor keys until the cantilever pulls off the
surface and the Z Center Position on the display monitor jumps to Limit (-220 V).
Increase the Setpoint slightly until the cantilever begins to touch the surface again
and an image appears. Another way is to use the Force Calibration command to
select the Setpoint and estimate the contact force, as described in Chapter 11. Note
that since the cantilever will typically adhere to the sample surface much less in
fluid, it is often possible to image at much smaller contact forces in liquid than in
air.
2. The optimal Integral and Proportional gains and Scan rate may be different
from air operation since the dynamics of the cantilever will change in fluid. Set the
two gains as high as possible (starting with the Integral gain) without causing
oscillations to appear in your image. Choose a Scan rate that is sufficiently slow to
image without distorting your data.

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7.4.13. Clean and Dry Parts When Done

When sample imaging is complete, drain the fluid tipholder and carefully remove it
from the head while avoiding spills. Rinse and dry the tipholder and o-ring to prevent the buildup of salts or other contaminants on these parts. When cleaning the
tipholder, take great care to avoid scratching the glass surfaces in the center of the
tipholder.

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MultiModeSPM Instruction Manual

Chapter 8

TappingMode AFM

TappingMode

8.1. Introduction to TappingMode AFM

This chapter covers procedures for operating the MultiMode SPM in TappingMode
for both air and in fluids (section 8.8). It is assumed that the operator has previously
prepared a TappingMode probe tip and aligned the SPM head per instructions provided in Chapter 5 of this manual. Additional information regarding cantilever
preparation is provided in Chapter 4.

Note:
TappingMode is disabled for users of NanoScope E configurations.

8.2. Basic Principle of TappingMode

Figure 8.1 represents a cantilever oscillating in free air at its resonant frequency. A
piezo stack excites the cantilevers substrate vertically, causing the tip to bounce up
and down. As the cantilever bounces vertically, the reflected laser beam is deflected
in a regular pattern over a photodiode array, generating a sinusoidal electronic signal. The signal is converted to a root mean square (RMS) amplitude value, which is
displayed in AC volts on the topmost ("TappingMode Output Signal") meter
located on the front of the MultiMode base.
Figure 8.2 represents the same cantilever at the sample surface. Although the piezo
stack continues to excite the cantilevers substrate with the same energy, the tip is
deflected in its encounter with the surface. The reflected laser beam ("return sig-

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nal") reveals information about the vertical height of the sample surface and some
characteristics of the sample material itself. These material characteristics may
include elasticity ("hardness"), magnetic and/or electric forces present.

Laser beam

Return signal
Cantilever

Figure 8.1. Tapping cantilever in free air.

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TappingMode AFM

Laser beam
Return signal
(deflected)

Sample surface

Figure 8.2. Tapping cantilever on sample surface.

Note deflection of cantilever and return signal (exaggerated).

8.3. Preparation Prior to Imaging

8.3.1. Switch to TappingMode and check parameters
The microscope must be switched to TappingMode. Go to the Real Time / Other
Controls panel and set the AFM mode parameter to Tapping. Toggle the selector
switch on the left side of the MultiMode base to TM AFM; the tiny LED indicator
on the front of the base should glow green.

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Check that the Real Time control panel parameters are set within reasonable limits
for TappingMode operation. If you are uncertain what parameter settings to start
with, try the values below:

Panel
Scan Controls

Feedback Controls

Parameter

Setting

Scan Size

25 m

X offset

0.00 nm

Y offset

0.00 nm

Scan angle

0.00 deg

Scan rate

1.00 Hz

Number of samples

256

Slow scan axis

Enabled

Z limit

440 V

Integral gain

0.300
(V)
10.8

3.6

Proportional gain

0.300

LookAhead gain

0.00

Setpoint
6.0

Other Controls

Interleave Controls

8.4
7.2

Drive frequency

200400 kHzb

Drive amplitude

50800 mV

AFM mode

Tapping

Input attenuation

1x

Engage Setpoint

1.00

Interleave mode

Disabled

a. Setpoint is initially set by the software during engagement. It may

be adjusted up or down afterward.
b. The Drive frequency varies according to the length and stiffness
of each cantilever. TappingMode cantilevers are shipped in boxes
stamped with their resonant frequency. The Drive frequency
should be set close to ( 50 kHz) this value.

8.3.2. Adjust laser and photodetector

Verify that the tipholder has been fitted with a TappingMode, single crystal silicon
probe and aligned per instructions provided in Chapter 5 of this manual. Photodetector voltage values are displayed on meters mounted on the front of the MultiMode base. The laser photodetector is adjusted using the photodetector adjustment
knobs on the left-top and left-rear of the head (see Figure 8.3 below). Recall that

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TappingMode AFM

RMS amplitude is an AC signal which does not have any real meaning until cantilever tuning is completed (see section 8.3.3). The laser spot will need to be approximately centered prior to entering the Cantilever Tune routine.
Photodetector adjustment knobs.

Photodetector output
signal (RMS AC volts).
This value is directly
influenced by the
Drive amplitude
parameter when tip
is at resonance.
Sum signal. This
value changes
according to how
much of the beam
falls on the
photodetector.

SUM
1.2

12.0

(V)
10.8

DIFF.

3.6

8.4
4.8

6.0

7.2

Deflection voltage. This

changes according to
how beam is centered
vertically. At 0.00 Volts
beam is centered.

Figure 8.3. Photodetector adjustment knobs and SPM voltage meters.

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Small laser signal amplitude

yields low output voltage.

SUM
1.2

12.0

(V)
10.8

er
Las

nal

sig

DIFF.

3.6

8.4
4.8

6.0

7.2

Sum voltage low due to

low amplitude laser signal
and/or misalignment.

Vertical voltage difference

high because laser signal
falls on bottom half of
photodetector only.

Larger laser signal amplitude

yields higher output voltage.

SUM
1.2

12.0

(V)
10.8

gna

r si

e
Las

DIFF.

3.6

8.4
4.8

6.0

7.2

Sum voltage higher due to

stronger laser signal (increased amplitude). All of
beam falls on photodetector.

Well centered laser

beam yields a vertical
voltage difference of zero.

Figure 8.4. Voltage meters on the MultiMode base reveal a great deal
about the amplitude and alignment of the TappingMode laser signal
on a tuned tip operating at its resonant frequency.

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TappingMode AFM

8.3.3. Additional preparations

In TappingMode, the AC voltage signal representing RMS amplitude is used to provide the dynamic feedback signal for surface height tracking. The vertical deflection signal (displayed on the "Vertical or Horizontal Difference" meter) should be
close to zero ( 1.0 V) prior to running Cantilever Tune and/or attempting engagement. If you are uncertain how to set parameters for the Channel 1 panel, try the
following settings:

Panel
Channel 1

Parameter

Setting

Data type

Height

Z range

04.50 ma

Line direction

Trace

Scan line

Main

Real-time Planefit

Line

Off-line planefit

Full

High-pass filter

Off

Low-pass filter

Off

a. A Z range value of 4.50 m is the maximum for most "J" scanners.

Always start with a low Z range value if feature height is
unknown, then increase until the image is optimized. On the 180
nm step height calibration sample, a reasonable Z range setting
would be 300 nm initially

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8.3.4. Tune the cantilever

This section describes steps required to find the resonance peak of the cantilever
and adjust the oscillation voltage so the cantilever will vibrate at an appropriate
amplitude. A range of vibration frequencies will be applied to the cantilever to
determine the frequency which produces the largest response (the resonance frequency). In most instances, the resonance peak will have a sharp Gaussian distribution but sometimes the peak can be somewhat ragged. The system will tolerate
some deviation in the shape of the peak.
1. Click on View / Sweep / Cantilever Tune, or use the Cantilever Tune icon. Several panels will appear...
Auto Tune Controls
Auto Tune Controls
Start frequency:

100.000 kHz

Target amplitude:

End frequency:

500.000 kHz

Peak offset:

2.000 V
0.00 %

Auto Tune

Sweep Controls
Graph Controls

Main Controls

Sweep width:

400.000 kHz

Amplitude setpoint:

Drive frequency:

300.000 kHz

Drive amplitude:

0.00 V
300 mV

256

Sweep sample count:

Motor

Interleave Controls

...while the Frequency Sweep ((a plot of cantilever response as a function of

applied vibrational frequency) is shown on the display monitor. The two main panels, Sweep Controls and Auto Tune Controls, allow the operator to either manually or automatically tune the cantilever. For most purposes, the Auto Tune function
will suffice. To tune the cantilever automatically, simply click on the Auto Tune
button; the computer and controller will do the rest, setting such parameters as Setpoint and Drive amplitude automatically.
At times, it may be useful to tune the cantilever manually, for example, to purposefully offset the drive frequency above or below the resonant frequency as is often
done during MFM and EFM imaging.

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TappingMode AFM

Note:
More than one type of cantilever exists. Different types have different dimensions
and therefore different resonance frequencies. Check the box used to ship the cantilever to see what its resonant frequency is, or refer to Appendix A in the Command
Reference Manual.
Tuning cantilevers manually
The parameter values, especially the drive frequency and the sweep width, given in
the following example apply to one type of cantilever. The nominal parameter values may vary depending upon the actual cantilever used.
For initial set-up, the Sweep Controls screens should be set to the values shown in
the example below.
Sweep Controls
Graph Controls

Main Controls

Sweep width:

400.000 kHz

Amplitude setpoint:

Drive frequency:

300.000 kHz

Drive amplitude:

0.00 V
300 mV

256

Sweep sample count:

Motor

Interleave Controls

Sweep Controls
Graph Controls

Interleave Controls

Sweep width:

400.000 kHz

Amplitude Setpoint:

Drive frequency:

300.000 kHz

Drive amplitude:

0.00 V
300 mV

256

Sweep sample count:

Motor

Main Controls

Figure 8.5. Sweep control panels for Main Controls (top) and Interleave
Controls (bottom).

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2. Set parameters in the Sweep Controls panel as follows:

Set the Drive frequency parameter to a value near the center of the range of the
resonance frequencies specified for the cantilever. For example, if the frequency
range is specified as 240420 kHz, select a drive frequency of 330 kHz.

Start with a Drive amplitude of about 300 mV. It is possible to detach the
cantilever from the substrate by applying too large of a drive amplitude;
therefore, it is important to exercise some caution when adjusting the Drive
amplitude parameter. Note that the Drive amplitude is reset automatically by
the Auto Tune command.

Set the Sweep width to about the same value as the Drive Frequency, or at
least some value large enough to cover the frequency range specified for the
wafer.

Zero the Amplitude Setpoint. Note that the Amplitude Setpoint will be reset
automatically by the Auto Tune command.
3. If a peak in the frequency response plot does not appear, perform the following
steps:

Increase the Drive amplitude to 600 mV.

Increase Sweep width to the maximum value.
If the peak still has not appeared, then increase the Sweep width by first increasing
the Drive Frequency, then maximizing the Sweep width. If there is still no peak
on the response plot, check the laser alignment.
4. After identifying the maximum amplitude peak with the lowest frequency in the
frequency response plot, center the peak on the frequency sweep plot shown on the
display monitor. This is most easily accomplished with the Zoom In and Offset
subcommands in the menu bar of the display monitor. The Offset subcommand
shifts the plot by setting the center frequency equal to the cursor position. The
Zoom In subcommand stretches the plot by decreasing the sweep width and shifting the center frequency value.
If the top of the resonance peak is off the plot, increase the Amplitude Setpoint
until it appears. Continue to Zoom In and center the peak until the peak coincides
with the vertical center line within about 10 Hz. The value displayed for center frequency is now used as the resonant frequency of the cantilever.

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TappingMode AFM

In reality, the system will work well in TappingMode if the drive frequency is at, or
below, the peak in the resonance plot. The Drive Frequency can be decreased to
the point where the vibrational amplitude reaches 90 percent of the maximum
value. It is often preferable to operate at a frequency lower than the resonant frequency due to shifting of the resonant frequency upon approach of the tip to the surface.

8.3.5. Setting the Drive amplitude and Setpoint

After tuning the cantilever to its resonant frequency, the free-vibration amplitude
must be specified. The desired operating amplitude depends on the sample, and
other scanning conditions.
Prior to engagement, the Amplitude Setpoint parameter is used to scale the cantilever response (vertical) axis of the frequency sweep display graph. It does not
actually adjust the operating feedback setpoint, since the computer automatically
determines the initial engagement setpoint during engagement.
Only after engagement does the Setpoint parameter in the control panel define the
operating amplitude to be maintained by the feedback loop. Perform the following
operations to adjust the oscillation drive amplitude and the frequency sweep graph
vertical axis scaling.
1. Increase the Drive amplitude until the peak amplitude in the Frequency Sweep
plot reaches the desired amplitude. A good amplitude would be 13 volts. In general, the peak amplitude will reach 3 volts with the drive amplitude set to under 500
mV.
The amplitude value can be determined by adjusting the amplitude setpoint value
until the center frequency crosses in the middle (horizontally) of the cantilever tune
graph. You can also Quit the Cantilever Tune menu and adjust the Drive amplitude until the RMS value is appropriate. The actual setpoint value adjusted by the

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user prior to engage is meaningless because the operating setpoint is determined

automatically during engage by the control program.

Frequency Sweep
Cantilever
Response
0.50 V/div

Setpoint

DriveFrequency - 337.8723 KHz

Center
0.05 KHz/div

Figure 8.6. Sample starting control point.

2. Click on Quit and the parameters set in the Cantilever Tune control panel will
now appear in the Feedback Controls panel. The value of the RMS amplitude displayed on the laser signal display will now hold steady at the amplitude that coincided with the selected Drive frequency. After the microscope is engaged, the
RMS amplitude value displayed on the display monitor will match the Setpoint
parameter specified in the Feedback Controls panel.

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8.4. Engaging The Microscope

After cantilever oscillation has been adjusted and the operating point is defined, the
microscope is nearly ready to engage. The following items remain to be done:
1. Recheck all control panel parameters. For the calibration standard, set control
panel parameters as shown in Figure 8.7. The feedback gains and the scan rate are
the most important parameters. Start with the Integral gain set to 0.50 and the Proportional gain set to about 1.20 and set the LookAhead gain (if supported) to
zero. The scan rate should be set below 2 Hz. Verify that Input attenuation is set at
1x on the Other Controls panel before imaging.
Scan Controls Settings
Scan Controls
Scan size:

25.0 m

X offset:

0.00 nm

Y offset:

0.00 nm

Scan angle:
Scan rate:
Number of samples:
Slow scan axis:
Z limit:

0.00 deg
1.51 Hz
256
Enabled
440 V

Figure 8.7. Suggested Scan Controls settings during TappingMode set-up.

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Other Controls Settings

Other Controls
Units:
Color table:
AFM mode:
Input attenuation:
Engage Setpoint:
Z modulation:

Metric
2
Tapping
1x
0.90
Disable

Figure 8.8. Suggested Other Controls settings during TappingMode set-up

2. Move the sample to the area of interest using the stage manipulator.
3. Use the meters to verify that the vertical deflection is between -1 and +1, the
RMS amplitude (topmost meter) is 12 volts, and the sum voltage is greater than 1
volt.
4. The operator should now be ready to engage. Go to the upper Real Time menu
bar and click on Motor followed by Engage. You should now see a pre-engage
check, followed by Z-stage motor sounds. If for any reason the engage aborts
because the tip is still too far away from the surface, use the coarse adjustment
screws to bring tip and surface closer together. If all goes well after re-engaging, a
well formed image will begin to appear on the display monitor.
If it becomes necessary to image another part of the sample, execute a Withdraw
command before moving the X-Y translation stage; otherwise, the tip may be damaged. After the tip is engaged, the control panel values can be readjusted to provide
the desired scan parameters. Refer to section 8.6 below for scan parameter optimization.

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TappingMode AFM

8.5. Withdrawing the Tip

Select Withdraw from the Motor menu. The SPM will stop scanning, then ascend
approximately 7 microns. If more clearance between tip and sample is desired, toggle the Up / Down switch on the top-right side of the MultiMode base. Never withdraw samples without carefully observing that the tip has adequate clearance during
the entire sample removal sequence.

8.6. Beyond Basics with Resonating Techniques

This section discusses some of the subtle aspects of the operation of the MultiMode
in TappingMode. Without a thorough understanding of principles associated with
cantilever resonating techniques, distorted data may be generated. Understanding
the Cantilever Tune process and the effects of Real-time scan parameters is very
important to effective operation of the microscope. It is also very important to
understand similarities and differences between the force calibration mode of contact AFM and force calibration mode while in TappingMode.

8.6.1. Subtleties of Cantilever Oscillation

The response of the cantilever to inputs plays an important role in the operation of
the MultiMode microscope while in TappingMode. There is an important trade-off
between the response time of the cantilever and the force applied to the sample. The
cantilever does not respond instantly to perturbations in its vibrational amplitude.
The cantilever drive system pumps energy gradually into the cantilever oscillation.

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Cantilever Vibration Amplitude

Figure 8.9 shows a typical response curve of the cantilever amplitude as a function
of time. To demonstrate the conflicting requirements, the performance of the system will be analyzed at two operating points.
Free Amplitude
x

Setpoint 1

Setpoint 2
t2

t1

Time

Figure 8.9. Cantilever response curve.

At Setpoint 1 the operating point is only slightly lower than the free vibration
amplitude. This has the advantage of dissipating very little energy to the sample
surface. (The drawback is that the system takes longer to recover from a given perturbation in the amplitude.) Consider the case where the tip travels off a step with a
height of x. At Setpoint 1 it takes longer for the amplitude of the cantilever oscillation to increase. Therefore, the feedback system will be slow in responding to the
error created by going off of the step. At operating Setpoint 2 the cantilever amplitude builds up more rapidly. Therefore, the feedback system will sense the error
caused by going off of the step and respond more rapidly. Unfortunately, more
energy is transferred to the sample surface while scanning at this operating point.
Making the choice between response time and contact force can be made easier by
the nature of the sample. For example, harder samples can withstand higher contact
forces so the response time can be improved by lowering the Setpoint amplitude.
Soft samples that are relatively flat should be run with higher Setpoint values to
reduce the energy imparted to the sample. In general, the solution to the problem is
to decrease the scan rate and increase the feedback gains. In some situations, the
feedback gains cannot be increased without causing piezo oscillations; in such
cases there is no choice but to reduce the scan rate.
It should be noted that this effect is only a problem when the tip encounters a low
point in the sample. The amplitude of the cantilever vibration decreases very
quickly when taller portions of the sample are encountered. As a result, the system
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response can be markedly different depending on whether the tip is climbing or

descending a feature in the sample. For this reason, the Scope Mode can be very
useful when setting scan parameters. As the tip descends, features can be evaluated
by comparing the Trace and Retrace in the Scope Mode. Figure 8.10 shows the
effects of poorly selected scan parameters on a calibration standards that includes a
series of sharp-walled pits. Regardless of the scan direction, the tip does not track
the wall of the pit when the tip encounters a pit. It does, however, track the surface
closely when moving out of the pit.
Trace
Retrace

Z Range
50.00 nm/div

Scan Size - 2.50 m/div

Figure 8.10. Scope trace with high Scan rate.

Figure 8.11 shows the same sample with a slight increase in the Integral gain and a
twofold decrease in the Scan rate. The tip now tracks the surface when it descends
into the pit as well as when it exits. The Trace/Retrace lines now coincide closely.
Trace
Retrace

Z Range
50.00 nm/div

Scan Size - 2.50 m/div

Figure 8.11. Scope trace with correct Scan rate.

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8.6.2. Tuning the cantilever Drive frequency

The Drive frequency selected to oscillate the cantilever plays an important role in
the performance of the microscope while in TappingMode. As a first step it is
important to determine the resonance frequency of the cantilever, but the Drive frequency should be further tuned to improve scanning performance.
It has been determined that the microscope produces better data in TappingMode
when the Drive frequency is set lower than the resonance peak of the cantilever. The
Drive frequency should be set such that it coincides with a 10 percent decrease in the
vibration amplitude. Figure 8.12 shows the suggested operating region. It should be
noted that this is a suggestion based on our observations; users are certainly encouraged to experiment with the microscope and decide what produces the best results.
Drive Frequency should
be within this range.
Cantilever
Response
12.54 nm/div

Setpoint

Center Frequency - 338.8723 KHz

5.0 KHz/div

Figure 8.12. Example of Cantilever Tune frequency sweep.

8.6.3. Optimization of scanning parameters

Careful selection of the scan parameters is important to the successful application
of the MultiMode in TappingMode. In general, the effects of the various scan
parameters are the same for the TappingMode as they are for contact AFM mode.
The user is encouraged to review section 5.2. which discusses parameter optimization for contact AFM.
This section focuses on parameters specific to TappingMode. As with other
operating modes, the optimal parameter selection depends greatly on the sample.
All of the parameters in the real-time control panel are discussed in the Command
Reference Manual. The user is encouraged to review all parameter descriptions.
This manual analyzes the effects of the most important parameters.

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8.6.3.1. Data Type (Channel panels)

Data type is the first parameter to set because the settings of other parameters
depend on it. The Data type parameter in the Channel 1, Channel 2 and Channel
3 panels selects the type of data that is collected by the system. Height data corresponds to the change in piezo height needed to keep the vibrational amplitude of the
cantilever constant. Amplitude data describes the change in the amplitude directly.
The Sensitivity parameter in the Force Calibration control panel must be determined, as described in the discussion of the Force Calibration mode, before Amplitude data is accurate.
The scan parameters required to collect good Height data are different than the optimal parameters for Amplitude data. To collect Height data while tracking the sample surface with minimal change in the tips vibrational amplitude, the feedback
gains must be high. The position of the piezo during the scan reflects the height of
the sample.
TappingMode microscopy should not be conducted with low feedback gain values,
as this will cause damage to both the tip and sample. The maximum amplitude of
the cantilever oscillation is not sufficient to track tall features.
Amplitude data collected with high feedback gains is essentially the derivative of
the height; this is commonly referred to as the error-signal mode. The error-signal
mode provides a sensitive edge detection technique. With the dual screen mode it is
possible to capture both Height and Amplitude data simultaneously.

8.6.3.2. Gain settings

The Integral, Proportional, and (on some software versions) Look ahead gains
on the Feedback Controls panel must be high enough to force the feedback system
to track the sample surface. When scanning in TappingMode, the Integral and Proportional gains must be set to lower values than are used in the contact mode. Oscillation usually occurs with Integral gains of 12. The Proportional gain can
usually be set a factor of 510 times higher than the Integral gain. To optimize
the gains, increase the Integral gain until the piezo begins to oscillate, then eliminate the oscillations by reducing the gain with two or three clicks of the left arrow
key. Repeat the process for the Proportional gain. Piezo oscillations typically
cause high frequency wavy lines in the Real-time image.

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8.6.3.3. Scan Size, Scan rate, and Setpoint

As discussed above, the Scan size, Scan rate, and Setpoint values have dramatic
effects on the data. As in contact mode, the Scan rate must be decreased as the
Scan size is increased. Scan rates of 0.51.0 Hz should be used for large scans on
samples with tall features. High scan rates help reduce drift, but they can only be
used on flat samples with small scan sizes.
The Setpoint parameter defines the desired voltage for the feedback loop. The Setpoint voltage is constantly compared to the present RMS amplitude voltage to calculate the desired change in the piezo position. When the gain values are high, as
they should be when the Data type is set to Height, the Z piezo position changes to
keep the amplitude voltage close to the Setpoint; therefore, the vibration amplitude
remains nearly constant.
As discussed above, changing the Setpoint alters the response of the cantilever
vibration and changes the amount of force applied to the sample.

8.6.3.4. Lowpass filter (Channel panels)

The Lowpass filter invokes a digital, one-pole, low-pass filter to remove high-frequency noise from the Real-time data. The filter operates on the collected digital
data regardless of the scan direction. Settings for this item range from Off (typical
setting) through 9. Off implies no lowpass filtering of the data, while settings of 1
through 9, successively, lower the cut-off frequency of the filter applied to the data
stream.

8.6.3.5. Highpass filter (Channel panels)

The Highpass filter invokes a digital two-pole highpass filter which removes low
frequency effects such as bow (caused by Z hysteresis). As with the Lowpass filter,
it also operates on the digital data stream regardless of scan direction. This parameter can be Off or set from 1 through 9. Settings of 1 through 9, successively, lower
the cut-off frequency of the filter applied to the data stream.

Note

It is important to realize that in removing low frequency information from the

image, the highpass filter distorts the height information in the image. As a
result, this filter should be Off when accurate height information is desired.

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8.7. Force Calibration (Z Scan Controls) Mode

Force Calibration mode in TappingMode is similar to Force Calibration mode in
contact AFM mode; however, there are some notable differences. The Force Calibration command is in the Real-time / View menu. In Force Calibration mode,
the X and Y voltages applied to the piezo tube are held at zero (unless a DC offset is
in effect) and a triangular waveform is applied to the Z electrodes of the piezo tube.
As a result of the applied voltage, the sample is moved up and down relative to the
oscillating tip as shown in Figure 8.13. The Z scan start parameter sets the offset
of the piezo travel while the Z scan size parameter defines the total travel distance
of the piezo. Therefore, the maximum travel distance is obtained by setting the Z
scan start to +220 volts with the Z scan size set to 440 volts. In practice, the maximum scan size should not be applied to the piezo because the cantilever is delicate
and may break if too much deflection is induced.
CAUTION: Use caution when working in Force Calibration mode. This mode
can potentially damage the tip and/or surface.
ATTENTION: Digital Instruments recommande dutiliser le mode Force Calibration avec une prcaution. Lutilisation du mode Force peut endommager la
pointe ou lchantillon.
WARNHINWEIS: Seien Sie vorsichtig, wenn Sie im Force Calibration Mode
arbeiten. Dieser Memode kann unter Umstnden Mespitze oder Probe beschdigen.
Z scan size
oscillating tip
Z scan start

Distance fixed
by adjustment
screws

Retracted

Extended

Figure 8.13. Piezo travel in Amplitude Cal. mode

As the piezo moves the sample up and down, the RMS value of the cantileverdeflection signal is monitored. The Force Calibration plot (a plot of the RMS signal

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as a function of the voltage applied to the piezo tube) shows on the display monitor.
The control panel containing the parameters used to control the microscope in the
Force Calibration mode is visible on the control monitors top menu bar.
Force Calibration mode is used to compare the amplitude of cantilever oscillation
on the surface to the free-air amplitude. Other uses of Force Calibration mode
include characterizing the forces on the cantilever tip, diagnosing the performance,
and calibrating the RMS amplitude voltage as a function of the oscillation amplitude of the cantilever.

8.7.1. The Force Calibration plot

Figure 8.12 depicts a typical Force Calibration plot for TappingMode operation.
The vertical axis of the graph represents the RMS of the cantilever deflection signal. The voltage applied to the Z electrodes of the piezo tube is plotted along the
horizontal axis. The left side of the graph is equal to the Z scan start voltage while
the right side of the screen is equal to the quantity (Z scan start minus Z scan size).
The Force Calibration plot represents the RMS signal for one complete extension/
retraction cycle of the piezo. The Z scan rate parameter in the Force Cal control
panel defines the rate at which the piezo completes an extension/retraction cycle;
therefore, the rate at which new curves are displayed.
The right side of the plot reflects the free vibration amplitude of the cantilever. At
this piezo position the vibration amplitude is not influenced by the sample. Eventually as the piezo extends the vibrating cantilever toward the sample, the probe contacts the sample surface and the vibration amplitude decreases. After the tip begins
to contact the sample surface, each nanometer decrease in the cantilever position
decreases the vibrational amplitude of the cantilever by two nanometers. The vibrational amplitude of the cantilever continues to decrease as the probe lowers. When
the piezo turns around and begins to retract the sample, the vibrational amplitude of

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the cantilever begins to increase. It continues to increase until the tip is free of the
surface, then it levels off at the free-standing amplitude.
Free Vibrational Amplitude
(tip is free of the surface)

RMS of Cantilever
Deflection Amplitude

Setpoint

+Z
(Scan start)

Z Piezo Voltage

-Z
(Scan start Scan size)

Slope = RMS of Deflection voltage/nanometers (or volts) of piezo travel

Figure 8.14. Typical Force Calibration curve.

The display monitor also presents a linear scale of the Z piezo voltage. The scale
ranges from +220 volts at the extended end to -220 volts at the retracted end.
The range of the piezo travel, as defined by the Z scan start and Z scan size parameters in the Force Calibration control panel, is represented by two white lines on the
scale. The lower, white line corresponds to the Z scan start parameter in the control panel while the spacing between the lines corresponds to the Z scan size. The
average voltage applied to the Z electrode on the piezo tube just prior to entering
the Force Calibration mode is represented by the blue, Z center line.

8.7.2. The Force Calibration control paneladditional features

The Force Cal control panel is shown in figure 8.13. The setpoint voltage used in
the feedback loop can be adjusted from this panel. With the Tip Up and Tip Down
buttons, the stepper-motor can be used to adjust the position of the vibrating cantilever relative to the sample. The Capture button stores the Amplitude Calibration
plot for Off-line viewing. It should be noted that some of the parameters influence
the Real-time operation of the microscope while most of the menu parameters
affect only Force Calibration mode.
The input sensitivity of the MultiMode head must be defined properly to keep the
values on the vertical axis of the Amplitude Calibration plot accurate. The In

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sensitivity parameter should be set to 0.125 by using the Real-time / Microscope /

Calibrate / Detector command for the MultiMode microscope.
Z Scan Controls
Graph Controls
Z scan start:

100 nm

Other Controls
Trigger mode:

Z scan size:

500 nm

Trig threshold:

Z scan rate:

4.88 Hz

Trigger channel:

X offset:

0.00 V

Z step size:

Y offset:

0.00 V

Step threshold:

Number of samples:
Average count:
Sensitivity:
Units:

512
1
0.0379 V/nm

Off
0.00 V
Amplitude
2.40 V
7.53 V

Start mode:

Calibrate

End mode:

Extended

Indent Feedback:

Disabled

Metric

Figure 8.15. Force Cal. control panelTappingMode.

Most of the parameters in the control panel have the same function as the Force
Calibration parameters used for contact AFM, which are discussed in Chapter 6 of
this manual. Those parameters not discussed in Chapter 6 are discussed in the following paragraphs:
Setpoint The RMS value of the cantilever deflection voltage maintained by the
feedback loop in the Real-time mode can be adjusted by changing this parameter. In
the TappingMode Force Calibration menu, this parameter defines the centerline of
the vertical, Tip Amplitude axis of the amplitude calibration plot shown on the
display monitor. Changing the Setpoint shifts the amplitude curve on the graph,
because the centerline value is always equal to the Setpoint. For example, if the Setpoint is at 3.0 Volts, the RMS amplitude axis of the graph will be centered around
3.0 Volts; raising the Setpoint to 4.0 Volts will shift the amplitude curve down by
one volt, so the graph will be centered at 4.0 Volts. Changing the value of this
parameter in the Amplitude Calibration mode also changes the Setpoint parameter
in the Real-time control panel.
Drive frequency This item defines the frequency at which the cantilever is oscillated. This frequency should be very close to the resonant frequency of the cantilever. Changing the value of this parameter in the Force Calibration menu also
changes the Drive frequency parameter in the Real-time control panel.
Drive amplitude This parameter defines the amplitude of the voltage applied to
the piezo system which drives the cantilever vibration. Changing the value of this
parameter in the Force Calibration mode also changes the Drive amplitude
parameter in the Real-time control panel. It is possible to fracture the cantilever by
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using too high of a drive amplitude; therefore, it is safer to start with a small value
and increase the value incrementally. If the amplitude calibration plot consists of a
flat line all the way across, changing the value of this parameter should shift the
level of the curve. If it does not, the tip is probably fully extended into the surface
and the tip should be withdrawn before proceeding.
Sensitivity This item relates the vibrational amplitude of the cantilever to the Z
travel of the piezo. It is calculated by measuring the slope of the RMS amplitude
versus the Z voltage when the tip is in contact with the sample as shown in figure
8.12. The NanoScope system automatically calculates and enters the value from the
graph after the operator uses the mouse to fit a line to the graph. This parameter
must be accurately calibrated before Amplitude data obtained in Lift mode will be
accurate.

Note

Sensitivity can only be set on channel one.

8.7.3. Examples of amplitude calibration plots
Figure 8.16 shows a typical amplitude calibration plot. Depending on the sample
and the operating conditions, the curve may include other notable features. This
section presents examples of some of those conditions.

8.7.3.1. Very high contact force

Figure 8.16 shows a curve produced when the tip is too close to the sample. This is
a very dangerous condition because the cantilevers used in the TappingMode are
very stiff and brittle. If they are driven into the sample surface so that the oscillation
amplitude changes to zero, they will break.
DI recommends using Force Calibration only when the tip is known to be bad, or
when it is important to obtain experimental information shown in Force Calibration
The flat portion on the left side of amplitude curve in figure 8.18 occurs because the
tip is so close to the surface that it no longer vibrates. As the piezo extends the sample further and further, the amplitude of vibration does not change because the tip is
always in contact with the sample surface. The contact force is very high due to the

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stiffness of the TappingMode cantilevers and the cantilever or tip can be shattered if
the deflection continues.

Figure 8.16. Amplitude force plot with high contact force.

This situation can be avoided by reducing the value of Z scan start so there is no
flat portion on the left side of the curve. Rapidly increasing the value of Z scan size
is very dangerous since the total vibrational amplitude of the cantilever is small relative to the total Z travel of the long-range scanner. The total amplitude of the cantilever oscillation is usually less than 100 nanometers while the "J" scanner travels up
to 6 microns along the Z axis. In general, the Z scan size parameter should be much
smaller than the value entered into the Force Cal. menu of contact AFM.

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8.8. TappingMode in FluidsIntroduction

Operation of TappingMode in fluid provides the same advantages of TappingMode
in air, with the additional ability to image samples under native liquid conditions. In
fluid TappingMode, the probe is oscillated so that it only intermittently contacts the
sample surface. This can reduce or eliminate frictional forces that often damage soft
or fragile samples in contact mode. The following sections provide general instructions for TappingMode imaging in fluid, then provide practical instructions for
imaging two different biological samples. Instructions should be adjusted for different samples and imaging conditions.
Before attempting TappingMode in fluids, it is recommended that the user become
familiar with standard TappingMode operation in air (see above sections) and contact AFM in fluid (Chapter 7).
CAUTION! When imaging fluid samples, use extraordinary precautions against
spillage. Fluids must NOT be spilled on or around the sample stage electronics
boxes, or other components containing electronic parts. Avoid spilling all corrosive
fluids on exposed surfaces; otherwise, damage may result! In the case of a spill,
immediately clean and thoroughly dry all affected surfaces carefully
ATTENTION! Lors dun travail en milieu liquide, prendre toute prcaution pour
viter des fuites. Les liquides ne doivent pas se rpandre sur la platine porte chantillons, le botier lectronique ou toute autre partie du microscope contenant de
llectronique. Eviter toute fuite de liquide corrosif sur les surfaces exposes. Le
non respect de cette recommandation peut entraner des dommages. En cas de fuite,
nettoyer et scher immdiatement les surfaces touches.
WARHINWEISS! Falls Sie Proben in Flssigkeiten abbilden, lassen Sie uerste
Vorsicht walten, damit keine Flssigkeit verspritzt wird. Flssigkeiten drfen nicht
auf die oder nahe der Probenhalterung, der Elektronikbox oder anderen Komponenten, die elektronische Bauteile enthalten, verspritzt werden. Vermeiden Sie bitte,
korrosive Flssigkeiten auf freiliegende Oberflchen zu verspritzen; andernfalls
wren Beschdigungen die Folge! Falls Sie Flssigkeit verspritzt haben, subern
und trocknen Sie alle betroffenen Flchen sorgfltig.

8.8.1. Acknowledgments
Digital Instruments, Inc. wishes to express its appreciation to the following individuals for their assistance in preparing the following sections: Monika Fritz, Manfred
Radmacher, Magdalena Benzanilla, Helen G. Hansma, Jan H. Ho, Daniel Mueller,
Craig B. Prater.

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8.8.2. Overview
TappingMode in fluid combines the advantages of TappingMode with the ability to
image samples in native liquid environments (e.g., physiological buffer solutions).
Digital Instruments would appreciate receiving any further suggestions and is anxious to hear about new sample preparation techniques and experience with TappingMode in fluid.

8.8.3. Fluid cell preparation

Required Materials

TappingMode Fluid Cell, Model MMTFC

Cantilevers (100m, narrowed-leg, Oxide-Sharpened Silicon Nitride tips,
Models NP-S or NP-STT, work well)

Deionized water
Source of filtered (0.2 m), compressed air or dry nitrogen (chromatographicgrade)

UV lamp, high-intensity; Oriel Mod. 6035 pencil-style spectral calibration lamp

or equivalent (optional for cantilever cleaning).

1 cc and 5cc syringes or micropipettes (200 l pipette tips)

Fluid cell liquid lines (silicone tubing and fittings)
Fluid cell o-ring (optional see Section 8.8.5.)
Hemostats or similar clamping device (for liquid lines)
Filter paper

8.8.3.1. Clean fluid cell and o-ring.

To reduce contamination problems and to obtain high-quality images, the fluid cell
and o-ring must be as clean as possible. The following cleaning procedure works
well:

While soaking in warm, soapy water, place a few drops of liquid dish soap on
the fluid cell and o-ring, then rub gently with a cotton swab or finger. Take care
not to scratch the glass surface with any abrasive material.

Rinse completely free of detergent with distilled water.

Blow dry the fluid cell with 0.2 m-filtered, compressed air or dry nitrogen until
all moisture is evaporated.

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8.8.3.2. Select and install cantilever.

Best results are usually obtained with the 100 micron, narrow-legged cantilevers
with oxide-sharpened silicon-nitride tips (Model NP-S or NP-STT). Some users
also use electron beam deposited (EBD) tips for fluid work. Contact Digital Instruments for information on making or purchasing EBD tips. Try oxide sharpened tips
to start. Good results have also recently been obtained with etched silicon cantilevers (standard air TappingMode cantilevers, Mod. ESP or FESP), used at very small
oscillation amplitudes. Users should experiment to find which cantilevers work best
for their sample.
Install a cantilever snugly into the fluid cells tipholder. Check that the spring clip
holds the cantilever tightly.

8.8.3.3. Clean cantilever with UV light if desired.

The AFMs resolution can be limited by contaminants on the cantilever tip. Here is
a procedure to remove organic contamination from the tip:
Place the fluid cell with installed tip face-up on a clean surface. Position a UV lamp
very close (3-5 mm) to the fluid cell and allow the unit to be irradiated for 15-30
minutes at full intensity.

8.8.4. Sample mountingMethod 1 (with an o-ring).

Secure a sample substrate (cover glass or mica) to a magnetic stainless steel sample
puck using double-sided adhesive. Load the prepared sample substrate onto the
AFM scanner.

8.8.4.1. Install o-ring on sample.

Place the o-ring onto the sample substrate. It should be positioned so that it forms a
seal around its periphery and does not overlap any edges.
Fluid drop

O-ring
Sample or
substrate
Figure 8.17. Place the o-ring on the sample and slowly fill with fluid using a
micropipette.

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CAUTION! Do not add excessive amounts of fluid or the cell will overflow and
damage the piezo tube scanner.
ATTENTION! N'ajoutez pas trop de fluide. Sinon, la cellule dbordera et endommagera le scanner du tube piezo.

8.8.4.2. Fill o-ring with liquid.

Drip enough liquid solution into the o-ring to form a small pool, as shown in
Figure 8.17. Use filter paper to wick away small droplets from the top of the o-ring
until the top is dry. Verify that the o-ring is not leaking around its edges.
CAUTION! When imaging fluid samples, use extraordinary precautions against
spillage. Fluids must NOT be spilled on or around the sample stage, electronics
boxes, or other components containing electronic parts. Avoid spilling all corrosive
fluids on exposed surfaces; otherwise, damage may result! In the case of a spill,
immediately clean and dry all affected surfaces carefully
ATTENTION! Lors dun travail en milieu liquide, prendre toute prcaution pour
viter des fuites. Les liquides ne doivent pas se rpandre sur la platine porte chantillons, le botier lectronique ou toute autre partie du microscope contenant de
llectronique. Eviter toute fuite de liquide corrosif sur les surfaces exposes. Le
non respect de cette recommandation peut entraner des dommages. En cas de fuite,
nettoyer et scher immdiatement les surfaces touches.
WARHINWEISS! Falls Sie Proben in Flssigkeiten abbilden, lassen Sie uerste
Vorsicht walten, damit keine Flssigkeit verspritzt wird. Flssigkeiten drfen nicht
auf die oder nahe der Probenhalterung, der Elektronikbox oder anderen Komponenten, die elektronische Bauteile enthalten, verspritzt werden. Vermeiden Sie bitte,
korrosive Flssigkeiten auf freiliegende Oberflchen zu verspritzen; andernfalls
wren Beschdigungen die Folge! Falls Sie Flssigkeit verspritzt haben, subern
und trocknen Sie alle betroffenen Flchen sorgfltig.

8.8.4.3. Pre-wet the fluid cell.

Occasionally air bubbles will form in the fluid cell and block laser light. This step
can reduce the chance of forming bubbles.
Before installing the fluid cell into the head, insert a syringe or pipette filled with
liquid solution into a fluid port. Flood the fluid cell port with buffer solution, allowing liquid to drip out the bottom of the cell.When you have finished, leave the
buffer-filled syringe inserted. A small amount of buffer solution should be held to
the bottom of the cell by surface tension, as shown in Figure 8.18.

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Fluid Cell

Syringe

Liquid Drop
Figure 8.18. Flush the fluid cell before installation
to reduce bubble formation.

8.8.4.4. Install SPM head and fluid cell.

Place the SPM head onto the scanner and secure the head stabilizing springs. Plug
the heads 15-pin connector into the scanner support ring. Use the three scanner
screws to lift the SPM head so that there will be sufficient clearance to install the
fluid cell without breaking the cantilever. Make sure the head is level side-to-side
and that the head is tilted slightly forwards so that it will be level when the tip contacts the surface. Carefully install the fluid cell into the SPM head, lowering the
fluid cell onto the o-ring until seated securely. Tighten down the clamp to hold the
fluid cell in place. If you have purchased a vertical-engage scanner, leveling problems are eliminated.

8.8.4.5. Fill the fluid cell with liquid.

Attach a drain line to the other fluid cell port. Slowly flush the fluid cell with buffer
solution from the syringe. Check for leaks and wick away any spilled liquid with
filter paper until SPM components are dry.

8.8.4.6. Remove bubbles and clamp off fluid cell lines.

Observe the fluid cell and cantilever through the viewing port using an optical
microscope. Bubbles inside the fluid cell near the cantilever can interfere with the
laser beamthese should be removed.
To remove bubbles from the cell, rapidly push liquid through the cell with a
syringe. If sufficient force is applied, the bubbles will be washed away. To prevent
the introduction of air and spillage, be certain to maintain a good seal between the
syringe and fluid cell port.
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When the fluid cell has been filled and bubbles have been removed, clamp off the
drain line with a pair of hemostats or similar clamp.

8.8.5. Sample mountingMethod 2 (without an o-ring).

The fluid cell may be used without the o-ring. Place the fluid cell close to the sample surface, and slowly inject fluid until a liquid drop forms which is held by surface tension between the sample surface and the glass cantilever holder.
Use Loctite 770 (recommended adhesive) to affix a teflon cover over the steel sample puck (teflon should slightly extend over the edge of the sample puck) and then
use 2 component epoxy to attach the mica to the teflon. The hydrophobic teflon
will help confine the solution without installing an o-ring.
Aqueous Sample

Mica
Teflon
12 mm

Stainless Steel
Sample Puck

Figure 8.19. Stainless steel sample puck with teflon cover.

CAUTION! Do not use a sample volume that exceeds 50 l as excess fluid may be
squeezed onto the AFM scanner. Do not pre-wet the fluid cell when using the oring-less method.

To use this method of fluid imaging, align the SPM head and mounted fluid cell
(cantilever installed) with the dry sample puck first before applying the aqueous
sample. Allow 0.5 mm clearance between the tip and dry substrate surface. Once
the optics and laser are aligned, remove the SPM head and fluid cell. Take the dry
sample substrate off the scanner and apply the sample in a volume of approximately
25-40 l. The liquid should form a small dome over the mica and not spread onto
the surrounding teflon. Carefully replace the prepared sample puck. Slowly mount
the SPM head and fluid cell onto the sample. Since the aqueous sample will change
the light deflection, the laser photodetector will need to be re-adjusted. Course
adjustments are made by tilting the deflection mirror while fine adjustments are
made with the photodetector adjustment knobs on the left-top and left-rear of the
head. Adjust the photodiode position to give a deflection signal 0 V.
An alternative method to removing the SPM head after alignment is, with the dry
sample substrate in place on the scanner, slowly deliver 25-50l of sample solution

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Be sure that the pipette tip is inserted

into the smaller rear delivery hole in
the fluid cell.

Pipette

into the fluid cell using a standard micropipette (e.g. Eppendorf, Gilman) with a
200l capacity pipette tip. The end of the pipette tip fits into the fluid cell port holes
(refer to figure below). Inspect from the side to make sure the fluid is well confined
to the mica area only.

8.8.5.1. Aim the laser on cantilever and adjust photodiode position.

Instructions for adjusting the laser beam and photodiode through fluid are provided
in previous sections. Adjust the photodiode position to give a deflection signal of
around 0 V.

8.8.5.2. Check that the microscope is dry.

Verify that all MultiMode surfaces are free of spilled fluid. Wick away moisture and
droplets with filter paper.

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Note
Over time, evaporation of the fluid may necessitate replenishing the fluid cell using
a standard micropipette. The pipette will fit conveniently into the fluid chamber
port.

8.8.6. TappingMode operation in fluid.

At this point in the procedure, the sample should be loaded in the AFM and the fluid
cell filled with fluid. The laser should be aligned on the cantilever and the photodiode centered to give a deflection signal near 0 V.

8.8.6.1. Choose TappingMode operation in software.

In the Other Controls screen, set the AFM mode parameter to Tapping. If using a
Dimension or BioScope system, switch the Z modulation parameter to Enabled.

8.8.6.2. Set initial scan parameters.

For initial imaging, try the following settings:

Drive frequency = Tune to a peak between 8-10 kHz.

Drive amplitude = 500 mv (should correspond to 0.5 V rms amplitude)
Scan speed = 1 Hz
Integral gain = 0.5 (MMAFM); 1.5 (BioScope)
Proportional gain = 0.75
Z modulation = Enabled (BioScope and Dimensions only)
Z range = 50 nm
First Image Data type = Height
Second Image Data type = Amplitude
Third Image Data type (optional) = Phase; Height retrace

The user should try to adjust and optimize these settings for each imaging condition and sample.

8.8.6.3. Select the drive frequency using the Cantilever Tune command.
This is similar to the Cantilever Tune process used for standard TappingMode in
air. Unlike operation in air, the cantilever resonance will be largely damped by liquid and the AutoTune function cannot be used.

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Enter the View / Sweep / Cantilever Tune menu to select a drive frequency. Users
of TappingMode in air will notice that there is no single, well-defined resonance
peak, but a number of broader peaks when viewing a wide cantilever sweep. The
user must manually select a peak that corresponds to the resonant frequency of the
cantilever being used. For the short, narrow Si3N4 cantilever, the resonant frequency in fluid is a broad peak centered around 10 kHz. Best results are achieved
by tuning the cantilever to a peak between 7-12 kHz. Higher and lower frequencies
have also been used depending on the type of cantilever employed. Start with a
Sweep width of 20 kHz and a Sweep setpoint of 9 kHz in the Sweep Control
menu. A typical Cantilever Tune screen is shown in Figure 8.20.
Note: Make certain the cantilever is very close to the sample surface when tuning
the cantilever under fluid.

Figure 8.20. Typical Cantilever Tune curve for 100m, narrow-legged

silicon nitride cantilever in fluid. The user must manually tune using Zoom
in and Offset functions.

8.8.6.4. Adjust the Drive amplitude.

Adjust the Drive amplitude until a desired cantilever RMS amplitude is obtained.
For samples with small height variations, try an RMS amplitude of around 0.5 V.
Usually, this requires a Drive amplitude of 250-500 mV. For rougher samples try
larger RMS voltages (1-2 V). Experiment to find what level of cantilever oscillation
gives best results for specific applications. Good results are usually not obtained on
soft samples if it is necessary to use a Drive amplitude above 1.0 V.

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Note

The RMS amplitude must be adjusted when the AFM tip is near the sample
surface (< 50m).

8.8.6.5. Recenter the photodiode.

Readjust the photodiode until cantilever deflection is roughly zero. The cantilever
deflection signal can drift when the cantilever is first in fluid, so it is best to readjust
prior to engaging.

8.8.6.6. Engage.
Use the Engage command to bring the tip into tapping range. The NanoScope software will automatically select a setpoint, then will stop the engagement when the
surface is detected.

8.8.6.7. Adjust the setpoint.

Usually the best topographic images are obtained at setpoints 10-20 percent less
than the cantilever RMS amplitude before engaging. The setpoint may be optimized
in one of two ways, using the Force Cal (View / Force Mode / Plot) command or
by optimizing the image quality. Both techniques are described below.
Plotting Force
The View / Force Mode / Plot command plots the cantilever amplitude versus the
scanner position. The curve should show a mostly flat region where the cantilever
has not yet reached the surface and a sloped region where the amplitude is being
reduced by the tapping interaction. Set up Force Cal as described for TappingMode
in air (experienced users may use the Force Step command instead). To protect the
tip and sample, take care that the cantilever amplitude is never reduced to zero.
Adjust the Setpoint until the green setpoint line on the graph is just barely below
the flat region of the Force Cal curve. This is the setpoint that applies the lowest
force to the sample.

Note

The slope of the Force Cal curve shows the sensitivity of the fluid TappingMode
measurement. In general, higher sensitivities will give better image quality. If
the sensitivity is very poor, check the mounting of the sample and fluid cell.

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Optimizing Image Quality

The Setpoint can also be adjusted by simply monitoring the image quality. Select a
Scan size of 500 nm. Increase the Setpoint in small increments until the cantilever
pulls off the surface and the Z center voltage goes to -220 V. Reduce the Setpoint in
small increments until an image appears. Continue reducing the Setpoint until the
image is optimized. (Usually the best images are obtained at setpoints just below
where an image appears.)

8.8.6.8. Optimize other scan parameters.

The NanoScope IIIa will attempt to keep the cantilever amplitude constant during
the scan. Optimize the Integral gain and Proportional gain so that the Height
image shows the sharpest contrast and there are minimal variations in the Amplitude image (the error signal). It may be helpful to optimize the Scan rate to get the
sharpest image.

8.8.7. Troubleshooting tips.

8.8.7.1. Cantilever Tune plot looks badfluid cell/loose tip
Become familiar with the characteristics of the Cantilever Tune plot when good
images are obtained. The Cantilever Tune plot can be used as a diagnostic tool. If
the plot looks substantially different from previous successful experiments, there
may be a problem with the fluid cell. For example, the cantilever may be loose in its
holder.

8.8.7.2. O-ring slides across sample surface, causing drift

To reduce movement of the o-ring which can cause drift in AFM images, the fluid
cell needs to be set up such that there is minimal lateral movement of the optical
head with respect to the sample once the o-ring is installed. This is best accomplished by keeping the head level while positioning the tip as close as possible to
the surface before installing the o-ring so that the tips lateral movement is minimized during engagement. Moving the positioning screws at the bottom of the optical head should also be minimized once the o-ring is installed. Further suggestions
for solving this problem consist of the following:
1. The new vertical engage scanner allows the tip to approach samples without the
lateral offset caused by older, three-point supports. Thus, stress on the o-ring from
lateral movement during engagement is not present. Call DI for more details.

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2. Lightly coating the area of the o-ring which contacts the sample surface with
white petrolatum or vacuum grease will allow the o-ring to slide across the surface,
minimizing lateral stress. This also forms a better fluid-tight seal between the o-ring
and sample. However, some solvents (i.e., nonpolar organic solvents) may dissolve
some of the lubricant into the fluid.
3. Replace the o-ring with a slice of thin-walled glass, plastic, or stainless steal tubing. The diameter and thickness of the ring of tubing should be chosen so that it
does not contact the inner or outer walls of the circular groove in the glass cantilever holder. This gives the optical head room to move laterally during engagement
and for positioning the tip over the sample surface. The height of the ring of tubing
must be chosen so that it is not too tall so that the tip cannot reach the sample surface, or too short so that the ring does not reach the bottom of the glass cantilever
holder before engagement. Glue the ring of tubing to the steel sample puck or to
the sample to prevent leaks.

Note

When using the ring of tubing in the fluid cell, fluid is blocked from exiting and
cannot be circulated through the cell.
4. When positioning the o-ring on the surface, adjust the positioning knob at the
base of the optical head to move it slightly forward. This will counter some of the
lateral stress on the o-ring which comes from the optical head moving back during
engagement.

Note

Remember that to prevent leaks when using the standard o-ring, it is best to
place the o-ring on the sample before placing the optical head on the scanner,
instead of inserting the o-ring into the groove in the glass cantilever holder
before placing the optical head on the scanner.

8.8.7.3. Laser sum signal absent or weakair bubbles

Check that all bubbles are removed from the cantilever. Bubbles may attach themselves to the cantilever, causing the laser beam to be diffracted. Bubbles can sometimes be removed by forcing fluid through the fluid cell. Degassing your imaging
fluid prior to use in the AFM will solve bubble problems.

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8.8.7.4. Poor image quality

Contaminated Tip Some types of samples may adhere to the cantilever and tip
(e.g., certain proteins). This will reduce resolution giving fuzzy images. If tip
contamination is suspected to be a problem, it will be necessary to protect the tip
against contamination. See section 8.8.6 for a method of reducing tip contamination.
Dull Tip AFM cantilever tips can become dull during use and some unused tips
may be defective. If imaging resolution is poor, try changing to a new cantilever.
Also, check the cantilever type being used. Oxide sharpened silicon nitride cantilevers are usually much sharper than standard silicon nitride cantilevers. The user
may also wish to try electron beam deposited (EBD) tips to improve resolution.
Contact Digital Instruments for details on making or purchasing EBD tips.
Multiple Tip AFM cantilevers can have multiple protrusions at the apex of the
tip which result in image artifacts. In this case, features on the surface will appear
two or more times in an image, usually separated by several nanometers. If this
occurs, change or clean the AFM tip.

8.8.8. Model sample preparations.

This section overviews sample preparation techniques for two different samples: 1)
the protein lysozyme; and, 2) DNA. These protocols can serve as a model when
developing methods to bind other samples.

8.8.8.1. General notes on sample binding

Samples for AFM imaging should be immobolized on a rigid substrate. Macroscopic samples (biomaterials, crystals, polymer membranes, etc.) can be attached
directly to a stainless steel sample disk with an adhesive. Dissolved or suspended
samples like cells, proteins, DNA, etc. are usually bound to a flat substrate like
mica or glass, for example. Many different sample preparations have been developed and SPM applications articles are an excellent source of information on sample binding. For a list of articles describing biological applications of AFM,
including sample preparation techniques, contact Digital Instruments.
Binding Specimens to Mica
The following procedures will describe how to bind two different samples to a mica
substrate. Mica is commonly used because atomically flat substrates can be simply
and inexpensively prepared. In aqueous solutions, the mica cleavage surface
becomes negatively charged. Specimen binding is usually accomplished using electrostatic attraction between charges on the specimen and those on the mica surface.
Proteins, for example, can usually be made to stick to mica by operating at a pH
where they exhibit positively charged domains. DNA, on the other hand, is negatively charged and can be bound either by altering the mica surface charge from
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negative to positive (using a silanization process) or by dissolving the DNA in a

divalent metal counter ion (e.g. Mg++, Ni++). Both of these techniques are discussed separately below.
Many other techniques are being developed for chemically modifying mica, glass
and other substrates to bind a variety of biological samples. Contact Digital Instruments for a bibliography of references on imaging of biological specimens.

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8.9. Lysozyme on micaA model procedure for

protein binding
Protein binding theory
All proteins contain free amino groups that become positively charged at sufficiently low pH. If sufficient free amino groups are located on the outside surface of
the protein, then the protein will bind to a negatively charged mica surface. Proteins
will become positively charged at pH below their isoelectric point and are then able
to bind to mica. The protein lysozyme, for example, becomes sufficiently positively
charged to bind to mica at pH 6. This is shown schematically below in Figure 8.21.

proteins

buffer
pH<pI

+++

+++

mica
Figure 8.21. Proteins will typically bind to negatively charged mica when
the pH is reduced below the proteins isoelectric point, pI.
Protein binding procedure:
The following section gives a detailed procedure for preparing and imaging the protein lysozyme by TappingMode in fluid. The procedure was kindly provided by
Monika Fritz at the University of California, Santa Barbara and is described in the
following papers:

Radmacher, M., M. Fritz, H.G. Hansma, P.K. Hansma (1994). "Direct

Observation of Enzyme Activity with Atomic Force Microscopy." Science 265,
1577.

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Required Materials

Deionized water
Mica substrates
Lysozyme protein L-6876 from Sigma Chemical
Phosphate buffer solution, 10 mM KH2PO4, 150 mM KCl, pH 6 (buffer may be
adjusted for other proteins)

TappingMode Fluid Cell, Model MMTFC

Syringes: (1) 1 cc; (2) 5 cc; Micropipettes

Cantilevers (Oxide-Sharpened Silicon Nitride tips, Model NP-S, work well)

Source of filtered (0.2 m), compressed air or dry nitrogen
UV lamp, high-intensity; Oriel Mod. 6035 pencil-style spectral calibration lamp
or equivalent (optional for cantilever cleaning).
Fluid cell liquid lines (silicone tubing and fittings)
Fluid cell o-ring (optional see Section 8.8.5.).
Hemostats or similar clamping device (for liquid lines)
Filter paper

8.9.1. Dissolve protein.

Dissolve the lysozyme in phosphate buffer (PBS) solution to a concentration of 1
g per ml (this concentration provides a convenient coverage for AFM imaging and
may be used for a variety of similar size samples). This mixture should be drawn
into a clean, 1 cc syringe and capped. Prepare another 5 cc syringe of straight buffer
solution.
When imaging fluid samples, use extraordinary precautions against spillage.

8.9.2. Prepare fluid cell.

Prepare the fluid cell for TappingMode in fluid operation. Clean the fluid cell and
load a cantilever. For best results, clean the cantilever with UV light.

8.9.3. Prepare mica.

Cleave a fresh mica surface by first pressing some adhesive tape against the top
mica surfaces, then peeling off the tape.

8.9.4. Deposit protein solution on mica.

Deposit 50 l of protein solution on the freshly cleaved mica.
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8.9.5. Allow protein to bind to substrate.

Allow 20-30 minutes for the protein solution to bind to the mica substrate. Binding
time may vary with different samples. For longer binding times, put the mica in a
covered dish with a wet piece of filter paper to keep the liquid from evaporating.

8.9.6. Rinse unbound proteins from fluid cell.

Rinse the sample with a large quantity of buffer to remove unbound protein. Leave
a drop of buffer on the mica.

8.9.7. Assemble fluid cell.

Mount the sample on the scanner end cap. Seal the fluid cell and fill with buffer.

8.9.8. Clamp fluid drain line.

After the fluid cell has been flushed with buffer solution, reclamp the drain line.
This is important for low-noise, low drift imaging. The sample is now ready for
TappingMode imaging. A good TappingMode image of lysozyme protein on mica
is shown in Figure 8.22

Figure 8.22. TappingMode image of lysozyme in buffer solution

using above sample preparation (scan size 500 nm).

Note

It is also possible to prepare samples inside the fluid cell by flowing the protein
solution through the fluid cell. In this case, it may be helpful to engage the tip in
contact mode with a zero Scan size to protect proteins from binding to the tip.

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8.10. Binding DNA to Mica

DNA Binding Theory
DNA and mica are both negatively charged, and so it is necessary to modify the
mica surface or the DNA counter ion to allow binding. The counterion method is
done by adsorbing the DNA onto the mica in the presence of a divalent (+2
charged) ion, like Ni+2. The divalent ion will serve as a counterion on the negatively
charged DNA backbone and will also provide additional charge to bind the mica.
This is shown schematically in Figure 8.23.

DNA molecule

Buffer solution
Mica

Ni+2 or Mg+2 ions

- --- --- - -++

- -++-++- ++
- ++
- -++-++- ++- +-

Figure 8.23. Negatively charged DNA may be bound to negatively charged

mica in the presence of divalent counterions, such as Ni+2.
DNA binding procedure
The following procedure is adapted from these sources:

Dunlap, D.D., A. Maggi , M.R. Soria & L. Monaco (1997) "Nanoscopic

Structure of DNA Condensed for Gene Delivery." Nucl. Acids Res. 25, 3095.

Kasas, S., N.H. Thomson, B.L. Smith, H.G. Hasma, X. Zhu, M. Guthold, C.
Bustamante, E.T. Kool, M. Kashlev & P.K. Hasma (1997) "Escherichia coli
RNA polymerase activity observed using atomic force microscopy."
Biochemistry 36, 461.

Lyubchenko, Y.L. & L.S. Shlyakhtenko (1997) "Direct Visualization of

Supercoiled DNA in situ with Atomic Force Microscopy." Proc. Natl. Acad. Sci.
USA 94, 496.
Many other references regarding DNA imaging are listed in the Digital Instruments
Biological Applications Bibliography; call Digital Instruments for a copy.

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Required materials

Mica substrates
DNA: BlueScript II SK9(+) double stranded plasmid DNA, 2961 base pairs,
1mg/ml in 10mM Tris, 1mM ethylenediaminetetraacetic acid (EDTA) from
Stratagene, La Jolla, CA.

Buffer solution: 10 mM HEPES and 5 mM NiCl2 pH 7.6 (for loose binding and
air imaging), or NiCl2 (for tight binding and fluid imaging)

8.10.1. Dilute DNA in buffer

Dilute DNA in buffer solution to a final concentration of 2.5 ng/l.

8.10.2. Deposit drop on freshly cleaved mica.

Glue a piece of mica to a metal support as described in section 8.8.5. Cleave mica
substrate with a piece of adhesive tape. Place 30 l of the DNA solution in the center of mica disk. The DNA will bind to the mica within 1 minute.

8.10.3. Prepare AFM and fluid cell

Load prepared sample onto the AFM scanner and assemble the fluid cell, as previously described in Section 8.8.5. It may be helpful to wait for the temperature of
the buffer to stabilize (20 minutes or more) before imaging.
The sample is now ready for TappingMode imaging.

8.10.4. Acknowledgments
Digital Instruments, Inc. wishes to express its appreciation to the following
individuals for sharing their experience to assist in preparing this section: Monika
Fritz, Manfred Radmacher, Magdalena Bezanilla, Helen G. Hansma, Paul Hansma,
Jason Cleveland, Jan H. Hoh, Serge Magonov, Chris Johnson, Don Hersch, Tom
Kovaleski, Gouliang Yang, Jamie Vesenka, and Eric Henderson.

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8.11. Troubleshooting Tips

8.11.1. Cantilever Tune plot looks badloose fluid cell or tip
Become familiar with the characteristics of the Cantilever Tune plot when good
images are obtained. The Cantilever Tune plot can be used as a diagnostic tool. If
the plot looks substantially different from previous successful experiments, there
may be a problem with the fluid cell: for example, the cantilever may be loose in its
holder.

8.11.2. 8O-ring slides across sample surface, causing drift

See Chapter 15 (Section 15.10.20) in this manual.

8.11.3. Laser Sum Signal absent or weakair bubbles

Check that all bubbles are removed from the cantilever. Bubbles may attach themselves to the cantilever, causing the laser beam to be diffracted. Bubbles can sometimes be removed by gently squirting the tip and sample with a stream of fluid. Do
not squirt or splash fluid into spaces above the protective skirt.

8.11.4. Poor image qualitycontaminated tip

Some types of samples may adhere to the cantilever and tip (e.g., certain proteins).
If tip contamination is suspected to be the problem, it will be necessary to protect
the tip against contamination. There are at least two ways of accomplishing this:
a) If the sample is adhered to a surface through diffusion (e.g., diffusion of protein
onto mica) it may be necessary to first diffuse the sample substance into the substrate, then flush away stray substance by using a straight fluid media. The tip is
then lowered into a fluid containing little or no stray substances which may adhere
to the tip.
b) If the sample is short-lived and must be imaged quickly, it may be possible to
mask the tip against contamination by bringing the tip into gentle contact with an
uncontaminated substrate surface. This may be accomplished by first putting the
MultiMode into contact AFM modeswitch the AFM mode parameter on the
Other Controls panel to Contact. Engage the substrate surface using a zero scan
size.
While the tip is kept in gentle contact with the substrate surface, the sample substance to be imaged may be added to the petri dish and allowed to diffuse/settle
onto the substrate. After a diffusion/settling period has lapsed, the tip may be

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quickly lifted from the substrate surface, switched to TappingMode, then used to
image the sample before it becomes contaminated.

8.11.5. Unable to locate particulate samplesattraction to cantilever

Some particulate samples such as proteins may prove difficult to find directly
beneath a cantilever if the cantilever has remained stationary during a diffusion or
settling period. This may be due to the fact that some types of particulates are more
attracted to the cantilever than to the substrate intended to support them. The result
is a shadow on the substrate directly beneath the cantilever where fewer sample
individuals can be locatedthey are stuck to the cantilever.
If this problem is suspected, simply shift the imaging site to a location outboard of
the tip and cantilever. More individual samples should be found there.

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MultiMode Instruction Manual

Chapter 9

Scanning Tunneling
Microscopy (STM)

STM

9.1. Introduction
STM relies on tunneling current between the probe and the sample to sense the
topography of the sample. The STM probe, a sharp metal tip (in the best case,
atomically sharp), is positioned a few atomic diameters above a conducting sample
which is electrically biased with respect to the tip. At a distance under 1 nanometer
(.001 m), a tunneling current will flow from sample to tip. In operation, the bias
voltages typically range from 10 to 1000 mV while the tunneling currents vary
from 0.2 to 10 nA. The tunneling current changes exponentially with the tip-sample
separation, typically decreasing by a factor of two as the separation is increased 0.2
nm. The exponential relationship between the tip separation and the tunneling current makes the tunneling current an excellent parameter for sensing the tip-to-sample separation. In essence, a reproduction of the sample surface is produced by
scanning the tip over the sample surface and sensing the tunneling current. The first
STM operated in ultrahigh vacuum on cryogenically cooled samples. In the years
following its invention, many variations on the STM theme appeared. P.K. Hansma
and J. Tersoff wrote a good review article on the subject, containing experiments,
theory, and over 100 references for The Journal of Applied Physics, 61 pp. R1-23,
Jan 1987. Digital Instruments, Inc. introduced the first commercial STM, the NanoScope I, in 1986.

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9.1.1. Overview of STM

MultiMode SPMs shipped before spring 1996 were provided with STM tipholders
that fitted to the MultiModes standard head. Units shipped after this time must be
fitted with MultiMode STM converter heads as shown in figure 9.1. These provide
improved stability and visual access to the sample.

Figure 9.1. STM converter head.

There are three types of STM converter heads available: a standard version which
measures current in the nanoampere range (Model #MMSTMC), a special, lowcurrent version which measures current in the picoampere range (Model #MMSTMLC), and an electrochemistry version (Model #MMSTMEC). The low-current
converter head includes an in-line electronics package; information regarding the
low-current head is available in Support Note 222.
The STM option is generally employed under the following conditions:

For samples having deeply relieved features, where AFM probes may not be
able to penetrate, and/or where feature verticality is very close to 90 degrees.

On polished samples, where it is necessary to image different layers having

similar topography but different electrical conductivities.

Under conditions where contact with the sample surface is prohibited.

STM relies on a precise scanning technique to produce very high-resolution, threedimensional images of sample surfaces. The STM scans the sample surface beneath
the tip in a raster pattern while sensing and outputting the tunneling current to the
NanoScope control station. The digital signal processor (DSP) in the workstation
controls the Z position of the piezo based on the tunneling current error signal. The
STM operates in both constant height and constant current data modes,
depending on gain settings on the Feedback Controls panel. The DSP always

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adjusts the height of the tip based on the tunneling current error signal, but if the
feedback gains are low (e.g., Integral gain < 1.0; Proportional gain < 0.5), the
piezo remains at a nearly constant height while tunneling current data is collected.
With the gains high (e.g., Integral gain > 1.0; Proportional gain > 0.5), the piezo
height changes to keep the tunneling current nearly constant, and changes in piezo
height are used to construct the image. The exponential relationship between tipsample separation and tunneling current allows the tip height to be controlled very
precisely. For example, if the tunneling current stays within 20 percent of the setpoint value (the current to be maintained by the feedback system), the variation in
the tip-sample separation is less than 0.02 nm.

9.1.2. STM hardware

Some individual STM components are described below:
Converter head and tipholder The STM converter head (so-called because it
"converts" the MultiMode to a scanning tunneling microscope) consists of a rigid
ring bisected by a solid support for the tipholder. Because of the converter heads
compact construction, it holds the STM tip rigid, minimizing vibrational noise. The
converter head features a built-in preamplifier.
Tips Probes for the NanoScope STM must be less than 0.012" in diameter to fit
into the tipholder. The two most commonly used tips are made from either a platinum iridium (PtIr) alloy or tungsten. The PtIr tips are mechanically formed and can
be purchased directly from Digital Instruments. At the end of this chapter, instructions are provided on how to etch tungsten tips from tungsten wire with an electrochemical process. In general, PtIr tips provide better atomic resolution than
tungsten tips, but tungsten tips are more uniformly shaped. They may perform better on samples with steeply sloped features such as compact or optical disks.
PreampMounted within the converter head is a circuit which contains the
preamplifier for the tunneling current and provides interconnections to the MultiMode SPM electronics.
The preamplifier is an FET input amplifier with an input bias current of 25 picoamps, which is small compared to the nanoamps (or fractions of nanoamps) being
measured. The preamp is configured such that the tunneling tip is connected
through a 1 megohm resistor to ground. The tip is also connected to the input of the
amplifier which is wired as a x100 non-inverting amplifier with a cutoff frequency
of 15 KHz. The transimpedance gain of the input resistor/preamp combination is
100 mV/nA with an input range from 0 to 100 nA. The noise of the preamp is
essentially the Johnson noise in the 1 megohm resistor and the standard filtering is 2
mV rms, equivalent to an input tunneling current of 0.02 nA rms.

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A disadvantage of this amplifier configuration is that there is a voltage drop across

the 1 megohm resistor which raises the voltage of the tip above ground, reducing
the effective bias voltage. The actual bias voltage is equal to:
Vsample = Vbias - Itunneling x Rinput
This effect is accounted for in the NanoScope III software so the actual bias voltage
between the tip and the sample agrees with the menu value.

9.1.3. Fine points of STM operation

Getting the best images on the NanoScope III requires a good interface between
sample and tip, reasonable vibration isolation, and proper settings in the software
menus. This section provides greater detail on the operation of the STM.

9.1.3.1. STM operating modes

Recall that the two operating modes available on the NanoScope STM are selected
with the Data type option in the Channel panel (refer to figure 9.2). Height data
reflects the change in tip position required to maintain a constant tunneling current.
The DSP senses the tunneling current, calculates the difference from the desired
tunneling current, and determines the voltage that must be applied to the piezo tube
to keep the tunneling current constant. Due to the known characteristics of the
piezoelectric material, the change in voltage applied to the piezo tube translates
directly to a change in distance. This distance data is recorded throughout the scan
and displayed on the screen as the height of the sample.
Channel 1
Data type:

Height

Z range:

30 nm

Line direction:
Scan line:

Retrace
Main

Realtime Planefit:

Line

Offline Planefit:

Full

Highpass filter:

Off

Lowpass filter:

Off

Figure 9.2. Typical STM Channel 1 control panel parameters.

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Current data is a measure of the tunneling current at each point tested on the sample. The DSP measures the voltage drop across a resistor in series with the tip and
calculates the tunneling current as the tip scans the surface of the sample. The tunneling current at each data point is recorded and displayed on the screen. It should
be noted that if different chemical species are present in a sample, the height data
may not be a direct representation of the topography of the surface of the sample.
Different atomic species within a sample may produce larger tunneling currents for
a given bias voltage.
The two scan modes (height and current) require subtle changes in the menu parameters to operate effectively. The parameter changes also affect the application of the
two modes. To operate effectively in collecting height data, the tip must closely
track the sample surface. The gains must be maximized to force the piezo to
respond quickly to the variations in the sample surface. The height mode is used for
most applications. Conversely, the gains must be very low to keep the piezo from
responding while collecting current data. After engaging, the tip scans the surface
of the sample with very little variation in the piezo height. This constant height provides a reference from which to measure and record the fluctuations in the tunneling current. The current mode is most useful for imaging atoms with relatively
small scan sizes.

9.1.3.2. STM-specific menu parameters

In addition to the Data type discussed above, the STM control panels contain three
items that are specific to the operation of the scanning tunneling microscope. The
Feedback type, Bias, and Setpoint parameters pertain exclusively to the control of
the STM.
The Feedback type parameters in the Other Controls panel determine the transformation performed on the tunneling current prior to the feedback calculations.
The three settings select Linear, Log, or Boost operations. Remember that tip-tosample separation is proportional to the log of the tunneling current. The Linear
selection causes the error signal for the feedback loop to be the difference between
the instantaneous tunneling current and the setpoint current. The Log and Boost
selections calculate the error signal as the difference between the log of the instantaneous tunneling current and the log of the setpoint current. The Boost mode performs additional operations to optimize the feedback performance for high scan
rates over rough surfaces.
The Bias parameter controls the magnitude and sign of the bias voltage applied
between the tip and the sample. A bias voltage encourages the tunneling current to
flow. Although settings of 20100 mV are typical for conductive samples, the
allowable setting ranges from -10.010.0 Volts. Positive settings of the bias voltage induce negative tunneling currents (i.e., electrons flowing from the tip-to-sample).
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9.1.3.3. Optimization of STM scanning parameters

The process of selecting and optimizing scan parameters can be streamlined. In
most cases the scan parameters are dictated by the sample. The Data type is usually
the first parameter set and the Proportional and Integral gains are directly related
to the Data type. The Scan size depends on the sample and the features of interest.
The maximum Scan rate is usually related to the Scan size. The Bias voltage and
the tunneling current Setpoint depend on the sample. Usually, they are set at a standard value for engagement and fine-tuned along with the gains and filters to
enhance the quality of the image.
As discussed above, a Data type of Current is the best for atomic-scale images.
This mode is not practical for rough surfaces, because the tip will crash into the surface at low feedback gains. Having Data type set to Height is usually better for all
but atomic-scale scans. In general, height data images are best at higher feedback
gains and slower scan rates.
Settings for feedback gains depend on many factors, but perhaps the most important
is the Data type. If the Data type is set to Current, the Integral and Proportional
gains should be set as close to zero as possible. The LookAhead gain adds information from the previous scan line into the feedback calculation, so it is most useful for samples with long features oriented along the slow scan axis. The gains
should be lowered for data captured using the linear Feedback type (Lin), especially with high Setpoint current levels. Large-scale images should be taken at
increased gain, except for the LookAhead gain, which is best kept to zero (0).
When Data type is set to Height, often the best way to set gains is to view the Real
Time scan in Scope Mode with the Slow scan axis set to Disabled. This allows the
feedback to be tuned while looking at a single scan line of data. First, increase the
Integral gain until oscillations start to appear, and then, back off a little. Next,
adjust the Proportional and LookAhead gains. High frequency fuzz will appear
on the signal when the Proportional gain is set too high. Setting the LookAhead
gain too high will cause oscillations in the scope image and ripples on topview
images. Setting the LookAhead gain even higher will cause the feedback loop to
become unstable. The Setpoint current and the Bias voltage can also be adjusted
using the scope display.
Bias voltages below 20 mV usually provide the best quality images on samples
with surface conductivities equal to or better than graphite, but there are exceptions.
Resistivity across the surface of a sample can be measured with an ohmmeter. For
samples with high resistivity (greater than 1 megohm/cm), bias voltages of 100 mV
or even higher may work best. For scans larger than 0.5 m, it is sometimes better
to increase the bias voltage by 50 mV to 100 mV over the value for smaller scans. A
higher bias keeps the tip further from the surface, giving the feedback loop greater
tolerance in tracking the surface at high speeds.

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Increasing the Setpoint current can also be helpful for larger scans. This has the
effect of raising the gain, but also brings the tip closer to the surface by a small
amount. High setpoint currents of 6 nanoamps or more can also be useful in
improving the signal-to-noise ratio for atomic images on some materials.
The Feedback type can be set to either Log, Boost, or Linear input transformations. Because the tip-to-sample separation is proportional to the log of the tunneling current, the transformation performed on the tunneling current prior to the
feedback calculation can have dramatic effects on the performance of the feedback
loop. Linear input is more protective of the tip, because the feedback error signal
responds exponentially to tip-sample separation. When the tip-to-sample separation
decreases, the error signal rises exponentially, quickly driving the tip away. However, the error signal is unsymmetrical. The same sample-to-tip separation change
that caused the tip to move away so quickly will generate a small error signal when
the tip is higher than it is supposed to be. This unsymmetrical response in linear
(Lin) mode will distort data. For this reason, the Boost and Log modeswith ln(I)
used in the feedback calculationare preferable for most samples, because they
respond in a more symmetrical fashion to positive and negative sample slopes. The
Boost mode is preferable for large scans with high vertical features such as compact disc stampers or integrated circuits. The proportional and integral gain can be
reduced greatly when the Boost mode is used. The log input has the advantage of
having a gain which is insensitive to the value of the Setpoint current.
Large scans cannot be taken at the same scan rate as small scans. When using the
large scanners with scans above a few microns, the Scan rate should be lowered
below 10 Hz. Best results can be obtained at scan rates of 1 Hz or less, although
image-taking is slow. At these scan rates, the 128 X 128 and 256 X 256 data formats are most useful, quadrupling and doubling the frame rate over the 512 X 512
format for a given scan rate. To ensure there is no image degradation due to a high
Scan rate, lower the rate and check for changes in the image. Check the Scope
Mode view to ensure that the scan is not slew-rate limited in Z, as evidenced by an
artificial sawtooth appearance in the scope trace.
The Highpass and Lowpass filter parameters provide the option of filtering the
tunneling current signal. A lowpass filter with a cut-off frequency of 25 KHz can be
applied to the analog tunneling signal in hardware. Typically, the filter is selected
for atomic-scale images; otherwise, no filtering should be selected.

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9.1.3.4. Tunneling tips

Although the microscope will accept any .010" diameter tip, tips made of platinum
iridium (PtIr) and tungsten are used most often. PtIr and tungsten tips are supplied
by Digital Instruments. Tungsten tips can be electrochemically etched from tungsten wire by following instructions at the end of this chapter. In general, most of the
discussion in this manual involving tips and noise reduction applies to both types of
tips, but there are some applications which are tip specific.
PtIr tips seem to give better atomic resolution than tungsten in air and liquids, probably due to the lower reactivity of platinum. The PtIr tips are not as uniformly
shaped as the tungsten tips, so freshly etched tungsten tips may provide cleaner data
when scanning steeply sloped surfaces such as compact or optical disks. For tunneling on surfaces immersed in conductive liquids, coated tips have been used. Glass
coatings are removed from the very end of the tip by briefly applying a high-bias
voltage. The quality of the mechanically formed PtIr tips will vary. Some give beautiful images as soon as tunneling starts; others start well but degrade over time;
while others start noisy and stay noisy.

9.1.3.5. Sample surface

Samples to be imaged with a scanning tunneling microscope must conduct electricity to some degree. In many cases nonconductive samples can be coated with a thin
layer of a conductive material to facilitate imaging. The sample surface must be
conductive enough to allow a few nanoamps of current to flow from the bias voltage
source to the area to be scanned. NanoScopes have been used to scan gold, silver,
platinum, nickel, copper under oil, chrome plating, doped silicon under oil, conducting polymers, amorphous carbon, blue diamond, diamond-like carbon films,
carbon fibers, graphite, iron-oxide compounds, semi-metals, doped semiconductors
(molybdenum disulfide), cobalt-chromium compounds, stainless steel, liquid crystals, and other materials. Oxide layers more than a few atoms thick on the sample
tend to affect the scanning and wear down the tip as it is dragged through the oxide.
The feedback loop will extend the tip until a tunneling current flows, even if it must
push the tip through an oxide layer (if it can). If oxide presents a problem, keep the
sample covered with oil or operate the microscope in a glove bag filled with nitrogen or argon. The standard NanoScope microscope heads were not designed to
operate in UHV.
On samples which are noisy or tend to oxidize, tunneling under oil or scanning in a
glove box filled with inert gas can improve the imaging. Silicon oil or paraffin oil
(mineral oil) also work well with some samples. The only problem involved with
the use of oil is the increased difficulty in the coarse positioning of the tip. The
reflection of the tip comes off the liquid instead of the surface of the sample. It is
difficult to tell when the tip is close to the sample surface. The best approach is to
lower the tip until it just touches the surface of the oil, then select Engage.

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9.1.3.6. Vibration isolation

The microscope should be isolated from sources of vibration in the acoustic and
subacoustic frequencies. This requirement can be relaxed somewhat for large-scale
images, but atomic-scale work is extraordinarily sensitive to ordinary room vibrations.
As a final note, the best way to reduce coupling from vibrations is to eliminate as
many sources of vibration as possible. Remember that vibrations can be transmitted
to the microscope over the cable. To reduce this phenomenon, prevent tension in the
cable and keep it away from fans and other noise sources. Also, keep the microscope away from sources of acoustic noise. Loud conversation can disrupt atomic
scale images. Air currents can also disturb atomic images, so it is best to run the
microscope with the hood or similar cover on.

9.2. Basic STM Operation

9.2.1. Imaging samples
This section explains how to use the NanoScope to image a conductive sample
(e.g., the 10-micron, silicon reference supplied with the system).
1. Select the STM option. Click the left mouse button with the cursor on the Real
Time icon in the menu bar to select the Real Time operating mode. Pull down the
Microscope menu by clicking on the Microscope item in the menu bar, click on
the Select command, then click on STM and Ok to place the microscope into STM
mode.
2. Attach a sample to a metal puck using an electrically conductive (e.g., silverbased) epoxy such as Dynaloy 325 or equivalent. Ensure that the sample itself is
conductive and in electrical contact with the top of the scanner tube (the scanner
cap).
3. Insert a new tip in the STM converter head tipholder. The tips come in a small,
plastic snap-box filled with foam. Grip the tip with tweezers near the sharp end,
then insert the blunt end of the tip into the tipholder. On some older tipholders, it
may be necessary to put a slight bend in the tip to help it stay in; newer tipholders
feature a curved tube to help grab the tip better. The tip must be inserted so that it
protrudes beyond the bottom profile of the tipholder; otherwise, the tipholder will
bottom out on the sample surface before the tip engages. Ensure that the tip is
tightly held.

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4. Place the converter head atop the scanner, checking for clearance between the tip
and the sample as the head is lowered. If the tip appears to be too low and threatens
to crash into the sample, adjust the scanner screw(s) to obtain more clearance. The
head will sit securely atop the scanner under its own weight, assisted by the pull of
magnets mounted in the scanner.
5. Verify that the mode switch on the MultiModes base is toggled to STM. The
LED on the front of the base should glow blue. For "J" scanners, set the Scan Controls panel parameters to the values shown below. It is sometimes helpful to start in
Scope Mode (Real Time / View / Scope Mode) at a reduced Scan size. Once gains
are adjusted for the small scan, the Scan size may be increased.
Scan Controls
Scan size:

10.0 m

X offset:

0.00 nm

Y offset:

0.00 nm

Scan angle:
Scan rate:
Number of samples:
Slow scan axis:
Z limit:

0.00 deg
2.44 Hz
256
Enabled
440 V

Go to the Feedback Controls panel. To prevent crashing the tip into the sample,
verify that the Integral gain value is set at 12, and that the Proportional gain
value is set between 210. For now, turn off the LookAhead gain (0.00). Set the
Bias to 100.0 mV1.0 V, and Setpoint to 2 nA.

Notes

The Bias and Setpoint parameters must be set according to the conductivity of
the sample. Samples which are excellent conductors (e.g., gold) exhibit high
electron flow; therefore, the error signal is relatively large. Good conductors can
operate with a Bias of 150 mV. Conversely, if the sample is a semiconductor,
the Bias may have to be set higher (e.g., 100 mV) to obtain an image. Beware of
high bias values! If the Bias is set too high for a given conductor, electrical
arcing may occur, damaging the tip and/or sample.
6. At this point, the value of the head preamplifier offset may be measured using the
Offset command in the Real Time / Microscope menu. Checking the Offset is recommended as a good final check prior to engagement. The procedure is as follows:

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Verify that the tip is withdrawn from the sample surface.

Invoke the Offset command to observe the offset current of the preamplifier in
nanoamps. The offset should read 0.1 nA. If the value is too high, check that
all cables are plugged in, that the MMAFM switch is set for STM, and that the
tip is not touching the sample.
7. Engage the sample surface by selecting the Motor / Engage option or by clicking on the Engage icon. The display monitor should render an image of the sample
surface immediately. Depending on the condition of the tip, the image on the screen
will be either clear or noisy. The status bar on the control monitor shows how many
microns the tip has traveled. When the tip engages with the surface and tunneling
occurs, the computer will beep and an "Engaged" message will appear in the status
bar.
The Z Center Position bar graph to the right of the image on the display monitor
reflects the Z position of the piezo during the scan. Under most circumstances, the
white bar should be in the center of the graph, indicating that the Z voltage for the
piezo is fluctuating around zero volts. If the sample is not level, or if there is drift in
the mechanical system after the tip has engaged, the Z center position will fluctuate
during the scan or drift off-scale.
8. After the sample is engaged, the Scan Controls and Feedback Controls parameters will probably require some adjustment to optimize the image. Carefully and
slowly increase the Integral gain and Proportional gain and vary the Bias voltage
to see how the image changes. (Sudden changes to these parameters may cause a
crash!) Vary the Scan size to observe how the image can be magnified, then vary
the X offset and Y offset to see how the image can be moved. Transfer to the Channel panels, and instead of displaying an image using height data, select Current at
the Data type field to observe image changes.

Notes

Generally, the Date type field is set to Height on the Channel panel whenever
the Multimode is used in STM mode to image sample surfaces with large fields
of view. The Current setting is usually selected for imaging atomic features.
9. Click on the Scope Mode command in the View menu (or use the Scope Mode
icon) to see what the signal looks like for each scan. Return to Image Mode by
clicking on the View / Image Mode command or the Image Mode icon.
A poor tipeither because it has touched the sample, has contamination on the
end, or because of its manufacturingwill render a poor image. In this case, there
is little likelihood that the tip will recover and the best procedure is to replace the

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tip. Pull down the Motor menu by clicking on Motor in the menu bar, then click on
Withdraw (or click on the Withdraw icon) to stop scanning, and retract the probe
from the surface. After the tip is withdrawn, the Secured message will appear in
the status bar of the control monitor. Remove the bad tip and install a new one. Verify there is sufficient clearance between tip and sample after installing the new
tipa new tip will extend a different distance out of the tipholder than the old tip.
To Improve Image Quality...

Vary the Scan size and the X offset and Y offset. Move to a new location on the
sample by changing the X offset and/or Y offset of the scan. The X and Y offset
parameters define the center of the scan. Often, a better image can be obtained
on a different portion of the sample. The X and Y offsets can be changed by
altering the values in the control panel, or by using the Offset command in the
menu bar on the display monitor.

Alternate the commands Withdraw and Engage a couple of times. This raises
and lowers the tip and may get rid of contamination on the end of the tip.

Use the Step Motor command to single-step the tip up a step or two. Be sure to
minimize the SPM step size before stepping the motor down. Watch the Z
Center Position scale on the display monitor to verify that the piezo has
sufficient room to retract so the tip will not harm the surface of the sample.
Stepping the tip down until the Z Center Position goes to the retracted end of
the scale where the indicator turns red will usually destroy the tip.

Vary the Setpoint current over the range 2 to 10 nA. As a last resort, current
may be increased up to 48 nA for a very brief period of time.

As a last resort, oscillate the tip by setting the Integral gain high (about 100)
for a second. The oscillation will show up on the display as a grainy pattern of
light and dark. Set the Integral gain back down and check if the signal is
quieter than before. Setting the Integral gain high for a brief period is also useful
for cleaning debris from the tip.

If none of the above procedures improves the quality of the signal, replace the
tip and try again. If that doesn't work, call Digital Instruments for technical
assistance.
10. After a clean image has been obtained, it can be saved onto disk with the Capture command in the Capture menu (or click on the Capture icon) . The Capture
command saves the current scan image (or the next image if any changes have been
made in the STM control panel) into the Capture directory. The Capture Filename command can be used to define a custom filename or the captured file will be
named with a date/time stamp. In either case, a three-digit suffix which is incremented after each capture operation is appended to the filename. If the date/time
stamp is used, a file captured at 3:32 p.m. on July 31 would be assigned the file

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name 07311532.001. A second file captured the same minute would be named
07311532.002, etc.
11. Some simple filtering operations can improve the look of the captured image.
Enter the Off-line mode and select an image by clicking on it in the file list. There
are a number of image processing options available in the Off-line / Modify menu.
Click on Modify in the menu bar to display the menu. The simplest way to remove
high frequency noise is using a lowpass filter.
Pull-down the Modify menu and click on the Lowpass command to apply the lowpass filter to the image and redraw it on the display monitor. Successive Re-execute
clicks will continue to filter and redraw the image. The entire filtering operation can
be undone with the Undo command, the filtered image can be saved, or the Quit
command will return the system to the Modify menu. There is also the option of
changing the display with the Color table, Color contrast, or Color offset parameters.

Notes

The Z range parameter will have no effect if the Plot type parameter in the Top
View menu is set to Equal area.

9.3. Spectroscopy with the STM

The NanoScope STM performs limited spectroscopic operations under the two
scanning tunneling spectroscopy STS modes of operation. The variation of the tunneling current due to variations of the bias voltage or tip-to-sample separation can
be tested and recorded at a single point with the View / STS Plot modes. These are
discussed in this section. A related form of imaging, current imaging tunneling
spectroscopy (CITS) is described in an appendix of the Command Reference Manual.

9.3.1. STS plot modes

In the STS Plot modes, the tip is positioned at a point on the surface, and a spectroscopic plot is acquired and displayed in a scope format. Between plots, the feedback is run to establish the tunneling current to the setpoint value. The different
types of STS Plots that can be acquired are:

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STS i(v) The tunneling current as a function of the bias voltage is displayed. The
tip height is held constant while the current (I) versus voltage (V) plot is being
acquired. In addition to I versus V, it is also possible to plot the following:
di
------ versus V
dv
d ln ( i )
---------------versus V
dv
d ln ( i )
----------------versus V
d ln ( v )

STS i(s) The tunneling current as a function of the tip height is displayed. The
bias voltage is held constant while the current (I) versus tip height (S) plot is being
acquired. In addition to I versus S, it is also possible to plot ln ( I ) versus S.

9.3.2. Operation of STS

In the following sections, the operation of the spectroscopic functions of the NanoScope III STM will be discussed. Additional information can be obtained from the
Command Reference Manual.
STS Plot
There are several items that you should be aware of when using the NanoScope to
acquire spectroscopic plots with the STS Plot commands. The spectroscopic capabilities can provide information that can help to distinguish different species
although exact species identification is difficult, especially in air. The spectroscopic
plots should aid in comparative studies between samples or between different
regions on a sample, but they will not reveal the precise make-up of that sample.
A comparison to STM imaging reveals two somewhat conflicting requirements. As
a good starting point, the sample and tip should produce consistent STM images.
The images should repeat well from frame to frame and be fairly free of noise or
areas on the surface that appear unstable. For current-versus-voltage type plots, the
spectroscopic plots may be nice and smooth and repeat well, but switching back to
the STM imaging mode reveals images which are quite noisy. This can be attributed
to the fact that the quality and uniformity of the tip is probably more critical for
imaging than for making the rather simple spectroscopic plots. This is generally not
true for the I vs. S plots. Some general recommendations for acquiring spectroscopic plots are:
1. Low settings for the Integral gain are preferred. Since the tip is not tracking any
topography, the lower gains are acceptable and tend to make the plots more stable.

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2. The maximum input range of 100 nA on the NanoScope with the standard
preamps will restrict the current-versus-voltage plots.
3. The spectroscopic functions do not adjust for any loss of bias voltage due to IR
losses caused by the input impedance of the preamplifier. This has different effects
for the STS i(v) and STS i(s) functions which are discussed individually below:
STS i(v)
The spectroscopic plots do not correct for reductions in bias voltage caused by the
preamplifier, which for current-versus-voltage is typically small, anyway. For
example, a 1-volt scan on the bias voltage, producing a 50 nA response in the tunneling current would have a 5 percent error at the extremes of the scan (50 nA X 1
M = 50 mV or 5 percent of 1 volt).
Input impedance of the preamplifier leads to reduced bias voltages at increased tunneling currents. This effect can cause the I vs. S plot to be inaccurate. For example,
a bias voltage of 20 mV will restrict the upper limit of the tunneling current to 20
nA since that level of current would effectively reduce the bias voltage to zero.
Even before the tunneling current gets to 20 nA, the reduced bias voltage will make
the measured current appear lower than it should be for a given tip height.

9.3.3. Continuous Imaging Tunneling Spectroscopy (CITS)

For information regarding CITS, see Appendix C in the Command Reference Manual.

9.4. Obtaining Images with STM

This section gives suggestions for obtaining STM images. Procedures are included
for imaging:
1. Highly ordered pyrolytic graphite (HOPG).
2. A gold calibration ruling.
Note that vibrational stability is crucial to obtaining atomic-scale images. This is
achieved through the use of vibration isolation and, more importantly, the use of
shorter, more rigid scanners (e.g., "A" or "E" scanners). In some limited cases, it
may be possible to obtain atomic-scale images using larger scanners ("J"); however,
this often proves difficult or impossible for certain materials.

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9.4.1. Imaging highly ordered pyrolytic graphite (HOPG)

This section describes how to use the NanoScope to image graphite atoms in highly
ordered pyrolytic graphite (HOPG).
1. The microscope should be placed on a vibration-isolation platform and connected to the controller. (You may find it easiest to perform this at step 5 below.)
2. As it comes from Union Carbide, the HOPG sample is already cleaved and clean
enough for tunneling. There is usually no need to re-cleave the sample. If you feel
an overwhelming need to cleave the sample again, it can be done by carefully pulling off a layer with sharp tweezers or pressing some sticky tape to the surface and
pulling off a layer. You will notice that graphite is slippery and easily dropped. Be
careful! Verify that the sample is electrically bonded to the puck.
3. Insert a new tip in the tip-holding tube mounted on the white ceramic crossmember of the converter head. The tips come in the small plastic snap-box filled
with foam. The tips are inserted into the foam blunt end first so the sharp end of the
tip protrudes from the foam. Grip the tip with a tweezers near the sharp end and
insert the blunt end of the tip into the tipholder. The tip should be inserted so that it
protrudes about 2 mm and should be fairly tight in the tipholder.

Notes

Handle the converter head as little as possible during these operations to prevent
thermal drift.
4. Place the head on the three magnetic balls mounted on the threaded screws in the
scanner. (Make sure that the screws are extended enough so that the tip does not hit
the sample.) The head has a hole, a groove, and a flat which mate kinematically
with the three magnetic balls. A suggested method of placing the head on the scanner is to slowly lower the head while it is slightly misaligned until its underside
touches the screws, then slowly rotate the head until the hole and groove on the
underside mate with the screws (all the while watching the tip-sample separation).
If it looks like the tip will hit the sample, toggle the motor switch Up to raise the
head and/or use the coarse adjustment screws.
After the head is securely mounted on the magnetic balls of the base, insert the 15pin preamp plug into the socket on the scanner support ring. When placing the head
down onto the balls, try to prevent it from slamming onto the balls, as excessive pitting in the flat area can cause irregular engagement.
5. Looking at the tip with the 25X magnifier, lower the tip down with the coarseadjustment screws until the tip is about a tenth of a millimeter or less (about .004

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inch or less) above the sample. It is usually easier to use only one coarse-adjustment screw to do this if you do not need to move the tip too far. Try and adjust the
screws such that the head is not tilted to one side or the other. If necessary, adjust
the rear screw so that there is a minimal amount of tilt in the head from front to
back. A reflection of the tip will be visible on the sample. Using the coarse-adjustment screws, lower the tip until there is only a slight gap between the end of the tip
and its reflected image do not bring the ends together. If you do, you will almost
certainly have to replace the tip. Don't worry at this point if the head is tilted.
If you haven't placed the microscope on the vibration-isolation platform, do so now.
Verify that the mode switch on the left side of the MultiModes base is toggled to
STM.
6. Be sure the power to the controller is on. If you have not already done so, start
the program by entering "Z".
7. Set the scan parameters. Pull down the microscope menu by clicking on the Real
Time / Microscope /Select command, then click on the scanner being used. Click
the Ok button to select parameters for the converter head. The "A" scanner is the
preferable option for imaging on an atomic scale, but the "E" scanner has also been
used effectively.

To look at graphite atoms, it is necessary to set the Scan size to about 520 nm.
Use the mouse to change the parameter. Select the parameter and drag the
mouse right and left with the left button pressed to change the parameter; the
new parameter value will take effect when the mouse button is released. The
right or left arrow keys can also be used to set this parameter. Note that the up
and down arrow keys move from one item to the next, while the right and left
arrow keys change the selected parameter. Numerical parameters may also be
set by simply typing over the existing values and pressing the enter key.

Set the remaining parameters so that the Feedback Controls panel is as shown
in figure 9.3 below.
8. As a final check, click on the Offset command in the Real Time / Microscope
menu. The offset should be very close to 0.0 nA. Proceed to the next step if the system reports a reasonable value.
If the offset reads 99 nA, the feedback loop is open (i.e., the microscope or controller cables are not properly installed), or the tip may be in contact with the sample surface. Check this by clicking on the Withdraw command and retesting the
offset . Remedy this problem before continuing.

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Feedback Controls
Integral gain:

2.00

Proportional gain:

2.00

LookAhead gain:

0.00

Bias:

20.0 mV

Setpoint:

2.00 nA

Analog 1:

0.00 mV

Analog 2:

0.00 mV

Figure 9.3. Feedback Controls panel for graphite.

9. Now, let's start tunneling. Click on the Real Time / Motor item and then click on
the Engage command, or use the Engage icon. The status bar on the control monitor shows how many microns the tip has traveled. If the travel distance gets up to
250 microns, engagement will halt and the software will prompt you to check the
tip alignment. When the tip engages with the surface and tunneling occurs, the
computer will beep and an "Engaged" message will appear in the status bar.
If the message "Engaged" occurs immediately after the engage command is given,
there is a problem. Either the tip was already touching the surface due to misadjustment of the coarse-adjustment screws, the power to the controller was not turned
on, the wrong head was selected, or the 15-pin connector to the scanner was not
connected. If the tip was on the surface, you can try backing off the screws and try
again. However, after the tip has crashed into the surface, the images will tend to be
unacceptably noisy. To try again, click on the Withdraw command. The "Secured"
message will appear in the status bar of the control monitor. Then, click on the
Engage command.

Notes

If version 4.22 or higher software is used, the STM must have the In polarity
parameter set to Forward on the Microscope / Calibrate / Detector panel. On
older microscopes, the setting didnt matter and may have been set to Reverse.
This setting will cause false engagement with newer Z.exe programs.
10. At this point, an image should begin to form on the screen. Depending on the
condition of the tip, the image on the screen will be either clear or noisy. Let's treat
the two cases separately:
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A good signal is one which clearly shows the repeating pattern of the carbon
atoms. Compare this image with the graphite image that may be stored in the
C:\DATA directory. Check to see how the image repeats on scans from bottomto-top and top-to-bottom. Usually, when the tip is first engaged, there will be a
drift in the piezo which will cause the image to repeat poorly. The most obvious
sign of drift is features which are compressed vertically in one frame and
vertically elongated in the next frame. This drift will decrease with time.
Click on a scan parameter and drag the mouse to change the parameter. Lower the
Integral and Proportional gains near zero and vary the Bias voltage to see how
the image changes. Vary the Scan size to get a feel for how the image can be magnified and vary the X and Y offsets to see how the image can be moved. Instead of
displaying an image of the tunneling current, select Height at the Data type line to
display the Z (vertical) signal. You will have to increase the gains and decrease the
scan rate to get a good Z-height image.
To use an "E" or "J" scanner on an atomic scale with the Data type set to Height,
the Z limit parameter (Scan Controls panel) should be decreased to 55 Volts.
Click on the Scope Mode command in the Real Time / View menu to see what the
signal looks like for each trace across the sample. Return to the Image Mode by
clicking on the View / Image Mode command, or icon.

A poor tip, either because it has touched the sample, has contamination on the
end, or because of its manufacturing, will give a noisy signal. In the worst case,
the image will have no pattern at all, and Z on the display will run off scale in
both directions. In this case, there is little likelihood that the tip will recover, and
the best procedure is to replace the tip. Pull down the Real Time / Motor menu,
then click on Withdraw (or click on the Withdraw icon) to stop scanning, and
retract the probe from the surface. After the tip is withdrawn, the "Secured"
message will appear in the status bar of the control monitor. Before removing
the head, it's a good idea to execute the Withdraw command several times to
protect the sample from being scratched when the head is picked up. Extend the
scanner screws a few turns, unplug the preamp, remove the head, and replace
the tip. Try to leave the new tip protruding the same amount as the old one. Be
sure there is sufficient clearance after installing the new tip, because the new tip
will extend a different distance out of the tipholder than the old tip.

The nominal Z position of the piezo provides useful diagnostic information. The
bar graph to the right of the image on the display monitor reflects the Z position
of the piezo during the scan. Under most circumstances, the "Z center position"
bar should be in the center of the graph to indicate that the Z voltage for the
piezo is fluctuating around zero volts.

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If the sample is not level or if there is drift in the mechanical system after the tip has
engaged, the "Z center position" will fluctuate during the scan or drift off scale. If
the "Z center position" reaches the "Extended" end of the scale, the maximum voltage is being applied to the piezo, but the tip still cannot reach the surface. Similarly,
the "Retracted" end of the scale means that the maximum voltage of opposite polarity has been applied to the piezo, and the tip cannot be lifted from the surface. The
"Retracted" end of the scale is more dangerous, because damage to the tip or sample can result.
If the "Z center position" gets close to either limit, use the Withdraw command followed by the Engage command to reposition the "Z center position" near the middle of its range. If there is drift in the Z center voltage, use the Real Time / Motor /
Step Motor command with a small Step size to keep the tip within the Z piezo
range. This drift will eventually settle out.
EXCEPTION: The Z limit represents only a portion of the maximum Z range
(440 V). When using a Z limit of less than 440 V, version 4.xx software will
attempt to recenter the Z-axis if you double-click on the Z limit value or change it.
Sometimes the tip will show atomic structure on graphite with noise which is large
enough to reduce the definition of the structure. In these cases, it may be possible to
reduce the noise without replacing the tip. Any or all of the following procedures
may be tried1:

Vary the Scan size and the X and Y offsets (Scan Controls panel). Move to a
new location on the sample by changing the X and/or Y offset of the scan. The
X and Y offset parameters define the center of the scan. Often, a better image
can be obtained on a different portion of the sample. The X and Y offsets can be
changed by altering the values in the control panel or by using the Offset
command in the menu bar on the display monitor.

Alternate the commands Withdraw and Engage a couple of times. This raises
and lowers the tip and may get rid of contamination on the end of the tip.

Use the Real Time / Motor / Step Motor command to index the tip down a step
or two. Be sure to minimize the Step size before stepping the motor down.
Watch the "Z center position" scale on the display monitor to be ensure the
piezo has enough room to retract so the tip will not harm the surface of the
graphite. Stepping the tip down until the "Z center position" goes to the
retracted end of the scale where the indicator turns red will usually destroy even
a moderately noisy tip. Sometimes, though, bad tips can be reconditioned by
being driven several steps into the surface and then withdrawn and re-engaged.

1. These suggestions also apply to larger-scale STM imaging and are provided in section
9.2.1 of this chapter.

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Vary the Setpoint current over the range 210 nA. As a last resort, you can
increase it up to 48 nA for a very brief period of time.

As a last resort, oscillate the tip by setting the Integral gain high for about one
second. The oscillation will show up on the display as a grainy pattern of light
and dark. Set the Integral gain back down and check if the signal is quieter than
before.

If none of the above procedures improves the quality of the signal, you should
cleave the sample, replace the tip, and try again. If that doesn't work, review all
parameter settings or call Digital Instruments for technical assistance.

9.4.2. Imaging a gold calibration ruling.

A gold calibration ruling is supplied with systems purchased with the 12-m range,
"E" scanners. This section describes how to image the ruling and assumes you have
performed the previous section for imaging graphite.
1. Although it is not as important for large-scale scans, the microscope should be
put on a vibration isolation platform. Also, connect the microscope to the controller
according to the instructions in the earlier part of this chapter.
2. Attach the calibration ruling to a sample puck with the ruled side facing up. Use
carbon glue or silver epoxy to provide a conduction path between the sample puck
and the top surface of the ruling. This step is very important because without a conduction path the Bias voltage will not be applied to the sample surface and the tip
will crash into the sample surface in a effort to detect the tunneling current.
3. Verify that a tip is in the tip-holding tube attached to the cross-member on the
converter head.
4. Place the head on the three magnetic balls mounted on the adjustment screws in
the scanner. Make sure the screws are extended enough that the tip does not contact
the sample.
5. Looking at the tip with the 25X magnifier, lower the tip down with the coarseapproach screws until the tip is about a tenth of a millimeter or less above the sample. This can be done by bringing the end of the tip as close as possible to the
reflected image without allowing them to meet. If the tip does touch the sample,
replace it, as it will almost certainly be unusable.
6. Be sure the power switch in the right rear of the controller is in the on (up) position. The power lamp on the front panel of the controller will be illuminated.

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7. If you have not already done so, start the main program by entering Z.

Go to the Real Time mode.

Click on the Microscope / Select command, then click on Small Sample
("Base" box), STM ("Head" box) and the appropriate "Scanner" selection (e.g.,
MMSTME if the "E" scanner is being used).
Set parameters in the Feedback Controls panel as shown in figure 9.4. The Scan
Controls panel can have its parameters set as follows: Scan size 100 Volts; Z limit
440 V; Number of samples 256; Scan rate 2.44 Hz. Set the Data type parameter
on the Channel 1 panel to Height.
Feedback Controls
10.00

Integral gain:
Proportional gain:

5.00

LookAhead gain:

0.00

Bias:

500.0 mV

Setpoint:

5.00 nA

Analog 1:

0.00 mV

Analog 2:

0.00 mV

Figure 9.4. STM control panel for calibration ruling

9. Click on the Real Time / Motor / Engage command to begin scanning. (See section 9.4.1 for suggestions on adjusting parameters.) At this point, an image should
begin to form on the screen; the supplied gold sample has cross rulings of 1m
pitch. Go to the Scan Controls panel and increase the Scan size item to 10 m. If
the picture appears grainy or noisy, the tip is probably poor and should be replaced.
In any case, you can try the following procedures to improve the image:

Change the Integral or Proportional gain parameters. Gain values which are
too high will cause graininess in the image, whereas low gains will cause image
smearing, particularly where the surface has sharp, abrupt features.

Vary the Scan rate. A Scan rate which is too high will cause smearing (like a
low gain setting) and lower scan rates may test your patience.

Vary the Setpoint current and Bias voltage items.

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9.5. Troubleshooting for STM

This section addresses errors or malfunctions encountered during the operation of
the MultiMode as an STM. Consult also Chapter 15 in this manual for additional
troubleshooting tips.

9.5.1. . Head and microscope-related problems

This section deals with problems related to the scanners or the microscope. If a
problem exists with a scanner, try a second one under the same conditions, if possible. Otherwise, the following list of symptoms and cures may be helpful:

9.5.2. . Head engages immediately

If the STM engages immediately after initiating the Motor / Engage command,
then one of the following probably occurred:
tip on surface Make sure the tip is not touching the surface of the sample. Adjust
the coarse-adjustment screws upward until the tip is far from the surface.
controller off Verify that power to the controller is on and that the controller is
connected to the computer workstation via the beige 25-pin cable.
MulitMode base switch not set for STM Verify that the switch on the left side
of the MultiMode base is toggled to STM.
head has offset Follow directions in section 9.4.1 to determine whether the scanner requires adjustment to its offset.
In polarity parameter set to Reverse Check to see that the In polarity parameter on the Detector Calibration panel (Microscope / Calibrate / Detector) is set
to Forward.
disconnected Verify that the 15-pin microconnector from the head is plugged
into the microscope and the microscope is plugged into the controller.

9.5.3. Tip never engages

If the tip never engages, test for the following:
disconnectedMake sure the microscope is connected to the controller.
binding on drive screw Feel the rear, motor-driven adjustment screw during
engagement to verify that it is rotating. If the motion is erratic, then the screw is

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fouled with debris and binding. Remove the screw, clean threads and regrease per
instructions provided in section 15.3 in this manual.
bias shortedMeasure the bias by using a voltmeter between the head and stage
chuck. If this is not in agreement with the settings in the Bias voltage item in the
STM Parameter control panel and appears to be grounded, then check to see if anything is providing a conduction path between the Base and the Base Support or any
other ground.
bias not applied to sample surface In some cases (e.g., the calibration reference), the sample consists of a layer of electrically conductive material on top of an
insulator. In these cases, a conduction path must be provided between the sample
puck and the sample surface. Carbon glue or silver epoxy can be used to connect
the bias voltage to the sample surface. With NanoScope software versions 4.23b3 or
later, verify that the In polarity parameter on the Detector Calibration panel
(Real Time / Microscope / Calibrate / Detector) is set to Forward.

9.5.4. Tip crashes

If the tip always crashes into the surface with the Z Center Position either changing erratically or stuck in the fully retracted position, try the following:
check sample conductivityThere are two problems associated with sample conductivity. First, the bulk conductivity of the sample may make it difficult to image.
If the resistance of the sample is greater than 1 Kohm/cm, higher bias voltages
should be tried. If the resistance is greater than 1 Megohm, bias voltages of 100 mV
or more should be used. Samples with resistances 1 Megohm or greater will be difficult to image even with high bias voltages.
Measuring the bulk conductivity of the sample with probes may not tell the whole
story. Probes may easily penetrate oxide or contamination layers on the sample surface yielding reasonable resistance measurements. However, oxide and contamination layers on the sample surface can make imaging very difficult. Higher bias
voltages are required for these types of samples.

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clean contacts The magnetic balls on the ends of the adjustment screws tend to
attract small metallic particles which may make the surface gritty. Clean them with
adhesive tape and then wipe with alcohol. Also, clean the kinematic mating surfaces on the underside of the head.
check for binding in the motorized screw Make certain the motorized adjustment screw rotation is smooth and not erratic, which can cause the screw to
advance in jumps. If this is the problem, clean the screws as described in section
15.3 in this manual. On newer scanners, the setscrew used to adjust tension on the
motorized screws plastic threaded bushing may need to be slightly loosened.
check sample conductivity there are two problems associated with sample conductivity. First, the bulk conductivity of the sample may make it more difficult to
image. If the resistance of the sample is greater than 1 k/cm, higher bias voltages
should be tried. If the resistance is greater than 1 M/cm, bias voltages of 100 mV
or more should be used. Samples with resistances of 1 M/cm or greater will be
difficult to image even with high bias voltages.
Measuring the bulk conductivity of the sample with probes may not tell the whole
story. Probes may easily penetrate oxide or contamination layers on the sample surface yielding resistance measurements. However, oxide and contamination layers
on the sample surface can make imaging very difficult. Higher bias voltages are
required for these types of samples.
check the polarity of the Z-axis piezo Use the Calibrate command in the Real
Time / Microscope menu to review the calibration parameters for the head in use.
The Z polarity should be set to Forward. (EXCEPTION: A few rare scanners
have serial numbers ending in "RP," reverse polarity; these should be set to Reverse
instead.)

9.5.5. Problems during Real Time operation

This section deals with problems that are associated with the Real Time aspects of
the NanoScope III software although they often point to the scanning head or
microscope.

9.5.6. Image goes out of range

If the Z center position tends to go out of range at the edges, top and bottom or right
and left of the scan, then try the following:
Level sample to headThe Z center position is affected by sample tilt, and larger
(e.g., "J") scanners may be less tolerant of sample tilt due to their having small vertical range compared to larger lateral scan range. Note the trend in Z Center Position across the sample scan profile using View / Scope Mode. Verify that the

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sample surface is parallel to the sample puck before mounting it atop the scanner
cap. Also verify that the channel panel (e.g., Channel 1) has its Realtime Planefit
parameter set to Offset or None.
Increase Z limit parameter If set too low, try increasing the Z limit parameter
value (Scan Controls panel).

9.5.7. Z drift
If the Z center voltage tends to drift out of range rather quickly after the head is
engaged, it may be a result of the following:
thermal drift Allow some time for the temperature to stabilize if the microscope
and/or scanner has been stored in a cold place overnight. Drift can be minimized by
keeping the STM in a thermally stable environment. Avoid operating the microscope near windows and air ducts.
tip not tight Make sure the tip is held tightly in the tipholder. Push and pull on
the tip with tweezers to see that it is not loose. (On older tipholders, put a slight
bend in the tip to help it mount firmly in the tipholder tube if it seems loose.)
sample hold-down Verify that the sample is flat against the puck and cannot
move vertically. This may be become problematic if the sample has been affixed
using uncured, conductive epoxy, and/or if foam adhesives are used.
scanner screws-converter head contact Clean mating surfaces between the
underside of the converter head and the scanner adjustment screws. If dirt or oil are
evident, carefully remove with a clean wipe and alcohol. Some scanners utilize
plastic threaded bushings in the scanner body through which the adjustment screws
are threaded. If the bushings become fouled with grit, or if they are loose, drift may
result. If loose, gently tighten setscrews in the scanner body to increase tension on
the adjustment screw bushings. (Do not overtighten!) For more information regarding removal and replacement of adjustment screws, refer to section 15.3 in this
manual.

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stiff rear screw If the rear screw is difficult to turn (due to an accumulation of
dust in the threads, etc.), the drive shaft can wind up while driving the screw and
unwind after the stepper motor has stopped. This will cause the tip to continue
towards the surface. Clean the threads and screw per section 15.3 in this manual.

9.5.8. Real Time image hides features

If the real time image appears flat, but captured images reveal detail, try rotating the
Scan angle to 90. The real time image leveling software tends to hide features that
are parallel to the fast scan direction.

9.5.9. Image is streaky or wavy

If high-resolution images appear streaky or wavy, it may be a result of the following:
Insufficient vibration isolation Atomic-scale scans are the most susceptible to
vibration in the acoustic and subacoustic frequencies. Verify that the MultiMode is
acoustically isolated with a functioning isolation pad and, if required, an acoustic
hood. If vibrational noise persists, try moving the microscope to a less noisy location or using an isolation tripod.
Bad tip Many strange effects have been pondered and hunted down for hours
only to find that changing the tip fixes the problem. Try a different tip to see if the
problem persists.
Low scan rates The brute force method for reducing the effects of drift and even
low frequency vibration is to simply increase the Scan rate. Collect small-scale
images at 122 Hz with 256 x 256 sample points.

9.5.10. Image is triangular over step-like features

The performance of the STM over large scans with high vertical features is very
dependent on the ability of the feedback loop to force the tip to track the sample
surface. The digital feedback used in the NanoScope has been designed to maximize performance on a variety of samples. Try the following to improve the image
quality over step-like features:
Log or Boost feedbackThe most dramatic increase in performance of the feedback over large scans is achieved using the Log or Boost feedback modes. These
make the error signal symmetrical for conditions with the tip too far or too close to
the surface. Boost mode further optimizes the feedback performance for large
scans.

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GainThe settings of the Integral and Proportional gain parameters also tend to
be critical for large scans. They should be just sufficient to produce a slight fuzz on
the image, but not so high as to cause oscillations.
Scan rateThe Scan rate should be lowered for large scans, especially, if the sample surfaces are rough or contain large steps. Moving the tip quickly along the sample surface at high scan rates with large scan sizes will usually lead to a tip crash.
Essentially, the Scan rate should be inversely proportional to the Scan size, since
the tip must still be maintained roughly 1 nanometer above the surface.
Setpoint currentRaising the Setpoint current will effectively raise the gain of
the feedback loop which can be quite helpful for large scans. It will also bring the
tip closer to the surface but only by a small amount (i e-s).

9.5.11. Image goes white ("A" scanners)

If images go white after a few scans and the Z Center Voltage is still within range,
check the Realtime Planefit parameter on the active Channel panel. When using
an "A" scanner, it should always be set to Line. In general, this will be a problem
anytime there is a significant amount of drift in the Z center voltage, but drift is
especially prevalent with "A" scanners.

9.6. Overview of Low-Current STM

The following sections provide detailed instructions for performing low-current
(sub-picoamp) STM using two Digital Instruments devices: the Low Current STM
Converter for the Contact AFM and the LFM (Model #CSTMLC); and, the Low
Current STM Converter for MultiMode AFM (Model #MMSTMLC), or with the
Extender Electronics Module (Model #MMSTMLCE). The reader will find a
general description in Section 232.8, followed by detailed instructions for use of
Digital Instruments low-current converters.

9.7. Description
Operation of conventional STMs with current (Itun) in the nanoamp range is characterized by strong tip-sample force interactions. The forces applied to the sample
during STM imaging in air actually exceed the forces in atomic force microscopy
(AFM). The effects of high STM forces were found when imaging materials which
included graphite [1a], inorganic layered compounds[1b], organic conducting crystals [1c] and organic adsorbates on conducting substrates [1d].
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For metallic surfaces, the tip-sample gap resistance, R gap = V bias I tun , can be used
as a qualitative measure of tip-sample separation. Where
V bias = bias voltage
I tun = setpoint current

In general, decreasing I tun will increase the tip-sample separation and decrease the
tip-sample force.
By operating at R gap in the G range, for example, V bias = 1.0 V
and I tun = 1 pA the tip-sample distance increases enough to allow less-destructive imaging of a variety of surfaces.
The ability to conduct STM measurements in a wide range of Rgap can also be useful for experiments aimed at observing the image variations as a function of Rgap.
Picoampere-level STM provides the opportunity to image insulating samples
deposited on conducting substrates. Indeed, it was shown that using STM at ultra
high Rgap allows imaging of the topmost layers of alkanethiol adsorbates on gold
surfaces and to reveal earlier unknown surface features.
Picoampere-level STM also opens the possibility of imaging biological macromolecules such as DNA deposited on a non-conducting mica substrate. Though such
imaging was explained by lateral conductivity across the water overlayer covering
surfaces in air, a true mechanism of electron transfer is not yet established.

9.8. Description of Hardware

The Low Current STM head, which allows STM measurements with Itun in the pA
range, is a new product of Digital Instruments, Inc. This head is constructed for
operation with our MultiMode and AFM bases.
Low-current STM operation also requires the Picoamp Boost Box, which is
installed between the control unit or extender box and the MultiMode or AFM base.

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Figure 9.5. Low-Current Converter components: MultiMode head and

Picoamp Boost Box.
The gain is switchable between 1010 V/A or 1011 V/A and the bandwidth is switchable among 400 Hz, 1.5 kHz and 4 kHz. Lower bandwidths allow for lower noise
levels which are essential for operation at sub-picoampere I tun .
IMPORTANT: The default calibration value of the detector in standard STM mode
is 10 nA/V. This value should be changed to either 0.1 or 0.01 nA/V for operation
of the low-current head with gain factors of either 1010 and 1011 respectively. To
changes values, click on Real-time / Microscope / Calibrate / Detector. The In
sensitivity parameter is listed on the Detector Calibration panel and can be
changed by simply entering the new value.

9.9. Precautions
Due to the low-current heads highly sensitive electronic components, special precautions must be taken.
1. The input stage operational amplifier is extremely vulnerable to electrostatic discharge (ESD) and is easily destroyed. It is recommended that the user be grounded
with a wristband at all times that the low current head is handled, especially when
tips are installed.
2. The feedback resistor and capacitor in the input stage are extremely vulnerable to
contamination. At no time should these delicate components ever be touched with
the hands. If these components are accidentally touched, they must be rinsed clean
in a highly purified degreasing fluid immediately.

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3. Good grounding is essential for low-noise performance. A good contact between

the SPM base and the metallic cover (can) included with the low current head is
needed to reduce the electrical noise level. A simple grounding kit is included with
the converter which includes a length of wire and connecting lugs. Make certain
that the can cover and SPM base are electrically connected by the wire and that the
can cover is in place. The can cover acts as a Faraday shield.
4. Leakage and offset current:

Offset current values vary slightly from head to head but are typically in the
range of 0.5-0.1 pA. Therefore, minimum operating currents are just slightly
below the 1 pA value.
5. Please note that cables connecting the SPM base, the Picoamp Boost Box and the
NanoScope controller should not be lengthened if possible.
IMPORTANT: Always disconnect the Picoamp Boost Box and Low-current STM
Converter head before performing other types of imaging.

9.10. Installation
The low-current STM converter is designed to be installed onto one of four Digital
Instruments devices: 1) the MultiMode SPM (standard); 2) the MultiMode SPM
(with Extender base); 3) the dedicated AFM; and 4) the dedicated LFM. Generally, installation consists of cable connections and nothing more; however, cabling
differs somewhat between the devices.

9.10.1. MultiMode SPM

IMPORTANT! If you are installing on a MultiMode SPM equipped with
Extender Electronics Module for performing phase modulation MFM and EFM
work, you must install the Picoamp Boost box with the jumpers inside set for
extended. A label on the outside of the Boost box indicates whether it was set for
standard (Model MMSTMLC) or Extender (Model MMSTMLCE) at the factory. If
you are not certain which base your MultiMode has, contact Digital Instruments for
guidance.
1. Turn off all power to the SPM controller. Disconnect and remove the MultiMode
head.
2. Connect the picoamp booster box (male receptacle) to the controller using the
37-pin-to-25-pin connector cable. If an Extender Electronics Module is being
used with the system, insert it between the controller and picoamp booster as diagrammed below in this section.
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3. Connect the picoamp booster to the SPM base using the 25-pin-to-25-pin cable
connector.
4. Connect the low-current converter head to the MultiModes support ring using
the micro-D, 15-pin connector cable. Set switches on the picoamp booster to the
desired current level and bandwidth.
6. Before repowering the system, double-check all cable connections. If atomiclevel scans are intended, verify the cable between the SPM and picoamp booster
box is unstrained (a taut cable will transmit vibrations). The cable should rest
loosely. Before loading samples and running the SPM, attach the ESD wristband to
prevent sudden electrical discharges.

Controller

37-pin-to-37-pin cable
Extender Electronics
Module (if equipped)

37-pin-to-25-pin cable

Low-current
Converter Head

25-pin-to-25-pin cable
Picoamp Boost Box

MultiMode
Base

9.11. Operation
Once you check that leakage is absent and the offset current is small, the operation
of the low-current STM head is typically checked in the atomic-scale imaging of
graphite and the large-scale imaging of a gold-coated grating. The atomic-lattice of
graphite is well resolved in the images obtained with Itun in the 2-20 pA and Vbias in
the 20-100 mV range. Mechanically-sharpened Pt/Ir tips are generally used for
such measurements, and a tripod is good enough for the vibrational isolation of the
SPM base.

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9.11.1. Peculiarities
The transition to low current, however, brings some limitations, which are absent in
STM measurements with standard heads. The bandwidth of the amplifier and, consequently, of feedback is substantially narrower than that used for standard measurements in the nA range (12 kHz). Therefore, the feedback mechanism can be
less effective at high scan speeds. This must be taken into account, especially during imaging of corrugated surfaces.
However, the low current STM head can be used for imaging of atomically flat surfaces such as graphite and inorganic layered crystals at line frequencies up to 50 Hz
and still achieve atomic-scale resolution.
NanoScope II Users: The low-current STM converter head may be used with the
AFM base and the NanoScope II version 5.5 software. The software should be run
in TipView mode. Readings will be seen in nanoamps; however, actual values are in
picoamps.

9.11.2. Illustrative Examples

Different prototypes of the low-current STM head were used for measurements in
several laboratories. In addition to the control measurements routinely conducted
on graphite, the operation of the low-current STM head has been checked on several layered crystals and alkanethiol layers deposited on gold.
Several images obtained using low-current STM are presented below.

Figure 9.6. STM current and height images of HOPG surface.

Scan size = 6.0 nm, Itun = 1.6 pA, Vbias = 29 mV.

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Figure 9.7. STM current image of layered crystal -RuCl3.

Scan size = 4.48 nm, Itun = 1.5 pA, Vbias = 42 mV.

Figure 9.8. STM height image of alkanethiol layer on Au (111) substrate.

Scan size = 178.5 nm, Itun = 2 pA, Vbias = 1 V. (Courtesy of Dr. I. Tuzov,
NCSU)

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Figure 9.9. Molecular-scale STM current image of alkanethiol

layer on Au (111) substrate. Scan size = 10.0 nm, Itun = 13 pA,
Vbias = 1 V. (Courtesy of Dr. I. Tuzov, NCSU)

9.12. Servicing the Converter

The Low-current STM Converter features sensitive components which may be
damaged if exposed to sudden voltage spikes. Spikes may be due to electrostatic
discharge (ESD), or from external voltage sources. Operators should always wear
an anti-static, grounding wristband (included in Low Current STM converter kit)
while handling the head to protect against ESD.
The op-amp is the most vulnerable component; several spares are shipped with the
unit. If it is damaged, it may be replaced by doing the following:
1. Turn off the microscope. Disconnect the Low-current STM Converter head by
unplugging its cable from the support ring. Set the head on a workbench area
grounded against ESD. Ensure that an ESD wristband is being worn.

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2. Use the 0.050 allen wrench, included in the converter kit, to loosen the two
retaining screws which secure the heads cover. It is not necessary to remove the
screws.

Loosen these two screws.

3. Pull the cover straight up and off to expose the PC board and electronics. It will
appear as shown below.
Op-amp

Precision resistor and capacitor.

DO NOT TOUCH!

NOTE: Throughout steps #4-6 below, avoid touching the precision resistor and
capacitor. Any contaminant from the hands, including body oils, may cause excessive current flow, disabling the head. If these components are touched, they will
have to be recleaned immediately using highly purified degreasing compounds.
4. Remove the op-amp by grasping it and pulling straight up. It should slide out of
its socket.
5. Remove the new op-amp from its protective package. The op-amp is stored in
conductive foam and its leads have been preformed to fit the socket. Be careful not

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to bend any of the leads. Orient the op-amp so that the metal tab on the edge of the
can is in the 10:00 position as shown below.

Metal tab at 10:00 position.

To remove, pull
straight up.

To install, push
straight down.
(Do not bend leads.)

6. Verify that each of the op-amps wire leads is properly aligned with the appropriate hole, then press the op-amp gently into its socket. Do not bend wire leads.
7. Replace the metal cover on the head. Retighten retaining screws to secure.

9.13. Etching Tungsten Tips

You can purchase tungsten tips from Digital Instruments or make them yourself.
This section describes the process of etching tungsten tips.
Materials and Equipment Required:

Variac auto transformer

Optical microscope (20-100X)
Sodium nitrite (NaNO2)

Distilled water
Ethyl alcohol
WD-40 (anti-oxidant)
Two 50-ml beakers
Tipholder (see below)
Platinum wire
Tungsten Wire, 0.010" Diameter
Miscellaneous Wire/Clips

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9.13.1. Procedure
1. Mix a 5 percent (by weight) solution of Sodium Nitrite in water.
2. Pour 40 ml of the Sodium Nitrite solution into a beaker.
3. Pour 40 ml of WD 40 into a beaker.
4. Construct an electrode out of the platinum wire and insert it into the beaker.
5. Adjust the variac for 30V, and with it Off, connect one output to the platinum
electrode.
6. Cut 10 to 12 pieces of tungsten wire 1.25 cm long. Before etching, check to
make sure that at least one end of the wire has not split by inserting the ends into a
tip holder. If an end has split, you will not be able to insert it into the tipholder. You
can etch the end that has split, however, preserve the unspoiled end.
7. Place the tungsten tips into a holder. We like to use an IC socket (the low cost,
edge-grip square contact type, not the machine-grip round contact type), with all
the pins soldered together. The tips will then be held in place while inverting them
over the solution. We also find it helpful to solder the IC socket to the back of a
proto-board (perf-board). You can then invert the tips over a beaker with the protoboard sitting on the rim of the beaker.
8. Invert the tips over the Sodium Nitrite solution with 2 mm of the tips surface
submerged. More than 2 mm will cause excessive foaming of the solution during
etching, and less than 2 mm will result in tips that are too blunt.
9. Connect the other output of the variac to the common of all the tips.
10. Turn on the variac and etch the tips. While the tips are etching, the solution will
foam, and the tips will start to glow. As the tips etch towards the surface, the foaming will be reduced. Continue to etch the tip until it stops.
11. Re-submerge the tips 1mm into the solution for 15 seconds at 30V. Turn on
the variac and re-etch the tips. There should be only slight bubbling from the tip and
it should not glow.

Notes:

It possible to vary the tip shape at this point by lowering the voltage on the
variac and increasing or decreasing the amount of time the tips are submerged.
Longer time gives blunter tips.

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12. Dip the tips into ethyl alcohol to clean them. If you plan to keep the tips around
for more than a day, dip them into the WD 40 after cleaning.
13. Examine the tips under the optical microscope. Ones that are too long, too
blunt, or split at the end will hardly ever be good tips and can be thrown out at this
time. Of course, this is a subjective process. As your experience in etching grows,
you will get better at throwing out the bad ones.
14. Repeat the etching procedure. Replace the etching solution when a fairly large
amount of residue is present. Typically, you can etch 60 to 80 tips in a 40 ml solution.

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MultiModeSPM Instruction Manual

Chapter 10

Lateral Force Mode

Lateral Force
Mode

10.1. Introduction
The MultiMode SPM is capable of measuring frictional forces on the surfaces of
samples using a special feature known as lateral force microscopy (LFM). The
name derives from the fact that cantilevers scanning laterally (perpendicular to their
lengths) are torqued more as they transit high-friction sites; low-friction sites tend
to torque cantilevers less. The relative measure of lateral forces encountered along a
surface yields a map of high- and low-friction sites.
After obtaining a good topographical image in AFM mode, it is relatively easy to
switch to LFM mode to view and acquire lateral force data. It is important to obtain
a good image in AFM mode before switching to LFM mode. The NanoScope system will continue to run the feedback based on the AFM signal and feedback gains
in the control panel while LFM data is acquired and displayed. Complete the following steps to switch the system to LFM mode:
1. Set up and run the system in contact AFM mode as described in Chapter 6,
assigning the Channel 1 image to Data Type: Height and the Channel 2 image to
Data Type: Friction. Set the Scan angle to 90.00
2. Optimize the scan parameters in AFM mode for Channel 1.
3. For Channel 2, set Line direction to Trace. This will place high lateral forces
on the top of the color bar and low lateral forces on the bottom of the color bar. If
the Line direction parameter is changed to Retrace, the plus-minus sign of the lateral force changes and low lateral force will be displayed on the top of the color bar.
LFM data can now be collected and stored.

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10.2. LFM Mode in More Detail

The following paragraphs provide more complete information concerning the operation of LFM in friction mode.

10.2.1. Optimal Setup for Frictional Measurements

Scan direction The cantilever is most susceptible to frictional effects when the
scan direction runs perpendicular to the major axis of the cantilever as shown in figure 10.1. The Scan angle parameter in the Scan Controls panel must be set to 90
or 270 to produce this scan direction.

Scan Direction
without Scan
Rotation
scan angle 0

Scan Direction
for Friction
Measurements
scan angle
90 or 270
Cantilever
(Top View)

Figure 10.1. Scan angle selection.

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The contact mode setpoint voltage will slightly adjust the gain of the lateral force
signal. By increasing the setpoint, the contact force applied will increase, and so
will the frictional or torsional forces in an approximately linear fashion. If the frictional effects are far too large or too small, it will be necessary to resort to changing
the cantilever probe used, but if the value is near the dynamic range desired, adjustment of the contact force will produce modest changes in the lateral force or frictional signal.
Tip selection The analog-to-digital converter on the auxiliary input channel
which is used for LFM data has a maximum input range of 10 volts. This, and the
anticipated interaction between tip and sample define the selection of the cantilever
to be used for the measurement.
The 200-micron cantilever with wide legs provides a good starting point for frictional measurements. It is flexible enough to provide reasonable signal levels on
samples with moderate friction. If the signal exceeds + 10.00 volts with the 200-m
wide-legged cantilever, one of the stiffer 100-m cantilevers should be used. If the
signal level is too small, the narrow-legged 200-m cantilever will provide a larger
signal.

10.2.2. Determination of friction

The lateral force on the tip is caused by both friction and the tip running into or
tripping on the edges of features. There are a few things the user can do to verify
that data obtained in Data Type: Friction is a result of friction between the tip and
the sample. The topographical information should be compared to the Friction data
in both scan directions. The Scope Mode can also be very useful when analyzing
frictional data.
Scope Mode The LFM user should be very familiar with the Scope Mode of
viewing the data. When using Scope Mode, verify that the Rounding parameter in
the Scanner Parameters window (selected with the Microscope / Calibrate /
Scanner command) is set to zero. In the dual-trace mode, the data from the trace
and the retrace of the sample under the tip is shown in an oscilloscope format. The
vertical axis represents the differential signal from the left and right photodiodes,
while the horizontal axis represents the tip position along the fast scan direction.
There are several general features to observe in the scope signal (see figure 10.2
below).

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Trace
Retrace

Z Range
0.10 V/div

Scan Size - 5.5 V/div

Figure 10.2. Example of a scope trace with low-friction areas.

With the scan direction rotated, the separation between the trace and retrace lines in
Scope Mode provides a general indication of the amount of friction between the
sample and the tip. For example, if there is no friction between the sample and the
tip, the trace and retrace will coincide vertically. As the frictional forces between
the tip and the sample increase, the cantilever twists to a larger degree and the vertical separation between the trace and the retrace increases. However, there is almost
always some friction between the tip and the sample.
The trace and retrace signals will move closer together when regions of low friction
are encountered. Figure 10.2 shows a theorized example of the scope trace for a
sample with two areas of relatively low friction. Note how the separation between
the traces decreases over the low-friction areas as the torsional deflection of the
cantilever decreases for both trace directions. When trace and retrace both deflect in
the same direction, this is often caused by non-frictional effects; for example, optical interference. In general, samples with areas of varying friction will include steplike features in the Scope Mode view.
Compare to topography Comparing frictional data to topographical data for the
same scan area provides another means of deducing the origin of the frictional features. Often, transient frictional features occur at the edges of topographical features. The tip trips over the feature, producing the transient frictional feature.

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Reverse scan direction Reversing the scan direction in the Image Mode while
viewing the friction channel, is also useful in verifying the origin of the data.
Remember that changing the Line direction parameter in the Real-time control
panel changes the direction of the scan during which data is collected. If the data
results from friction between tip and sample, the relative signal strengths will invert
as the scan direction is reversed. For most color tables, the image produced from
the trace in figure 10.2 (i.e., with the Line direction parameter set to Trace) would
be darker in the low-friction areas than it is in the high-friction areas. Conversely,
for the same color table, the image produced from the Retrace (i.e., with the Line
direction parameter set to Retrace) would be lighter in the low-friction areas.

10.2.3. Identification of Forces other than Friction

There are a few phenomena that will produce false features in friction data on the
auxiliary data channel:
Tripping Tripping occurs when the probe encounters a step on the sample surface. The side of the probe strikes the feature, causing the cantilever to twist. In the
Image Mode on the auxiliary channel, tripping appears as highlights which coincide with topographical features. In the Scope Mode on the auxiliary channel, tripping produces transients similar to those shown in figure 10.3. Regions of highfriction can also produce transients similar to those shown in figure 10.3, so the user
must be careful to analyze the data carefully.
Optical interference Optical interference between the laser light reflected off of
the cantilever and secondary sources (e.g., the laser light which spills over the sides
of the cantilever and the light transmitted through the cantilever, reflected off the
sample and back through the cantilever) produces evenly spaced lines in the image.
Spacing of the lines ranges between 1.5 and 2.0 microns and runs perpendicular to
the tip.
Rounding Use the Calibrate command in the Real-time / Microscope menu to
set the Rounding parameter to zero before looking at frictional data. In the Scope
Mode, the Rounding function shifts the trace and retrace lines horizontally and
makes it difficult to directly compare the two lines.

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Example of Sample Surface with Uniform Friction

Trace
Retrace

Z Range
0.08 V/div

Scan Size - 4.2 V/div

Figure 10.3. Tripping transients in Scope Mode.

10.2.4. Example of frictional data

Rarely will samples produce traces like the ones shown in figures 10.2 and 10.3.
Typically, combinations of the features discussed above will be present in each
trace and retrace. For example, figure 10.4 depicts what the scope mode might show
for a sample with two low-friction areas where one is a flat bump; i.e., low-friction
foreign material sticking up on a high-friction surface, and where the other lowfriction area is even with the sample surface. Notice on the trace that as the tip
strikes the edge of the bump (point 1 on the graph), the lateral force increases
momentarily and then decreases as the tip begins scanning across the low-friction
bump (region 2 on the graph). At the other edge of the bump, the lateral force may
decrease somewhat as the tip comes off the bump (point 3 on the graph), and then
will increase as the tip scans across the high-friction surface (region 4 on the
graph). At the second low-friction area, the spikes due to topography are not
present. On the retrace, notice that the sign of the frictional forces will change, but
the shape will remain the same. The lateral forces due to topography shift to the
other side of the bump and also change sign.

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Lateral Force Mode

Low Friction Bump

Low Friction Area

Example of Sample Surface with Two Low Friction Areas

Trace
Retrace
4

Z Range
0.10 V/div

Scan Size - 5.5 V/div

Figure 10.4. Scope Mode view of sample surface.

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MultiModeSPM Instruction Manual

Force Imaging

11.1. Introduction
Force plots are used to measure tip-sample interactions and determine optimal setpoints. More recently, microscopists have begun to plot force measurements across
entire surfaces to reveal new information about the sample. This area of SPM promises to open new chapters in materials science, biology and other investigative
areas.

11.1.1. Plotting Force in Contact AFM

The Force Plot command in the View / Force Mode / Plot menu allows the microscopist to quickly check the interaction between cantilever and sample. In Force
Plot mode, the X and Y voltages applied to the piezo tube are held at zero while a
triangular waveform (similar to the one depicted below) is applied to the Z piezo
tube.
Scan period
- 220
Z scan size
Z scan start
Z Voltage

Chapter 11

Time
1
Scan period (sec) = -------------------------------------Z scan rate (Hz)

+ 220
Figure 11.1. Z-axis voltage during force plot scanning.

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As a result of the applied voltage, the cantilever tip moves up and down relative to
the sample as shown in Figure 11.4. The Z scan start parameter sets the offset of
the piezo travel (i.e., its starting point), while the Z scan size parameter defines the
total travel distance of the piezo. Therefore, the maximum travel distance is
obtained by setting the Z scan start to +220 volts, with the Z scan size set to 440
volts.
As the piezo moves the tip up and down, the cantilever-deflection signal from the
photodiode is monitored. The force curve, a plot of the cantilever deflection signal
as a function of voltage applied to the piezo tube, shows on the display monitor.
The control monitor displays various control panels used to control the microscope
in Force Plot.
In addition to dedicated force measurement experiments, Force Plot may be used
to enhance routine topographic imaging. Force Plot is frequently used to adjust,
calculate, and minimize contact forces between the cantilever and sample.

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Force Plot may also be used to diagnose SPM performance and determine sensitivity of the cantilever deflection voltage versus voltage applied to the piezo.
1

7
6

Figure 11.2. Tip-sample interaction during a force plot.

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11.1.2. The Force Curve and Piezo Extension-Retraction Cycle

Figure 11.2 above compares portions of the force curve shown in Figure 11.5 to relative positions of the tip and sample at six points. The force curve represents the
deflection signal for each complete extension-retraction cycle of the piezo
(Figure 11.1). The Z scan rate parameter in the Force Plot control panel defines
the rate at which the piezo completes an extension-retraction cycle (and therefore
the rate at which new curves are displayed).
The deflection signal decreases as the piezo turns around and begins to pull the tip
away from the sample surface. Typically, the signal continues to drop after the flat,
zero deflection point of the force curve. At point 5, the cantilever is not deflected,
but due to attractive forces between the tip and the sample, the tip sticks to the sample, and the cantilever is pulled down as the piezo continues to retract. Eventually,
the spring force of the bent cantilever overcomes the attractive forces, and the cantilever quickly returns to its non-deflected, non-contact position. This is represented
by point 6 on Figures 11.2 and 11.4. Figure 11.3 below represents the effects of tip
pulldown due to attractive forces as the tip nears the surface (left), and the sudden,
sharp rebound that results as the tip is pulled free (right).
Pulldown

Upward rebound

Figure 11.3. As the tip approaches the surface, it is frequently pulled down
by attractive forces (left). As the tip lifts off, it sticks to the sample
until pulled away, resulting in a sharp rebound (right).
The display monitor presents a linear scale of the Z piezo voltage. The scale ranges
from +220 volts at the extended end to -220 volts at the retracted end. The range of
piezo travel, as defined by the Z scan start and Z scan size parameters in the Force
Plot control panel, is represented by two white lines on the scale. The lower white
line corresponds to the Z scan start parameter in the control panel, while the spacing between the lines corresponds to the Z scan size. The average voltage applied
to the Z electrode on the piezo tube just prior to entering the Force Plot mode is
represented by the Z center line.

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Notes

In NanoScope software version 4.2 and later, the tip is retracted by the Scan size
above the surface when first entering any of the force modes (Calibrate, Step,
Indent Volume). Ramping of the Z-axis piezo begins only when the user initiates
operation using one of the Probe commands (Run Continuous, Run Single,
Approach Continuous and Approach Single). The mode is indicated
simultaneously on the gray status bar at the bottom of the control monitor.

11.2. Contact AFM Force Plots

To minimize or calculate the contact force between the tip and sample, it is important to obtain a good force curve. This procedure is described in detail in
Section 6.4.1. Additional information relevant to obtaining force curves is provided
in this section.
False Engagement
Figure 11.4 illustrates a force curve due to a falsely engaged tip. Light reflected off
the sample is received by the photodiode, causing an increase in the deflection signal until the signal equals the setpoint and causes the system to Engage (even
though the tip is not on the surface). Interference in the reflected light causes the
hump-shaped waveform.
Although the Tip Down button can be used to move the tip down to the surface,
there exist other ways to correct a false engagement: 1) increase the setpoint and
engage again; 2) adjust the photodetector positioner to make the top/bottom differential voltage more negative, then engage the tip again. This has the effect of pushing the cantilever farther up before the setpoint is reached. Chapter 15 on
troubleshooting contains tips on false engagement.

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Retracting
Extending

Tip
Deflection
.25V/div
0.48
V/div

Setpoint

Z Position - 9.27 V/div

Figure 11.4. False engagement (J scanner).

Helpful Suggestions for Working with Force Plots
Motor Control / Tip Up and Tip Down buttons provide coarse adjustment of Z
scan start voltage. With these buttons the SPM head, including tip and piezo, is
moved vertically (in much the same way that piezo-travel positioning is adjusted
with the Z scan start parameter).

Notes

The Step Motor function is generally used only when the scanning range of the
Z piezo is exceeded and/or when it is necessary to position a force measurement
in the center of the scanners range. Because the Z-axis leadscrew has some
backlash, it may be necessary to rotate the screw several turns by clicking on the
Tip Up or Tip Down buttons before movement is obtained.
In an analogous manner, the photodiode positioner can be used as a coarse adjustment for Setpoint voltage. Changing the beams position on the photodiode by
rotating the mirror adjustment knob shifts the force curve on the graph. Moving the
photodiode down by rotating the positioner counterclockwise shifts the curve
down, just as decreasing the Setpoint parameter shifts the curve down. Conversely,
rotating the positioner clockwise moves the curve up by moving the photodiode up.

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11.2.1. Contact AFM Force Plots

Cantilever deflection
Down
Up

Lets begin with the simplest of SPM force plots: a contact AFM force plot using a
silicon nitride tip. Because of the pliant property (and lower spring constant) of silicon nitride probes, they are sensitive to attractive and repulsive forces. A force plot
in contact AFM is shown below. (See also Figure 11.2.)
3
Piezo extension
Piezo retraction
4
2

1
7

1
Piezo extends; tip descends. No contact with surface yet.
2
Tip is pulled down by attractive forces near surface.
3
As tip presses into the surface, cantilever bends upward.
4
Piezo retracts. Cantilever relaxes downward until tip forces
are in equilibrium with surface forces.
Piezo continues retraction. Cantilever bends downward as
surface attraction holds onto the tip.

As piezo continues retracting, tip finally breaks free of

surface attraction. Cantilever rebounds sharply upward.

6
7

As piezo continues retracting, tip continues its ascent.

No further contact with surface during this cycle.
Figure 11.5. Anatomy of a force curve.

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Here, the horizontal axis plots the probes movement relative to the sample. As the
probe descends toward the sample, the probe-sample distance decreases. A descent
is achieved by extending the Z-axis piezo crystal, which is plotted from right-to-left
in yellow on the NanoScope display monitor. As the probe ascends away from the
sample, the probe-sample distance increases. An ascent is achieved by retracting
the Z-axis piezo crystal, which is plotted from left-to-right in white on the NanoScope display monitor.
The cantilevers deflection is plotted on the vertical axis of the graph: when the cantilever is deflected downward, it is plotted on the graphs downward vertical; when
the cantilever is deflected upward, it is plotted on the graphs upward vertical.
The graph reveals at least two very important things:

Sample-tip attraction As the tip approaches the sample, various attractive

forces reach out and grab the tip. This is evidenced at point 2 (slight dip) in
the graph above. Notice how the tip suddenly plunges toward the sample here
during its descent. This is sometimes called the jump-to-contact point and is
usually due to electrostatic attraction and/or surface tension (capillary) forces.
Attraction is also evident between points 3 and 4 (sloped line) as the cantilever
is pulled away from the sample. If attractive forces are strong enough, the tip
will cling to the sample surface as it is pulled clear. Eventually, the sample lets
go and the tip rebounds sharply upward (white line, between points 4 and 5).
By knowing the spring constant of the cantilever, it is possible to measure the
attractive forces of tip-sample interactions with good precision.

Notes
Although attractive forces appear small, remember that the tip is extremely
sharp. Since only a few nanometers of the tip actually touch the sample, even
minute forces are distributed over an exceedingly small area, which add up
quickly. Many materials are easily dented by the tip under such conditions. Use
of force plots may be used to adjust a setpoint which applies minimal force to
the sample during contact AFM. (More on this topic below.)

Material elasticity It is possible to extract some information regarding the

elasticity of the material by studying force curves. In the graph above, the tip is
in constant contact with the sample between points 2 and 3. As the tip is pressed
further and further into the material, the probes cantilever flexes. The amount of
cantilever flexion for a given amount of downward tip movement gives an
indication of the materials elasticity.
For example, if the material is extremely hard, pressing the probe downward
will result in a relatively large amount of cantilever flexion. On the other hand, if
the material is soft, the cantilever will flex less during its descent. The shape and

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slope of the contacted portion of the force curve gives detailed information
about surface elasticity. It is sometimes possible to obtain quantitative measurements of sample elasticity. (See, for example: Radmacher, et al. 1994. Science,
Vol. 265:1577-1579.)
Two imaging techniques may be employed to measure and display elasticity at
multiple points on a sample surface: force modulation (see Section 11.5 below)
and force volume imaging (see Section 11.7 below).

11.2.2. Sensitivity Determination

Sensitivity represents the cantilever deflection signal versus voltage applied to the
piezo and is normally set from the Force Plot mode. The sensitivity must be calibrated before accurate deflection data can be obtained. Sensitivity is equal to the
slope of the force curve while the cantilever is in contact with the sample surface.
Complete the following steps to calculate the sensitivity:

Obtain a good force curve on the display monitor.

Position the cursor on one end of the contact portion of the curve.
Click on the left mouse button to fix the line segment.
Drag the mouse to position the rubber band line parallel to the contact portion
of the force curve (see Figure 11.6).

Click and drag line parallel to plot

Figure 11.6. Use the mouse to set the Sensitivity parameter.

The second click on the mouse causes the system to calculate the slope of the
line segment and enter the calculated value as the Sensitivity in the menu.

A click of the right mouse button will remove the line segment from the screen.
Note that Sensitivity can be expressed in terms of the photodiode voltage versus the
distance traveled by the piezo, or the photodiode voltage versus the voltage applied

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to the piezo, depending on the setting of the Units parameter. If Sensitivity is calibrated on a material much stiffer than the cantilever, it measures the value of the
AFMs optical lever sensitivity; i.e., how many volts of deflection signal are produced by a given deflection of the cantilever tip. The sensitivity will change for different cantilever lengths and styles (shorter cantilevers give higher sensitivities).
Sensitivity will also change with the position of the laser on the cantilever and the
quality of the laser beam reflection from the cantilever.

Notes

It is important to calibrate the Sensitivity parameter on a hard substrate as

described here BEFORE using the force curves vertical scale for quantitative
measurements.

11.2.3. Force Minimization

Force Plot allows the contact force of the cantilever on the sample surface to be
minimized. The force curve clearly shows the relationship between the Setpoint
and the cantilever deflection voltage when the cantilever is off the sample surface.
Setpoint can be adjusted to set the nominal deflection of the cantilever and, therefore, the nominal force applied by the cantilever during data collection.
The microscope can be run below the point of zero deflection of the cantilever to
minimize the contact force of the cantilever on the sample. It is possible to get a
negative deflection whenever the cantilever sticks to the surface. The system cannot
engage to a negative deflection operating point, because the engagement process
requires a setpoint which is greater than the voltage at zero deflection. However, the
operating point can be changed after the cantilever has been engaged.
In Force Plot, the setpoint can be adjusted to the zero cantilever-deflection point
and beyond, while viewing the force curve. The setpoint can be adjusted (most
often made more negative) so that it lies between the flat segment of the force curve
which corresponds to the zero deflection point, and the tip of the retraction scan
where the cantilever pulls off the sample surface VCSmin. The contact force is at its
minimum when VCSmin is on the centerline of the deflection-signal axis.
In practice, VCSmin should be a little below the centerline since VCSmin is the
point where the cantilever pulls off the surface and operation at this deflection will
be unstable. Finally, note that changing the Setpoint option in the Feedback Controls panel will change the Setpoint parameter in its Real Time counterpart when
the Force Plot routine is exited. After exiting, if the image looks good, the force
can be decreased further by lowering the Setpoint in small increments until the
cantilever pulls off. Resetting the Setpoint to a value higher than the top/bottom

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differential signal on the upper MultiMode meter display will recapture the cantilever. (Slowly adjust to a more positive value until the tip is back on the surface.)
Adjusting the Setpoint a few tenths of a volt above the point where the cantilever
pulled off will provide a low contact force.
If a high initial contact force will adversely affect the sample, engage the cantilever
with a very small scan size. Then, minimize the force while the tip is confined to a
small area of the sample where it will experience the relatively high initial engagement force. Once the force is minimized, increase the Scan size or offset the scan to
a different area of the sample. However, keep in mind that if the force is minimized
in a smooth area of the sample, the cantilever may pull off when it is translated to a
rougher part of the sample.

11.2.4. Calculating Contact Force

The force curve clearly shows the relationship between the setpoint and the deflection of the cantilever. Because the setpoint defines the value of the deflection signal
maintained by the feedback loop, the force curve can be used to calculate the nominal contact force of the tip on the sample if the spring-constant, k , of the cantilever
is known. The contact force is defined by the equation:
F = k ( Z )

where Z is the Z distance from the control point to VCSmin in nanometers. An

example of how to compute the contact force from the Force Plot graph is shown in
Figure 11.9.
Tip
Deflection
1.0 V / div
7.6 div

Setpoint

VCSmin
Z Position (10.0 V / div)
Figure 11.7. Computing contact force.

Recalling that contact force F is equal to k ( Z ) , we can calculate the contact

force from the sample plot above. Let us assume, for example, that the spring con-

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0.6N
stant of the cantilever is k = -----------m

12nm
and that Z piezo sensitivity = -------------- . The plot
V

above may be measured at the points where the retract portion of the curve intersects the setpoint to tip pull-off (rebound). The distance is then multiplied times the
Z piezo sensitivity to obtain Z . In this example:
Z = 7.6 div 10.0 V div 12 nm v = 152 nm

Therefore, the contact force is calculated as:

F = 0.6N m 152 nm
= 91.2 nN

When the Data type is set to Height with the feedback gains set high, the tip tracks
the sample surface with nearly constant deflection of the cantilever. When the cantilever deflection is constant, the force is constant and the force calculation determines the force between the tip and the surface over the entire scan area.
Force calculations are not as straightforward on images captured with the Data
type set to Deflection. When collecting deflection data, the feedback gains are ideally set low so the sample stays at a constant position relative to the cantilever
holder. In this case, the cantilever deflection (and therefore the force applied to the
sample) varies as features on the surface are encountered. The nominal force
applied to the surface can be calculated from the force equation. The force applied
at other points on the sample can be calculated relative to the nominal force by
using deflection data and the spring-constant of the cantilever. Note that the Sensitivity parameter must be accuratethat is, previously determined and entered
before the deflection data will be accurate.
An simple alternative to calculating force is to follow these five steps:
1. Set sensitivity using the mouse.
2. Change units to metric.
3. Count vertical units from Setpoint to UCS min.
4. Multiply by Tip Deflection Scale.
5. Multiply by the spring-constant, k.

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11.2.5. Interpreting Force Curves

An examination of force curves can prove useful in determining adhesion and hardness characteristics of samples. The examples in Figure 11.8 represent some of the
general variations in force curves. For more information regarding force imaging,
refer to Digital Instruments application note Probing Nano-Scale Forces with the
Atomic Force Microscope.

Large adhesion

Small adhesion

Hard sample

Soft sample

Long-range repulsion

Long-range attraction

Figure 11.8. Force curve examples.

11.3. Force Imaging in TappingMode

CAUTION: Because TappingMode cantilevers are relatively stiff, Force Mode can
potentially damage the tip and/or surface. DI recommends using Force Plot only
with extreme caution.
ATTENTION: Le pointes Tapping tant relativement raides, lutilisation du mode
Force peut endommager la pointe ou lchantillon. Digital Instruments recommande dutiliser le mode Force Plot avec une extrme prcaution.
WARNHINWEIS: Da TappingMode-Mespitzen relativ steif sind, kann im Force
Mode unter Umstnden die Mespitze oder die Oberflche beschdigt werden. DI
empfiehlt, den Force Plot nur unter grter Vorsicht anzuwenden.
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Force Mode allows the imaging of forces between the tip and surface, including
chemical bonds, electrostatic forces, surface tension, magnetic forces, etc. In TappingMode, forces may be observed by measuring changes in the tips RMS amplitude, phase, or deflection. The user may represent force plots in one of two forms:
Force Plot and Force Volume (see Section 11.5). Both are essentially the same,
with Force Volume generating a map of many individual force plots. To produce
high-quality force plots, it is necessary to very precisely control the tips position
relative to the surface.

11.3.1. Force Plots

When performing Force Plot in TappingMode, the piezo moves to the center of the
current XY scan, then turns off the XY scan motion. Next, a triangular waveform is
applied to the Z electrodes of the piezo tube. As a result, the oscillating tip is moved
up and down relative to the sample. This is exactly the same Z-axis piezo motion as
for contact AFM. In TappingMode, however, the force plot is a graph of the piezos
extension versus the oscillating tips amplitude, phase, or deflection.
Figure 11.9 represents a tip-sample-piezo relationship on a MultiMode system. The
piezo positions the sample just below the tip (at the Z scan start), then extends a
known distance closer to the tip (the Z scan size). If the oscillating tip encounters
any surface forces, it will respond (its amplitude may decrease and/or its phase may
change.
Z scan start
oscillating tip
Z scan size

distance fixed
by adjustment
screws

Figure 11.9. Relationship of Z scan start and Z scan size.

Uses of Force Plot in TappingMode include characterizing forces on the cantilever
tip, diagnosing SPM performance, and calibrating the RMS amplitude, deflection
or phase of the cantilever as a function of tip-sample distance. For example, as the
oscillating tip is brought closer to the surface, the tips motion is dampened, which

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shows as an immediate drop in amplitude. When plotted, the graph resembles

Figure 11.10.

Piezo extension
Piezo retraction

1
Tip is clear of the surface

4
3

Figure 11.10. Force plot of piezo extension versus

RMS amplitude (top) and deflection (bottom).
Figure 11.10 shows a two-channel TappingMode force plot. The vertical axes of the
graphs represent the RMS amplitude (top) and deflection signal (bottom) of the
cantilever. The position of the Z piezo is plotted along the horizontal axis. Channel
1 (top) demonstrates how the cantilevers RMS amplitude decreases as the tip is
positioned closer to the sample. The plot represents the RMS amplitude for one
complete extension-retraction cycle of the piezo. The Z scan rate parameter in the
Z Scan Controls panel defines the rate at which the piezo completes an extensionretraction cycle; therefore, the rate at which new curves are displayed. At point 1,
the tip begins its interaction with the sample. The tips oscillation amplitude begins
to recede, dropping off as the tip moves closer to the sample surface. Between
points 1 and 2, voltage to the piezo is increased, bringing the tip about 30 nm closer

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to the surface. Over the same interval, the cantilevers amplitude is diminished
about 1.75 volts due to dampening effects.
Dividing the change in amplitude by the change in Z piezo position gives the
responsiveness of the tip-sample interaction, displayed as a Sensitivity value in the
Z Scan Controls menu. This value may be found directly by using the mouse to
draw a line parallel to the plots slope in the region between points 1 and 2 where
the tips amplitude is dampened. Tip dampening occurs as a result of mechanicalacoustic coupling between the tip and sample. As the tip descends closer and closer
to the sample, oscillation eventually ceases and the amplitude drops to zero.
For TappingMode in this sloping region, each nanometer decrease in the cantilever
position decreases the vibrational amplitude of the cantilever by two nanometers.
Channel 2 (bottom) in Figure 11.12 plots the average cantilevers deflection versus
piezo extension. The deflection signal is low-pass filtered to eliminate the high-frequency TappingMode oscillation. Even as the tips RMS amplitude is dampened
during its encounters with the sample surface, the average deflection is unchanged.
This condition changes, however, once the tip has been positioned so close to the
sample that all oscillation ceases. Pressing the tip still further causes the average
deflection to increase, applying a constant force to the sample.
At point 3 in Figure 11.10, the cantilever has begun to deflect. The region between
points 3 and 4 may be hazardous to the tip, since the tip is pressed tightly against
the sample surface. Most single crystal silicon TappingMode tips fail in this region,
depending upon the hardness of the sample.

11.3.2. Obtaining a Force Plot of a Calibration Reference in

TappingMode
CAUTION: Because TappingMode cantilevers are relatively stiff, Force Mode can
potentially damage the tip and/or surface. DI recommends using Force Plot only
with extreme caution.
ATTENTION: Le pointes Tapping tant relativement raides, lutilisation du mode
Force peut endommager la pointe ou lchantillon. Digital Instruments recommande dutiliser le mode Force Plot avec une extrme prcaution.
WARNHINWEIS: Da TappingMode-Mespitzen relativ steif sind, kann im Force
Mode unter Umstnden die Mespitze oder die Oberflche beschdigt werden. DI
empfiehlt, den Force Plot nur unter grter Vorsicht anzuwenden.
When obtaining force plots in TappingMode, set up scan parameters so that the
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tude). If the amplitude is reduced to zero, the tip has almost certainly been blunted
or broken, and/or the sample has sustained damage.
To make a TappingMode force plot of a silicon calibration reference, try the following:
1. Verify the tipholder is fitted with a TappingMode tip. Set the AFM mode parameter to Tapping and obtain a TappingMode image. You are now in Image mode.
2. To switch to Force Mode, click on the Real Time / View / Force Mode / Plot
option. At least three panels should be visible: Z Scan Controls, Feedback Controls, plus one channel panel (e.g., Channel 1). Collectively, these panels allow the
user complete control over tip-sample interactions. If any panels are not visible,
pull down the Panels menu to select them.
The top menu bar offers a number of tip approach options detailed in the Command
Reference Manual, Chapter 10. These buttons are not generally used for TappingMode and may be ignored.
3. Set the Z Scan Controls, Feedback Controls and Channel panel parameters to
the settings shown below. (Note that the Sensitivity value shown here may differ
from yours.)
Z Scan Controls
Graph Controls
Z scan start:

Other Controls
Trigger mode:

*
*

Z scan size:
Z scan rate:

Trig threshold:

4.88 Hz

Trigger channel:

X offset:

0.00 nm

Z step size:

Y offset:

0.00 nm

Step threshold:

Number of samples:

256

Amplitude
10.0 nm
10.0 nm

Start mode:

Calibrate
Extended

Average count:

End mode:

Sensitivity:

Indent Feedback:

Units:

Off
-25.0 nm

Disabled

Metric

Channel 1
Data type:
Z range:

Amplitude
500 nm

Feedback Controls
Main Controls
Setpoint:
Input attenuation:
Interleave Controls

*
1x
Setpoint 0

* Do not adjust these values yet.

The Channel 1 panel should have its Data type parameter set to Amplitude.

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4. To obtain a satisfactory force plot, it will be necessary to adjust the Z scan start
parameter more positive. This may be easily done using the right arrow key.

11.3.3. Very High Contact Force

Figure 11.11 shows a curve produced when the tip is pushed too far into the sample.
This is a very dangerous condition because the cantilevers used in TappingMode
are stiff and brittle. If they are driven into the sample surface so that oscillation
amplitude changes to zero, they will break.
The flat portion on the left side of the amplitude curve in Figure 11.11 occurs
because the tip is so close to the surface that it no longer vibrates. As the piezo
extends the tip further and further, the amplitude of vibration does not change
because the tip is always in contact with the sample surface. The contact force is
very high due to the stiffness of the TappingMode cantilevers. The cantilever may
become cracked or the tip shattered if deflection continues.
Retracting
Extending

Tip
Deflection
0.5 V/div

Setpoint

Z Position - 21.9 nm/div

Zero Amplitude of Oscillation

-if any of this flat region is
observed on the graph, the
tip may possibly be broken
Figure 11.11. Amplitude force plot with high contact force.
This situation can be avoided by using triggers (see next section) and/or by reducing the value of Z scan start so there is no flat portion on the left side of the curve.
Rapidly increasing the value of Z scan start is very dangerous since the total vibra-

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tional amplitude of the cantilever is small relative to the total Z travel of the longrange scanner.
Plotting phase-versus-frequency in TappingMode force plots
Interest has increased in plotting the tips phase-versus-frequency while encountering sample surfaces in TappingMode. This is available only for SPMs having an
Extender Electronics Module. Just as imaging magnetic-electric forces in phase
gives better resolution than amplitude, plotting force in terms of phase-versus-frequency allows improved observation of long-range attractive and repulsive forces
between the tip and sample. Precise interpretation of force plots using phase-versus-frequency remains under investigation. Contact Digital Instruments for more
information.
Regarding the selection of tips...
Almost any TappingMode tip may be used to obtain TappingMode force plots;
however, the ultimate choice should depend upon the delicacy of the sample and/or
the magnitude of the forces to be gauged. Recall that longer tips have lower spring
constants (i.e., they are more pliant) and therefore offer greater sensitivity for most
samples. Shorter tips, on the other hand, may afford better control when gauging
strong attractive forces and are less prone to entrapment by surface tension forces.
The user must ultimately experiment to determine the best tip.

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11.3.4. Triggering
The Other Controls panel within the Z Scan Controls allows the use of various
triggers when obtaining Force Plot and Force Volume plots. The idea of a trigger
is simple: it limits the total amount of force exerted by the tip upon the sample.
Depending upon which trigger is used and how it is set, it is possible to operate the
trigger independent of drift (Relative) or at some arbitrarily fixed point (Absolute).

Total force

Figure 11.12. Reaction of absolute and relative triggers to drift.

The plots in Figure 11.12 above show the effect of drift on each of the two trigger
types. The plot series shown on the right side of Figure 11.12 utilizes a Relative
trigger and maintains force at a constant level defined by the Trig threshold parameter. As shown, the total force is maintained, even as the system drifts.
The plot series on the left side of Figure 11.12 utilizes an Absolute trigger. Notice
that as the system drifts (plot moves slowly downward), total force increases. Drift
may be due to mechanical causes, or due to thermal effects on the cantilever. An
Absolute trigger permits the total force to be set using Setpoint values.

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11.4. Force Plot Control Panels

The control panel window (Figure 11.13) is used to manipulate the microscope in
Force Plot mode and is displayed on the control monitor. Among other things, the
parameters control the start position and amplitude of the triangle wave applied to
the Z piezo. The setpoint value of the cantilever deflection voltage used in the feedback loop can also be adjusted. With the Motor / Tip Up and Tip Down buttons
(Figure 11.14), the stepper-motor can be used to adjust the position of the cantilever
tip relative to the sample. The Capture button stores the force plot for Off-line
viewing. It should be noted that some of the parameters influence the Real Time
operation of the microscope, while most of the menu parameters affect only the
Force Plot mode.
Z Scan Controls
Graph Controls
Z scan start:

146 nm

Other Controls
Trigger mode:

Z scan size:

500 nm

Trig threshold:

Z scan rate:

4.88 Hz

Trigger channel:

X offset:

0.00 V

Z step size:

Y offset:

0.00 V

Step threshold:

512

Number of samples:
Average count:
Sensitivity:

1
0.0379 V/nm

Units:

Off
0.00 V
Amplitude
2.40 V
7.53 V

Start mode:

Calibrate

End mode:

Extended

Indent Feedback:

Disabled

Metric

Figure 11.13. Z Scan Controls panel.

Motor Control
Step size:
Quit

Tip Up

1.00 m
Tip Down

Figure 11.14. Motor Control panel.

The input sensitivity of the SPM head must be defined properly to keep the values
on the vertical axis of the force plot accurate. The parameter In sensitivity should
be set to 0.125 by using the Real Time / Microscope / Calibrate / Detector command for each scanner used with the MultiMode microscope.

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11.4.1. Force Plot Control Panel Parameters

The various Force Plot control panels allow the operator to precisely control the
probe tips interaction with the sample surface. This is especially useful during contact AFM procedures, as it directly affects image quality and the degree to which
the sample is influenced by forces from the tip. Items in the various Force Plot control panels are discussed below.
Z Scan Controls panel
Z scan start Sets the maximum voltage applied to the Z electrodes of the piezo
during the force plot operation. The triangular waveform is offset up and down in
relation to the value of this parameter. Increasing the value of the Z scan start
parameter moves the sample closer to the tip by extending the piezo tube. The units
of this item are volts or nanometers, depending on the setting of the Units parameter. The initial value of Z scan start is equal to the average Z-center voltage defined
by the feedback just prior to entering Force Plot mode. Decreasing the value of this
parameter shifts the force curve on the display to the left, while increasing the
parameter shifts the curve to the right.
Z scan size Fixes the amplitude of the triangular waveform applied to the Z
piezo. The units of this item are volts or nanometers, depending on the setting of the
Units parameter. Regardless of the size of the scan, the entire scan is shown in the
force curve; therefore, increasing the value of this parameter has the effect of compressing the curve on the display.
Number of samples Defines the number of data points captured during each
extension-retraction cycle of the Z piezo. This parameter does not affect the number
of samples used in Image Mode.
Average count Sets the number of scans taken to average the display of the force
plot. May be set between 1 and 1024. Usually it is set to 1 unless the user needs to
reduce noise.
Sensitivity (as applied to contact AFM) This parameter relates the cantilever
deflection signal to the Z travel of the piezo. It equals the slope of the deflection
versus Z voltage line when the tip is in contact with the sample (e.g., between 3 and
4 in Figure 11.5). The NanoScope system automatically calculates and enters the
value from the graph after the operator uses the mouse to fit a line to the graph.
This item must be properly calculated and entered before reliable deflection data in
nanometers can be displayed in Real Time mode. For a proper force curve, the line
has a negative slope with typical values of 10-50 mV/nm; however, by convention,
values are shown as positive in the menu.
Sensitivity (as applied to TappingMode) Sensitivity relates the vibrational
amplitude of the cantilever to the Z travel of the piezo. It is calculated by measuring
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the slope of the RMS amplitude versus the Z voltage when the tip interacts with the
sample as shown in Figure 11.10. The NanoScope system automatically calculates
and enters the value from the graph after the operator uses the mouse to fit a line to
the graph. This parameter must be accurately calibrated before amplitude data
obtained in LiftMode will be accurate.
Units This item selects the units, either Metric lengths or Volts, used to define
the parameters and the horizontal axis of the graph. Changing this item in Force
Plot also changes it in the Real Time imaging mode. Metric units are obtained from
the Z sensitivity for the particular scanner. under microscope/calibrate/scanner.
Feedback Controls panel
Setpoint (as applied to contact AFM) The cantilever deflection voltage maintained by the feedback loop in Real Time mode can be adjusted by changing this
parameter. In Force Plot, this parameter defines the centerline of the vertical, Cantilever Deflection Voltage axis of the force plot curve shown on the display monitor. Changing the Setpoint shifts the force plot curve on the graph, because the
centerline value is always equal to the setpoint. For example, if the Setpoint is set
to -3.0 volts, the cantilever deflection axis of the graph will be centered around -3.0
volts. Raising the Setpoint to -2.0 volts will shift the force plot curve down by one
volt so the graph will be centered at -2.0 volts. Changing the value of this parameter
in the Force Plot mode also changes the Real Time setpoint in the Real Time control
panel.
Setpoint (as applied to TappingMode) The RMS value of the cantilever deflection voltage maintained by the feedback loop in the Real Time mode can be
adjusted by changing Setpoint. In the TappingMode force plot mode, Setpoint
defines the centerline of the vertical, Tip Amplitude axis of the amplitude calibration plot shown on the display monitor. Changing the Setpoint shifts the amplitude
curve on the graph, because the centerline value is always equal to the Setpoint.
For example, if the Setpoint is at 3.0 volts, the RMS amplitude axis of the graph
will be centered around 3.0 volts; raising the setpoint to 4.0 volts will shift the
amplitude curve down by one volt, so the graph will be centered at 4.0 volts.
Changing the value of this parameter in the Amplitude Calibration mode also
changes the Setpoint parameter in the Real Time control panel.
Input attenuationChanges the gain applied to the input signal. The input signal
can be reduced by a factor of eight to see more of the Force Plot plot's signal amplitude. This parameter is also changed in the Real Time menu and affects the resolution of the system; therefore, it should be changed to 1X before returning to
imaging.

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Drive frequency (TappingMode only) This parameter defines the frequency at

which the cantilever is oscillated. This frequency should be very close to the resonant frequency of the cantilever. Changing the value of this parameter in the Force
Plot menu also changes the Drive frequency parameter in the Real Time control
panel.
Drive amplitude (TappingMode only) This parameter defines the amplitude of
the voltage applied to the piezo system which drives the cantilever vibration.
Changing the value of this parameter in Force Plot mode also changes the Drive
amplitude parameter in the Real Time control panel. It is possible to fracture the
cantilever by using too high of a drive amplitude; therefore, it is safer to start with a
small value and increase incrementally. If the amplitude calibration plot consists of
a flat line all the way across, changing the value of this parameter should shift the
level of the curve. If it does not, the tip is probably fully extended into the surface.
Channel 1, 2, 3 panels
Data type Amplitude (TappingMode only), Deflection, Friction, Aux BD.
Z range Vertically scales the cantilever deflection signal versus Z voltage graph
shown in the force plot. Increasing this parameter expands the range of the display
about the centerline causing more of the force curve to fall on the graph. Initially,
this parameter should be set to its maximum value, then gradually reduced.
Motor Control panel
A separate Motor Control panel allows operators to move the probe at will. This
control is used during the Force Plot procedure to adjust tip height above the sample surface. Movement is limited to a maximum of 1.0 m per step.
Tip Up This command moves the tip up by the SPM step size displayed inside
the window.
Tip Down This command moves the tip down by the SPM step size displayed
inside the window.
Menu Bar Commands
Capture The Capture button stores the force plot for Off-line viewing.
Probe menu commands These commands allow for highly controlled probe
movements to prevent damage to the tip. Each of these commands has an icon
which can be accessed directly from the menu bar. Probe menu commands are
especially helpful when performing force plots in TappingMode and are described
in the Command Reference Manual.

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11.5. Imaging Local Elasticity with Force

Modulation
11.5.1. Introduction
This section describes the operation of force modulation (Forcemod) mode, which
can be used to image local sample stiffness or elasticity. This method may be especially useful for imaging composite materials or soft samples on hard substrates
where it is possible to obtain contrast between regions of different elasticity.
This section assumes knowledge of operation of contact mode AFM in air, as
described in Chapter 7. It is useful, but not essential also to have experience operating with TappingMode.
Force modulation measures local sample elasticity by oscillating a probe such that
its tip indents slightly into a sample. The tip will be able to indent a soft material
more easily than a harder material. The amount of cantilever deflection is inversely
related to the amount of indentation. For example, an extremely soft sample will
allow the tip to indent deeply into the surface, resulting in a very small deflection of
the cantilever. A very hard sample allows less indentation, with the cantilever
deflected by a larger amount. The relative elasticity of the sample is measured by
recording the amplitude of the tip deflection versus position over the sample as
depicted in Figure 17. Contrast is generated as the cantilever scans the surface from
left-to-right. When it encounters a hard site (dark area) embedded in the softer
medium, the harder material absorbs less of the cantilevers energy, causing an
increase in the cantilevers response and signal amplitude.

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Large cantilever response

on hard material
Small cantilever
response on soft material

Soft Material
Large Indentation

Hard Material
Small Indentation

Figure 11.15. How contrast is generated in force modulation mode.

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Force modulation requires the use of a special optional tipholder, shown in

Figure 11.18. This tipholder uses a piezoelectric bimorph to oscillate the cantilever
against a sample surface. The force modulation tipholder is similar to the standard
tipholder; however, its piezo stack is much larger and lower frequency than the
standard tipholder used for TappingMode operation.

Bimorph

Figure 11.16. MultiMode force modulation tipholder.

To obtain good contrast while using force modulation, choose a cantilever that has a
similar spring constant to the sample material. If the cantilever is much softer than
the sample material, the cantilever will not indent sufficiently into the surface to
generate an image. It may take some experimentation to find a cantilever that
matches the sample's requirements. For rubber and plastic samples DI recommends
trying, for example, 225 m long force modulation (Model # FESP) silicon cantilevers. For more delicate, biological samples, try 450 m long silicon cantilevers or
silicon nitride cantilevers.

11.5.2. Selecting a Force Modulation Tip

The key consideration when selecting a force modulation cantilever is its spring
constant. Ideally, the cantilever must have a spring constant which compliments the
pliancy of the two materials being contrasted. (Or close to the pliancy of one, but
not the other.) This way, the tip will indent into one material more than the other,
providing good force modulation image contrast. If the tip is so stiff that it indents
equally into both materials, or so soft that it indents neither material, then no contrast (elasticity) will be seen in the force modulation image. Instead, the image will
consist primarily of edge and frictional artifacts. If a force modulation tip proves
inadequate, the user may switch to a probe having a lower (softer) spring constant
(e.g., silicon nitride or a 450 m, contact AFM tip). Extremely hard materials may
require stiffer (harder) tips such as 225 m, single crystal silicon TappingMode
tips.

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Modulation Tips

Model No.

Cantilever Length

Spring Constant

Standard Silicon Nitride

NP, DNP

100200 m

0.010.6 N/m

Oxide-sharpened
Silicon Nitride

NP-S,
DNP-S

100200 m

0.010.6 N/m

Contact AFM
Etched Silicon

ESP

450 m

0.020.1 N/m

Force Modulation
Etched Silicon

FESP

225 m

15 N/m

TappingMode
Etched Silicon

LTESP

225 m

2070 N/m

TappingMode
Etched Silicon

TESP

125 m

20100 N/m

Cantilever

HARDER

TABLE 7. Force

SOFTER

Digital Instruments offers cantilevers having a wide range of spring constants

which are listed below. The choice of tip depends upon how hard the sample is.
Generally, it is preferable to use the stiffest cantilever giving the best elasticity contrast for the sample; try starting with a stiffer cantilever then working toward softer
tips. For samples of unknown hardness, start with a force modulation cantilever
(Model No. FESP) to determine whether the tip is sufficiently stiff, then adjust
accordingly.

11.5.3. Force modulationOperating Principle

Force modulation mode is very similar to contact AFM mode. The NanoScope III
system scans the cantilever over the sample surface while attempting to keep cantilever deflection constant. A setpoint is entered to tell the system how much the cantilever should be kept deflected during operation. In addition, the cantilever will be
oscillated up and down by a piezoelectric bimorph in the tipholder so that the tip
indents slightly into the sample surface as it is scanned across the surface. The
NanoScope III system records the amplitude of the cantilever motion, which indicates the relative indentation of the tip into the surface.
Harder sites on the sample surface cause increased cantilever response and amplitudes and are rendered as darker areas of the image. Softer sites absorb more of the
cantilevers energy, causing a reduced cantilever response and lower amplitudes;
these sites are rendered as lighter areas of the image.

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11.5.4. Force modulationProcedure

This section gives instructions for operating in force modulation mode.
1. Choose the Force Modulation operating mode.
Go to the Other Controls panel. Switch the AFM mode parameter to Forcemod.
2. Adjust the setpoint
Enter a Setpoint. It is usually convenient to enter a Setpoint of 0.0 V. Recall that
higher setpoints cause the cantilever to push harder on the surface during scanning.
3. Set the MultiMode switch to TappingMode.
When using Forcemod, the Vertical Deflection/Setpoint is shown in the center of
the lower meter.
4. Adjust the detector offsets
Turn the detector adjustment screws to center the laser spot on the laser detector.
Typically, the Vertical Deflection is adjusted to approximately -1.0 V. The force
that the cantilever will apply to the surface is related to the difference between the
Vertical Deflection and the Setpoint. If the sample is very delicate, it may be preferable to set the Vertical Deflection value closer to the chosen Setpoint.
5. Enter the Cantilever Tune menu
Regarding cantilever oscillation
The cantilever is oscillated by a small piezoelectric bimorph mounted in the
tipholder. For most samples it is necessary to oscillate the bimorph at or near its resonant frequency. This ensures the cantilever moves with sufficient amplitude to produce elasticity contrast.
The bimorph's resonant frequency is the frequency at which it produces the greatest
motion for a given Drive Amplitude (typically 530 kHz). In free air, this resonant frequency will appear as one or two among several peaks on the Cantilever
Tune screen; however, peaks due to cantilever resonance should be ignored. To distinguish between cantilever and bimorph peaks, the tip of the cantilever may be
brought into light contact with a sample surface. This will dampen all but the
bimorph peak(s), which will appear prominently on the Cantilever Tune screen. A
procedure is described below that is familiar to users of TappingMode.

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6. Set up and find the bimorph resonance.

Notes:

It should be necessary to find the bimorphs resonant frequency only once.

(Resonant frequencies are unique to each force modulation tipholder.) Once the
resonant frequency is found, write it down for future use. The resonant Drive
frequency may be used as a starting place each time that force modulation
imaging is performed; however, the bimorphs resonant frequency in free air
should be rechecked using Cantilever Tune each time a new tip is installed.
Ensure the tip is close to the surface (20-30 microns) before starting.
Select the View / Cantilever Tune menu, or click on the Cantilever Tune icon.
The display monitor will plot the Frequency Sweep, showing the cantilever's oscillation amplitude vs. frequency. This plot is used to find the frequency where the
bimorph oscillates with the largest amplitude.
Cantilever Tune
Auto Tune Controls
Start frequency:

0.000000 KHz

End frequency:

Auto Tune

500.000 KHz

Graph Controls

Main Controls
40.0000 KHz

Sweep width:
Sweep sample count:
Sweep graph range:

256
100 nm
Metric

Units:

Quit

Motor

Drive frequency:
Setpoint:
Drive amplitude:
Input attenuation:

20.0000 KHz
-0.200 V
867 mV
1x

Integral gain:

10.00

Proportional gain:

10.00

Interleave Controls

Start with a Drive frequency of approximately 20 kHz and a Sweep width of

approximately 40 kHz. Enter a Drive amplitude of 1.5 V to start (this will be

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adjusted later). A series of peaks should be observed on the Frequency Sweep plot.
A typical Frequency Sweep plot is shown in Figure 11.17.

Peaks due to bimorph

Peaks due to cantilever

Figure 11.17. Typical frequency sweep plot.

(NOTE: Several peaks may appear.)
Adjust the Sweep graph range and/or the Drive amplitude until the peaks are
clearly seen. Make certain, however, that the Sweep graph range and/or Drive
amplitude is adjusted so that the top of each peak is seen. Note that while in Forcemod the Setpoint cannot be used to move peaks up and down.
7. Locate bimorph peaks; eliminate stray peaks.
In order to separate cantilever peaks from bimorph peaks, it will be necessary to
lightly touch the tip to the sample surface. This will dampen all cantilever peaks,
leaving behind those which are due solely to the bimorph.

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To touch the tip to the sample surface, do the following:

Click on the Motor button located within the Cantilever Tune panel. The Motor
Control panel will be displayed.
Motor Control
Step size:
Quit

Tip Up

1.00 m
Tip Down

Set the Step size parameter at 1.00 m, then click on the Tip Down button repeatedly until the tip lightly contacts the sample surface. When the tip makes contact
with the surface, a rapid change will occur in the Frequency Sweep plot: multiple
peaks will give way to one or two larger peaks (e.g., at 8.00 and 20.00 KHz). An
example is shown in Figure 11.18.

Bimorph Peaks

Figure 11.18. Typical frequency sweep plot showing bimorph peaks.

Identify the bimorph resonant peak(s). Bimorph resonances usually occur around 8
kHz and 20 kHz. Choose a peak, then click on the Zoom In command (top menu
bar of display monitor) with the left mouse button. Two vertical lines will appear on
the Frequency Sweep plot. Use the mouse to move the vertical lines back and forth
until the selected peak is centered between the lines. Increase or decrease the zoom
range by clicking on the left mouse button again. When the peak is centered and the
zoom width has been adjusted, click twice on the right mouse button. This will
automatically change the Drive Frequency and Sweep width and zoom in on the
selected peak.

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An alternative method is to use the Offset command on the display monitor to center the peak in the graph. Click on the Offset command with the left mouse button;
a vertical green line will appear on the plot. Move the line until it is centered on the
desired peak (usually the frequency with the highest amplitude), then click the left
button again to lock it. Click on Execute. The computer will automatically change
the Drive frequency so that the peak is centered. It may be necessary to click on
this command more than once to get the peak properly centered.
Once the desired frequency is chosen, the Frequency Sweep plot should be recentered similarly to the plot shown below.

Figure 11.19. Correctly tuned forcemod frequency.

Drive frequency may also be changed by clicking on the Drive frequency parameter on the control monitors Feedback Controls panel, then entering a new value.
REMEMBER: Bimorph resonance should be between 5 kHz and 30 kHz. If peaks
are found at a much higher frequency, these are cantilever resonances, not bimorph
resonances.

Notes

If the bimorph resonant frequency was determined by placing the tip in contact
with the surface, do not use that tip for force modulation imaging. Replace the
cantilever with a new tip and double-check the resonant frequency without
contacting the tip to the surface. From this point forward, cantilever tune should

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be performed (without touching the surface) starting at or near the bimorphs

resonant frequency each time a new tip is installed. Slight shifts in the frequency
response may occur with different tips.
8. Check the scan parameters.
Check the various scan parameters, such as Scan speed, Scan size, Integral gain,
etc. to verify they are reasonable for contact mode imaging. Also, it may be desirable to readjust the photo detector vertical adjustment screw if the Vertical Difference signal has drifted from the value originally set.
9. Select the proper Data Types.
The multi-image capability will be used to view both the topography data and the
force modulation (elasticity) data at the same time. For the Channel 1 image, select
Data Type: Height. For the Channel 2 image, select Data Type: Amplitude.
The Data Type chosen for the Channel 1 image will be displayed when using the
Browse command. If desired, the above choice can be reversed so that the surface
topography (Height) is chosen for Channel 2.
10. Reduce the Drive Amplitude before engaging.
Reduce the Drive Amplitude to 0.00.
11. Initiate the Engage command.
Select the Motor / Engage command. The motor will begin to move the SPM head
down towards the sample and will stop once the cantilever is deflected to the chosen
Setpoint. Under some conditions the system may false engage immediately after
selecting the Engage command or before the cantilever actually reaches the surface. If this happens, reduce the Drive Amplitude and/or increase the Setpoint and
try again. If other difficulties are encountered, see the Troubleshooting section of
this manual.
12. Optimize scan parameters for Height Image.
First, adjust the Integral Gain, Proportional Gain, Setpoint, and Scan Speed to
obtain a good topography (Height) image. This procedure will be very similar to
optimizing the AFM for normal contact mode imaging, except that the gains will
probably be higher. Typically, force modulation operation requires Integral Gain
and Proportional Gain values of 10-20.
CAUTION: If employing stiffer cantilevers than those normally used, the sample
may be damaged by the cantilever tip. To minimize this damage, make the Setpoint
as low as possible.

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ATTENTION! Lutilisation dun levier plus rigide que ceux utiliss habituellement peut entraner un endommagement de lchantillon par la pointe. Afin de
rduire les risques dendommagement, ajuster la valeur cible du rtro-contrle (Setpoint) sa valeur la plus faible possible.
WARNHINWEIS! Falls Sie mit Cantilevern hherer Federkonstanten arbeiten, als
normal blich, kann die Probe durch die Spitze beschdigt werden.. Um eine evtl.
Beschdigung zu minimieren bzw. zu vermeiden, benutzen Sie bitte einen Arbeitspunkt (Setpoint), der nur geringfgig ber der freien Deflektion des Cantilevers
liegt. Die Differenz zwischen Setpoint im Feedback-Men und der freien Deflektion des Cantilevers (Photodetektorsignal A-B) sollte minimal sein.
Reduce the Setpoint using the cursor keys until the cantilever pulls off the surface.
Note the value of the Setpoint when the cantilever pulled off the surface (pull-off
value). Increase the Setpoint until the cantilever begins to touch the surface again
and an image appears. Finally, readjust the setpoint so that it is slightly more positive than the pull-off value.
Be aware that there is a trade-off here! If the Setpoint is adjusted very close to the
pull-off value, imaging will be performed with the smallest and least damaging
force. However, imaging may be more unstable, as the cantilever may pull off the
surface unexpectedly.
Also note that the setpoint value can affect the force modulation contrast as discussed below. It may be desirable to further adjust the setpoint after completing
step 11.4.19.
13. Examine the contrast of the force modulation image.
The amplitude signal shows how much the cantilever can indent into the surface.
Softer features will allow the cantilever to indent further into the sample, giving a
small deflection amplitude, while hard features will allow little indentation and create large deflection amplitudes. The force modulation software is configured so that
softer areas will appear lighter (higher) in the amplitude image. The relative elasticity of the sample is seen as contrast between dark and light areas in the amplitude
image. Therefore, the amplitude image is really the inverse. This allows soft samples mounted on firm substrates to show up as positive shapes relative to the background.
14. Optimize Drive Amplitude for Force Modulation imaging.
Next, optimize the force modulation signal, which is the amplitude data. The
amount of contrast and the quality of both Height and Amplitude images will
depend on the Drive amplitude. In general, increasing the Drive amplitude will
give greater contrast in the force modulation image.

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It is possible, however, to set the Drive amplitude too high. In this case, as the
Drive amplitude is increased, contrast will remain unchanged in the Amplitude
image. Instead, the overall contrast in the force modulation image will remain
roughly constant, but more artifacts will be observed in the image.
For example, if the drive amplitude is too high, the force modulation image will
become contaminated by edge effects or friction effects.
The best procedure is to operate at the lowest drive amplitude that gives sufficient
contrast to examine the sample. Low drive amplitudes will also help extend the life
of the cantilever tip and reduce sample damage.
Here is a suggested procedure for optimizing the drive amplitude:

Reduce the drive amplitude to a very small value (say 100 mV).
Increase the Drive amplitude with the arrow keys or by typing in new values.
The contrast of the Amplitude (force modulation) image should increase.

Continue increasing the Drive amplitude until sufficient contrast appears in the
Amplitude image.
If the Drive amplitude is increased to the point where contrast is no longer
improving, reduce the Drive amplitude slightly from this value.
As mentioned above, the force modulation contrast will also depend on the Setpoint. In general, if using a larger Setpoint (larger tracking force) it will be necessary to use a smaller Drive Amplitude to obtain good force modulation images
without artifacts.
If it is difficult to obtain a clear force modulation image that is free of artifacts, try
reducing (or sometimes increasing) the Setpoint and then optimizing the Drive
Amplitude again.
15. Readjust gains (if necessary).
The value of the Drive amplitude may also affect the contact mode image, making
the system more or less likely to go into unwanted oscillations. If the Drive amplitude is changed by a large amount it may also be necessary to readjust the Integral
gain and Proportional gain. The gains should be set as high as possible to track the
sample topography, but not so high that they show the oscillation due to the
bimorph oscillation. If the gains are set too high, parallel diagonal lines will be
observed on the Height image. If an oscillation is seen, the feedback system is trying to cancel the cantilever oscillation by moving the Z-axis piezo in the opposite
direction. If there is evidence of an oscillation in the Height data, turn the gains
down until the oscillation stops.

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Notes

Oscillations not visible in height Image Mode data may be seen more easily
using Scope Mode.
Sometimes an oscillation that appears in the data will be due to aliasing as
described in the next section. If gains cannot be adjusted to eliminate unwanted
oscillations without compromising the height images quality, see the next section
below.
16. Changing the Drive Frequency to eliminate aliasing.
Under some conditions, unwanted oscillations will appear in the data due to aliasing of the Drive Frequency with the image pixel rate. This problem can be eliminated by changing the Drive frequency by small increments. Use the arrow keys to
change the Drive frequency up or down very slightly until the oscillation disappears. On some materials, shifting the Drive frequency slightly (1-3 Hz) below or
above a resonant peak value may improve image contrast. Operators are encouraged to experiment.

Notes
It is possible to see artifacts in force modulation images that are not due to differences in elasticity. Some artifacts to watch for are outlined below:
Edge effects
Sometimes force modulation images will show changes in amplitude at the edge of
topographic features like steps or bumps. These artifacts may look like the derivative of the sample topography.
To see if a feature is an edge effect, try reversing the Scan direction from Trace to
Retrace, for example. If the contrast reverses or the amplitude change now appears
on the other side of the topographic feature, then the amplitude change is likely due
to the topographic edge, not differences in elasticity. To minimize edge effects,
reduce Drive amplitude, Setpoint or Scan speed. Also set the Integral gain and
Proportional gain as high as possible without causing unwanted oscillations.
Frictional effects
Because the cantilever is held at an angle to the sample surface, the cantilever tip
will slide laterally (skate) as the tip is pushed into the sample.

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This is shown schematically in Figure 11.20. The amplitude of cantilever motion

can then be affected by differences in friction between two different materials. For
this reason, force modulation images may also contain information about differences in local frictional forces. To reduce the influence of frictional effects, use a
smaller Setpoint and/or Drive amplitude.

1516

tip moves
down and left

substrate moves down

Effect of friction on force modulation images

Figure 11.20. Effect of friction on force modulation images.

Tip Shape
The amount of indentation into a surface for a given applied force depends on the
shape of the cantilever tip. For the same Drive Amplitude a sharper tip will indent
deeper than a dull tip. Since it is possible for the tip to dull during imaging, consider replacing the cantilever if the force modulation contrast deteriorates over
time. Also, note that it will be difficult to obtain reproducible, quantitative elasticity
measurements between different samples and different cantilevers because the tip
shapes may be different. In general, the force modulation technique is a qualitative
tool for identifying regions of harder and softer material on a sample, rather than a
tool for quantitative analysis.
Not all samples lend themselves to standard force modulation imaging. Even samples having excellent elasticity contrast may not show up in force modulation if
their absolute elasticity is out of instrumental range. A new method, negative LiftMode, is described below which may prove useful for imaging otherwise difficult
materials.

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11.6. Force Modulation with Negative LiftMode

A new form of force modulation imaging utilizing TappingMode and LiftMode
operation has recently been introduced. This method, known as negative LiftMode, allows imaging of certain materials previously not visible with contact
mode AFM force modulation. The method is especially suited for some softer
materials, yielding higher resolution. A general procedure is described below.

Notes

Force modulation contrast is very sensitive to the spring constant of the tip,
which varies according to the length and thickness of the cantilever.
TappingMode may be easily performed with either force modulation or
TappingMode cantilevers, but may prove difficult with contact AFM silicon and
silicon nitride cantilevers. (See table in Section 11.5.2 for guidance.)

11.6.1. Find Resonance of the Bimorph

The force modulation tipholder features a bimorph, which excites the probe and
cantilever mount. Refer to Section 11.5.9 for guidance on finding bimorph resonance.
1. Ensure the probe is withdrawn from the sample surface. Switch the AFM mode
parameter to Tapping.
2. Set Drive amplitude on the Interleave Controls panel to 200400 mV.
3. Go to the Real Time / View / Cantilever Tune dialog box. (For version 4.10 or
later software, also click on the Manual button within this box.)
4. Next, select the Interleave Controls button to access tuning controls for interleaved scans.
5. The bimorph resonance may be found using manual controls. Bimorph resonance
is usually about 8-12 KHz. Start with a Sweep width of 10 KHz and a Drive frequency of 10 kHz. Determine the Drive frequency, using Section 11.5.9 above as
a guide.
6. Verify that the Drive frequency parameter in the Interleave Controls panels is
set to the bimorphs resonant frequency. Click on the enable button next to the
Drive frequency parameter; the enable button should appear green. Quit the Cantilever Tune dialog box.

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11.6.2. Set Interleave Controls

1. Transfer to the Real Time / Interleave Controls panel.
2. Set the Interleave scan parameter to Lift. Set Lift start height and Lift scan
height to 0.00 nm.
3. For now, set the Interleave mode parameter to Disabled.

11.6.3. Obtain a TappingMode Image

While negative LiftMode force modulation data will be imaged using Channel 2,
height data will be obtained using TappingMode on Channel 1. The user must
therefore obtain a satisfactory TappingMode image.
1. Verify that the Interleave mode parameter on the Interleave Controls panel is
Disabled. Verify that the AFM mode parameter in the Other Controls panel is set
to Tapping.
2. Select Real Time / View / Cantilever Tune. On version 4.XX software, the cantilever may be tuned using Auto Tune. Enter a main controls Start frequency value
of 5 KHz and End frequency value of 400 KHz. On version 3.XX software, use
manual controls. Set the Drive frequency value in the Main Controls box of the
Cantilever Tune dialog box to the cantilevers resonant frequency. Exit the Cantilever Tune dialog box.
3. Verify that all Scan controls and Feedback Controls parameters are set for
obtaining a TappingMode image.
4. Set the Channel 1 panels Data type parameter to Height. Set the Line direction to Retrace and enter an appropriate Z range value for your sample.
5. Engage the sample surface and obtain a good TappingMode image.

11.6.4. Obtain a Negative LiftMode Force Modulation Image

1. Set the Data type parameter in the Channel 2 panel to Amplitude. The Line
direction parameter should be set to Retrace.
2. Switch the Interleave mode parameter in the Interleave Controls panel to
Enabled. Negative LiftMode imaging is now in effect.

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3. Using the left arrow key, optimize the negative LiftMode image by slowly
decreasing the Lift scan height parameter in the Interleave Controls panel from
zero until the surface is reached. In most cases, it should not be necessary to go
below -60.0 nm. (This is sometimes best performed while in Real Time / View /
Scope Mode.)

Notes

Use of a negative Lift scan height value here gives rise to the term negative
LiftMode. When the interleaved scan is enabled, the tips TappingMode height
above the sample will be reduced by the Lift scan height amount. This places
the oscillating tip in contact with the sample as surface features are profiled
(from TappingMode data). The contrast between light and dark reveals areas of
high and low elasticity, with the dark area indicating harder material and the
lighter areas indicating softer material.
4. Adjust the interleaved Drive amplitude and Lift scan height until the force
modulation image is optimized. This may require some experimentation.

Notes

If you are seeing a lot of contrast in the amplitude image before reaching the
surface, try reducing the Integral and Proportional gains. It may be necessary
to adjust gains slightly lower than when performing normal TappingMode
imagery. A good way to check this is to enter a Lift scan height of 100 nm, then
adjust gains (and possibly Drive amplitude) until you see the minimum amount
of contrast in the amplitude image. (This may be easily monitored in Scope
Mode.) Once contrast is minimized, enter a Lift scan height of 0.0 nm and
begin approaching the surface.

11.6.5. Final Comments

Best results using negative LiftMode have been obtained on relatively smooth samples (< 500 nm vertical features); however, DI encourages experimenting with this
technique on rougher surfaces as well.

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11.7. Force Volume Imaging

11.7.1. Description
The usefulness of force plots has been shown in the preceding sections of this chapter. Force plots may be made even more useful by plotting across the surface of a
sample at regular intervals, then analyzing the result. This is known as force volume
imaging. The word volume is used because for each X-Y position there is a force
curve in Z for some selected range. Each curve gives a cumulative force for that
area of the sample. By plotting these values along X and Y coordinates, a force volume image is rendered which permits the viewing of stratified layers of force at various Z-axis heights above the sample surface.
Force volume images require preliminary use of the Force Plot function. The
microscopist must have a basic working knowledge of this function before attempting Force Volume (see Section 11.2 above). Before obtaining a force volume
image, it is also important to determine exactly what is sought after and what is
available for a given mode of imaging. The matrix below summarizes each of the
major imaging types.

Signal Type

Contact AFM

Amplitude
Deflection
Frictiona
Phaseb
Frequencyb
Potentialb

4
4

TappingMode

4
4
4
4
4

a. The usefulness of force imaging with friction has not yet been determined.
b. Phase, frequency and potential measurements are available only on SPMs equipped
with the Extender Electronics Module.

The type of force image captured from a surface will depend upon how the SPM is
set up. For example:

If an MFM image is being captured, force volume imaging (phase) allows the
detection of long-range magnetic forces otherwise difficult to detect.

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For ordinary contact AFM, the use of force volume imaging (deflection) allows
the user to see otherwise invisible electrostatic forces.

Notes

It is incumbent upon the microscopist to carefully define all force volume

experiments. At this writing, there are at least ten types of force volume
imaging, including numerous combinations of triggers, drive frequency and
amplitude, Z-axis direction, offset, etc. The utility of each image is subject to
the interpretations and controls of the experimenter. This section of the
Instruction Manual cannot cover all possible force volume types; therefore,
discussion is limited to a general description of controls and an example in
contact AFM. Experimentation is encouraged. Interpretations are subject to
experimental controls.

11.7.2. Setting Up for Force Volume

To summarize, force volume imaging executes the following tip motions:

The tip is lowered and pressed against the sample surface until the cantilever is
deflected to the Trig[ger] threshold value. If the surface is not contacted within
one Z scan size distance, the tip is extended one additional Z scan size (for a
total distance of two times the Z scan size), then retracted one Z scan size. This
means that the tip is incrementally lowered (or racheted) one Z scan size for
each extension-retraction cycle until the surface is contacted, or the Z piezo
reaches its total maximum of 220 volts.

Once the tip contacts the surface and deflection attains the Trig[ger] threshold
value, sample height is recorded for that Z-axis threshold. A force curve is
recorded for the X-Y coordinate after the piezo retracts. The tip is lifted clear of
the surface and translated in X-Y to the next coordinate. The entire process is
then repeated.
The general sequence for obtaining a force volume image consists of the following:
1. Obtain a height, deflection, amplitude or phase image of the sample in Image
Mode. On the Channel panel, select the same Data type intended for force plotting and for triggering.
2. Obtain a Force Plot of the sample surface (any portion of the surface will suffice). Using the force plot, determine the samples general force characteristics and
set the following parameters: Setpoint, Z range, Z scan size, Z scan start, and
Trigger mode.

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Notes

A trigger will be required to obtain a height image during force volume

imaging.
3. Return to Image Mode.
4. Obtain a Force Volume image by selecting View / Force / Volume. Set the following parameters in the Z Scan Controls panel: Z scan rate, FV scan rate,
Number of samples, Force per line, Samples per line, Display mode, Sample
period. Fine tune Image Channel parameters to obtain a height image. Based upon
the experimental design, set parameters in the FV (Force Volume) Channel and
Force Channel panels.
5. Capture the Force Volume image. Note that this will take longer than a normal
image capturethe force volume image may consist of up to 512 samples taken
512 times per line at the Z scan rate per pixel.
6. Interpret the Force Volume image using Off-line controls.

11.7.3. Obtaining Force Volume Images Using Contact AFM

Contact AFM offers perhaps the most intuitive introduction to Force Volume imaging. The forces described here will be limited to simple attractive forces (e.g., electrostatic and surface tension) and repulsive forces (e.g., electrostatic, and hard
contact or coulombic). The reader should already know how to obtain a basic contact AFM force plot. If not, review sections 11.12 in this chapter before proceeding further.
1. Mount sample and obtain a contact AFM image.
Initially, the sample should be familiar enough to obtain an image easily (e.g., silicon calibration reference). Make certain the AFM mode parameter in the Other
Controls panel is set to Contact. After engaging the surface, use a moderate Setpoint value. Optimize the Channel 1 parameters for a good image: set Data type
to Height and Real Time Planefit to Line.
2. Obtain a force plot of the surface.
To obtain a force plot of the surface, select Real Time / View / Force Mode / Calibrate. Set the Feedback Controls panel Input attenuation parameter to 1x. On
the Z Scan Controls panel a recommended default for Z scan rate is 40 Hz. To set

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the Sensitivity parameter, use the mouse to draw a line on the force plots parallel to
their slope. Click the left button to drop each end of the line; click on the right button to enter the Sensitivity value and erase the line.
The Start mode parameter should be set to Calibrate. The Trigger mode may be
set to Relative.

Click here
Se
ity
iv

it
ns
pe

slo

Click here

Figure 11.21. Obtaining a good force plot.

3. Return to Image mode.
When a good force plot is obtained, return to Image mode.

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4. Obtain a Force Volume image of the surface.

To obtain a force volume image, click on the Real Time / View / Force Mode / Volume option. The display monitor will appear similar to the one shown below,
except that most of the image windows will be blank at first. (A minimum of several minutes are required to obtain complete images.)

Figure 11.22. Force volume image.

The large image on the left side of the screen is a height image similar to the one
shown in Real Time / Image mode; however, it may appear more pixelated. The
smaller image at upper-right plots force as a function of Z distance. The resolution
of the force plot will vary, depending upon various parameter settings. Finally, the
force plot at the bottom-right corner of the screen displays a series of superimposed
force plots for each scan line.
5. Set Force Volume parameters.
There are six Force Volume panels which control sampling and scanning for the
force volume image and force curve. They are organized by function:

Image Scan Controls Real Time parameters for the height image shown in
the upper-left corner of the display monitor, such as Scan size, X- and Y offset,
Scan angle, and Scan rate.

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Image Channel More Real Time parameters affecting the height image.
Z Scan Controls Parameters affecting the tips vertical movements,
including Z scan start, -size and -rate.

Feedback Controls Parameters controlling Setpoint, and where the tip is to

be turned around (triggered): Trigger mode, -threshold and -channel.

FV Channel Force Volume channel controls affecting the force volume

image in the upper-right corner of the display monitor, including Volume scale,
Force per line, Z direction and -display, and Volume offset.

Force Channel More parameters affecting the Force Volume image.

Remember: you are constructing a map of many separate force plots across the
sample surface; therefore, there may be a great deal of data to sort through.
Depending upon settings, capturing a detailed force volume image can require
hours.

Notes
The total amount of data for any given force volume image file is limited to a
maximum 1 Mb by the relation
2

Force per line Number of samples 4 1 Mb

The following parameters are carried over from Force Plot settings: Z scan start,
Z scan size, and Z scan rate. Although these parameters may be altered during
force volume imaging, they should obtain their initial settings from the Force Plot
window.
Enter the Number of samples parameter to set the resolution (or number of
shells) of the force volume image and number of points plotted on the force curve
at the bottom of the display screen. The value of this parameter will not affect the
speed of the scan, but will affect the file size. A good default setting is 32.
Next, enter the Force per line value. This parameter determines the number of
force curves taken along each line of the sample and significantly affects capturing
speed. Enter a number which allows sufficient resolving of force-defined features,
but minimizes capturing time. A good default value is 64.
Finally, enter the Samples per line value. This parameter sets the number of samples to be displayed in the height image only and does not affect the force volume
image in any way. Increasing this parameter increases the capture time. A setting of
128 provides sufficient detail to resolve many small features while helping to
reduce capture time.

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The Display mode parameter may be set to show the Extend portion of the plot,
the Retract portion, or Both.
For most imaging, the Sample period parameter should be held at 30 s. (Sample
periods less than 30 s may be too fast and cause errors.) This parameter determines the sampling rate of data at the SPMs digital signal processor, which some
experimenters may wish to increase. This parameter is coupled with two other
parameters: the Z scan rate and FV scan rate; that is, changes in the Sample
period will change both Z scan rate and FV scan rate.
Keeping the Sample period minimized at 30 s will yield optimal data averaging
between Z-axis sampling points. As this parameter is increased, data averaging is
lessened and data becomes discrete.
6. Adjust Feedback Controls parameters.
Feedback Controls panel parameters carry over from the Force Plot settings; however, changes may be required to protect the tip and optimize the force volume
image.
For silicon nitride tips, the Setpoint may be adjusted to within plus or minus several volts of the microscopes vertical deflection signal value. For crystal silicon
TappingMode tips, the Setpoint should normally be increased no more than 1-3
volts below the RMS amplitude voltage; this will help protect the tip.
In Force Volume imaging, triggers are used to set the turnaround point of the Zaxis piezo. The Trigger mode determines the type of trigger to be employed. Two
types are offered: Relative and Absolute, or the trigger may be turned Off.

Notes

If the Trigger mode is turned Off, no height image will be displayed.

The Trigger channel determines which data channel is to act as the trigger. (Normally, this will be the same as the Data type located on the Force Channel panel.)
A Relative trigger measures the trigger threshold relative to the free-air voltage
deflection value and accommodates drift. An Absolute trigger sets the threshold relative to the Setpoint. Normally, the Relative trigger is the preferable default, as it
offers better protection to the tip and sample, keeping total force on the surface
independent of setpoint.

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Notes

When using a Relative trigger threshold, be certain a sufficiently large Z scan

size is in effect to deflect the cantilever to the Trig[ger] threshold value AND
lift the tip clear of the surface. This will ensure the tip is not racheted into the
surface and dragged laterally through surface material during X-Y indexing.
(Pre-version 4.23 software releases.)
To limit forces on the sample and tip, the Z scan size may be clipped to within
some Trig[ger] threshold value. For example, a tip which is being oscillated along
the Z-axis with a Z scan size of 500 nm may have its Trig threshold set to -25.0
nm. When using a Relative type of Trigger mode, if the tip encounters the sample
surface after extending 300 nm, it will halt its Z-axis extension at 325 nm, then turn
around (retract). Thus, tip-sample forces are restrained and the force curve is
defined for a controlled interval of tip-sample interaction.

Notes

This example assumes the Sensitivity parameter has been properly set (see step
#2 above) and that the detectors range has not been exceeded.
7. Adjust Force Channel parameters.
The Force Channel panel features parameters for the force plot at the bottom of the
display monitor. In most ways it is exactly like a Force Plot graph, except that it
superimposes up to eight multiple force plots (depending on Samples per line)
simultaneously for each scan line. When the next line is scanned, previously shown
plots are cleared.
The available settings for the Data type parameter will depend upon the type of
imaging being done. For example, Phase is available only on microscopes in TappingMode which have an Extender Electronics Module. Also available are
Amplitude, Deflection, Phase, Potential, and Thermal. Set the Data type accordingly.
Begin with a large Z range to locate the force plots. (At full size, the force plots
will probably resemble a thin line.) Slowly decrease the Z range value until the
force plots fill most of the graph.

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The Offset parameter determines where force plots are to be graphed relative to the
current Setpoint. When the Offset is Off, the graphs center horizontal line is positioned at the tips Setpoint value. When Offset is Enabled, the center horizontal
line is positioned at the tips free-air voltage (i.e., voltage when the tip is clear of the
surface).
8. Adjust FV [Force Volume] Channel parameters.
Parameters on the FV (Force Volume) Channel panel control the type and range of
forces viewed in the force volume image on the display monitor. In addition, the
Volume scale parameter also affects the viewable range of data captured during
force volume imaging.
The Z direction parameter determines which portion of the Real Time force curve
cycle (Extend or Retract) is shown on the display monitors force volume image.
For example, if the force of interest is material elasticity, the Extend portion of the
curve is usually selected. If the force of interest is electrostatic attraction, the
Retract portion of the curve is generally used.
The Volume scale parameter sets the range of values represented by the force volume image. Because force volume data is displayed line-by-line at periodic intervals, optimizing this parameter may require several adjustments. The results of
changing this parameter are not seen until the next line of force volume data is displayed.
The Z display and Volume offset parameters work in unison to define which portion of the superimposed force curves is to be plotted in the display monitors force
volume image. These parameters are also simultaneously represented as a green
cursor on the force plot graph. Both Z display and Volume offset may be changed
by positioning the cursor cross with the mouse, or vice versa. (The cursor is repositioned automatically whenever these parameters are changed.) Each parameters
relationship to the cursor is shown in Figure 11.23.

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Volume offset

Force Imaging

Setpoint
Free-air
deflection

Figure 11.23. Z Display and volume offset in relation to cursor.

Changing the Z display parameter determines where along the Z-axis the force
curve is to be plotted. For example, a Z display value of 25.0 volts would plot that
portion of each force curves Z-axis having a minimum 25.0 volts tip-sample separation. The Z display parameter may be thought of as defining bands of force at
fixed distances from the sample surface.
The Volume offset parameter adds or subtracts a constant value to the data signal to
be plotted. For most applications, Volume offset should coincide with a value on
the force curve itself. This is most easily accomplished by positioning the cursor on
the force curve. This centers the force volume image within the color bar of the
specified Z range.

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MultiMode Instruction Manual

Chapter 12

Interleave Scanning and LiftMode

Preface: Interleave Scanning & LiftMode

Interleave is an advanced feature of Nanoscope version III software which allows
the simultaneous acquisition of two data types. Enabling Interleave alters the scan
pattern of the piezo. After each main scan line trace and retrace (in which topography is typically measured), a second (Interleave) trace and retrace is made with data
acquired to produce an image concurrently with the main scan.
Typical applications of interleave scanning include MFM (magnetic force microscopy) and EFM (electric force microscopy) measurements; Chapter 13 provides
detailed instructions for obtaining MFM images of a standard magnetic sample.
Enabling Interleave with the mode set to Lift enacts LiftMode (patent pending).
During the interleave scan, the feedback is turned off and the tip is lifted to a userselected height above the surface to perform far field measurements such as MFM
and EFM. Topography data recorded during the main pass is used to keep the tip a
constant distance from the surface during the interleave trace and retrace. By
recording the cantilever deflection or resonance shifts caused by the magnetic or
electric forces on the tip, a magnetic force or electric force image is produced; see
Chapter 13. LiftMode was developed to isolate purely MFM and EFM data from
topographic data.
Interleave can also be used in Normal mode. In this mode, the feedback is kept on
while additional topography, lateral force, or force modulation data is acquired.
The Interleave commands utilize a set of Interleave Controls which allow several
scan controls (Drive amplitude, Setpoint, and various gains) to be set independently
of those in the main scan controls.

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This chapter provides a general discussion of the Interleave action and commands,
with emphasis on LiftMode. Chapter 13 provides step-by-step instructions for
using Interleave scanning and LiftMode for obtaining magnetic and electric force
data. For purposes of learning to use Interleave scanning, this section may be useful
even to those users whose end application is not magnetic force microscopy.

12.1. Interleave Mode Description

Enabling Interleave changes the scan pattern of the tip relative to the imaged area.
With Interleave mode disabled, the tip scans back and forth in the fast scan direction while slowly moving in the orthogonal direction as shown on the left of figure
12.1. This is the standard scan pattern of the NanoScope III.
INTERLEAVE
DISABLED
(standard)

INTERLEAVE
ENABLED
four Main and four Interleave
scan lines shown

four scan lines

(trace/retrace pairs)
shown

slow scan
direction
INTERLEAVE
trace and retrace

fast scan
direction

MAIN trace
and retrace

With INTERLEAVE enabled scanner executes

trace/retrace pairs, alternately performing a
MAIN pair, then an INTERLEAVED pair.
Vertical Scan speed is 1/2 normal rate with
twice the number of lines.

Figure 12.1. X-Y scan pattern.

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Interleave Scanning and LiftMode

With Interleave mode enabled, the system first performs a standard trace and
retrace with the Main Feedback Controls in effect. The tip moves at half the normal
rate in the slow scan direction. As shown on the right of figure 12.1, an additional
trace and retrace are then performed with the Interleave Feedback Controls enacted.
The frame rate halves because twice as many scan lines are performed for the same
scan rate.
Two modes are possible for Interleave scan: Normal and Lift. With Normal
selected, the feedback remains on during the Interleave pass with the values under
Interleave Feedback Controls (Setpoint, Gains, etc.) in effect. In Lift mode, the
feedback is instead turned off, and the tip lifted off the surface and scanned at a
user-selected height; see below.

12.2. Lift Mode Description

With the Interleave scan option set to Lift, the motion of the tip during the Interleave trace and retrace is as shown in figure 12.2.
Lift Trace

Main Trace
(Height Data)
Lift
Start
Height

Lift
Scan
Height

Lift
Scan
Height

Figure 12.2. LiftMode profiles.

The tip first moves to the Lift start height, then to the Lift scan height. A large
Lift start height can be used to pull the tip from the surface and eliminate sticking.
The Lift scan height is the final tip height. This value is added point-by-point to the
height data obtained during the Main topography trace and retrace. Values can be
positive or negative.

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12.3. Operation of Interleave Scanning / Lift Mode

These instructions apply to STM, contact AFM, or TappingMode AFM modes. It is
assumed the user is familiar with TappingMode or contact AFM to obtain good
images of surface topography. Use of Interleave scanning requires the steps below;
see Chapter 13 for specific examples using MFM.
1) Obtain a topography scan using the appropriate (usually Contact or TappingMode) method.
When using LiftMode, it is important that the gains and setpoint under Feedback
Controls be adjusted to give a faithful image of the surface. Because the height data
is used in the lift pass to trace the topography, a poor measurement of surface height
may give inaccurate measurement during the lift pass or cause the tip to strike the
surface. Typically, the height data is displayed on Channel 1.
2) Adjust the Interleave Controls panel to desired settings.
Choose the Interleave mode (Normal or Lift) appropriate for the measurements to
be performed. Set the Interleave Controls as desired. When using TappingMode, the
Drive amplitude, Drive frequency, Gains, and Setpoint can be set differently in
the Interleave Controls panel than in the main Feedback Controls panel; see section 12.4. However, it is often convenient to begin with the main and interleave values set equal; this can be done by toggling the bullets to the left of the appropriate
Interleave parameters to an "off" (grayed) condition. The values can be changed
once engaged. If using Lift, set the Lift start height and Lift scan height. If using
Normal mode, set the Gains and Setpoint.
Note that certain constraints are imposed: scan sizes, offsets, angles, and rates and
numbers of samples per scan line are the same for the main and interleave data, and
the imaging context (contact, TappingMode, or force modulation) must also match.
3) Enable the Interleave Scan.
Toggle the Interleave mode switch under Interleave Controls to Enabled. This
begins Interleave scanning; note that the scan rate in the slow direction is halved.
4) Choose the Interleave Data Type
This can also be done before enabling the Interleave. In Normal mode, the choices
of Data Type are the same as for the main scan. Depending on the type of microscope, Lift mode allows the options of amplitude, phase, or frequency data types
for doing far-field (MFM or EFM) imaging; see Chapter 13 for detailed examples.
Auxiliary channels are also available for some applications. Interleave data is typically displayed as the Second (right) Image.

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Interleave Scanning and LiftMode

5) Display the interleave data by switching Scan line (in the Channel panels) to
Interleave.

Notes

Lift scan height

The lateral and vertical resolutions of the Lift data depend on the distance
between tip and sample: the lower the tip, the higher the resolution. However,
the Lift scan height must be high enough that the tip does not contact the sample during the Lift trace and retrace.

Tip Shape
As shown in figure 12.2, the tip separation in the LiftMode is defined in terms of
the Z direction only. The Lift scan height is added to the height values taken
from previous scan lines point-by-point. However, the tip may be closer to the
sample than the Z separation indicates. On features with steep edges, the tip
may get very close to the sample even though the Z separation is constant; see
figure 12.2.

Scan Line Direction

The Line direction should be set to Retrace for both the main and interleaved
scans. If it is set instead to Trace, a band may appear along the left side of the
images due to the ramp between the surface and the Lift scan height.

12.4. Use of LiftMode with TappingMode

There are additional considerations when using LiftMode with TappingMode.

12.4.1. Main Drive Amplitude and Frequency selection

As usual, these parameters are set in Cantilever Tune before engaging. It is helpful
to keep in mind the measurements to be done in LiftMode when setting these values. For example, if Amplitude data will be monitored during the Lift scan for
magnetic force imaging, the Drive frequency should be set to the side of the resonance; see Chapter 13. (However, certain parameters can be set independently for
the Interleave scan; see below.)

12.4.2. Setpoint Selection

When the main and interleave Drive amplitudes and Drive frequencies are equal
(bullets under Interleave Controls disabled), the cantilever oscillation amplitude
increases to the free oscillation amplitude when the tip is lifted off the surface in

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LiftMode. If a small setpoint value forces the oscillation amplitude low while the
feedback is running, the amplitude can grow considerably when the tip is lifted free
of the sample surface. The change can also be large if the main Drive amplitude
was increased or the main Drive frequency altered after the tip was engaged. (The
vibration amplitude remains at the setpoint during the main scan even if these
parameters are changed.) This could make the tip hit the surface in the lift scan for
small Lift scan Heights.

12.4.3. Interleave Drive Amplitude and Frequency Selection

The cantilever drive amplitude can be set differently in the Lift scan as compared to
the main scan by toggling the flag on the left of the corresponding Interleave Control to "on" (green) and adjusting the value. This allows the tuning of a measurement in the Lift scan lines without disturbing the topography data acquired during
the Main scan lines. The Interleave Drive amplitude must be set low enough that
the tip does not strike the surface during the Lift pass.
CAUTION: Before enabling the Interleave Drive Amplitude, check that its value is
not much larger than the main Drive Amplitude value to prevent possible damage to
the tip.
ATTENTION: Lors dun travail en mode intercal (Interleave Mode), vrifier que
la tension applique pour osciller le bras de levier lorsquil est en positon haute
nest pas beaucoup plus importante que la tension applique lorsque ce mme bras
de levier est en position basse (Main Drive Amplitude). Le non respect de cette
procdure peut entraner la destruction de la pointe.
WARNHINWEIS: Bevor Sie im Interleave-Mode die Interleave Drive-Amplitude einschalten, vergewissern Sie sich bitte, da der dort eingetragene Wert nicht
wesentlich grer ist, als der Wert der Main Drive-Amplitude, um evtl. Beschdigungen der Spitze vorzubeugen.
The Interleave Drive frequency can also be adjusted, which may be useful if
acquiring amplitude data in LiftMode; see Chapter 13.

Notes

The cantilever drive circuit features a filter capacitor to limit the rate at which
the drive amplitude is changed between Main and Interleave scanning. If using
scan rates above a few hertz, it may be advantageous to remove or disable the
filter. For more information on how to disable the filter, contact Digital
Instruments technical support.

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Interleave Scanning and LiftMode

12.4.4. Amplitude Data Interpretation

When monitoring amplitude data in LiftMode, brighter regions correspond to
smaller amplitude, and darker regions to larger amplitude.

12.4.5. Cantilever Oscillation Amplitude

The selection of the oscillation amplitude in LiftMode depends on the quantity to
be measured. For force gradients which are small in magnitude but occur over relatively large distances (sometimes hundreds of nm, as with magnetic or electric
forces), the oscillation amplitude can be large, which for some applications may be
beneficial. The Lift scan height must be correspondingly large so that the tip does
not strike the surface. However, the lateral resolution of far field (MFM or EFM)
measurements decreases with distance from the surface. Typically, the resolution is
limited to a value (in nm) roughly equal to the Lift scan height; see Chapter 13.
Small amplitudes must be used to sense force gradients, such as Van der Waals
forces, which occur over short distances (typically a few nm). As much of the cantilever travel as possible should be within the range of the force gradient.

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MultiModeSPM Instruction Manual

Chapter 13

Magnetic Force (MFM) Imaging

13.1. Magnetic Force Imaging Overview

MFM imaging utilizes the Interleave and LiftMode procedures discussed in
Chapter 12; users are advised to read appropriate sections prior to attempting MFM
imaging. Best results will be obtained with Digital Instruments Extender Electronics Module. This hardware unit allows phase detection and frequency modulation for optimal MFM imaging. Instructions for software installation of the
Extender Electronics Module can be found at the end of this chapter; complete
instructions for hardware and software installation are included when you purchase
your Extender Electronics Module.
In MFM, a tapping cantilever equipped with a special tip is first scanned over the
surface of the sample to obtain topographic information. Using LiftMode as shown
in Figure 13.1, the tip is then raised just above the sample surface. The surface
topography is scanned while being monitored for the influence of magnetic forces.
These influences are measured using the principle of force gradient detection. In
the absence of magnetic forces, the cantilever has a resonant frequency f0. This frequency is shifted by an amount f proportional to vertical gradients in the magnetic
forces on the tip. The shifts in resonant frequency tend to be very small, typically in
the range 1-50 Hz for cantilevers having a resonant frequency f0 ~100 kHz. These
frequency shifts can be detected three ways: phase detection, which measures the
cantilevers phase of oscillation relative to the piezo drive; amplitude detection,
which tracks variations in oscillation amplitude; and frequency modulation, which
directly tracks shifts in resonant frequency. Phase detection and frequency modulation produce results that are generally superior to amplitude detection.

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4
3

5
2

1&2
3
4&5

Cantilever traces surface topography on first trace and retrace.

Cantilever ascends to Lift scan Height.
Lifted cantilever profiles topography while responding
to magnetic influences on second trace and retrace.
Figure 13.1. MFM LiftMode principles.

All standard Dimension-series SPMs and MultiModes are capable of MFM imaging using amplitude detection techniques. By adding an Extender Electronics
module (see Figure 13-2), either system may also be used for frequency modulation
or phase detection, giving improved results. Amplitude detection has largely been
superseded by frequency modulation and phase detection. A more extensive discussion of force gradient detection and MFM imaging is given in the reprint Magnetic
Force Microscopy: Recent Advances and Applications. Contact Digital Instruments
to obtain a copy.

Notes

In the instructions below, steps specific to phase and amplitude imaging are
described independently. Use the icons in the margin to locate steps specific to
either frequency modulation and phase detection, or amplitude detection.
.

Figure 13.2. Extender Electronics Module (required for MFM phase

detection and frequency modulation).

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Magnetic Force Imaging (MFM)

13.2. MFM Using Interleave Scanning and

LiftMode
This section provides instructions for using the LiftMode of Interleave scanning to
obtain MFM images. These guidelines will help in obtaining an MFM image of a
standard magnetic sample (metal-evaporated video tape). Standard tape samples are
provided with purchase of MFM probes, and can be obtained free of charge from
Digital Instruments. Other samples can also be used; however, you will not have the
benefit of comparing your results with the images shown here. Obtaining a good
image of the tape sample will familiarize you with Interleave and MFM techniques
and provide a check that the system is correctly tuned to image magnetic samples of
interest. Many of the principles discussed here also apply to Electric Force Microscopy (EFM), described in Chapter 14.
For MFM procedures, NanoProbe magnetic coated tips are required. Various
kinds of MFM probes are available for specific applications; contact Digital Instruments for more information. The remainder of this chapter assumes that the reader
is familiar with the operation of TappingMode to obtain topographical images of a
sample surface and has read the description of Interleave scanning in their manual.
LiftMode allows the imaging of relatively weak but long-range magnetic interactions while minimizing the influence of topography (Figure 13.1). Measurements
are taken in two passes across each scanline; each pass consists of one trace and one
retrace. In the first pass, topographical data is taken in TappingMode on one trace
and retrace. The tip is then raised to the lift scan height and a second trace and
retrace performed while maintaining a constant separation between the tip and local
surface topography. Magnetic interactions are detected during this second pass.
Using LiftMode, topographical features are virtually absent from the MFM image
(see Figure 13.7).
The procedure below gives suggested parameter values that should work well for
most applications. Further adjustment will, in some cases, improve the quality of
MFM scans, and some experimentation may be needed to optimize the imaging of
specific samples. See the suggestions at the end of this section.
As mentioned above, the NanoScope III uses force gradient detection for MFM
imaging. Within this general technique, there are three possible schemes, known as
frequency modulation, phase detection, and amplitude detection. All three are discussed here. Prior to 1994, amplitude detection had been the standard method for
magnetic force imaging on the NanoScope III. However, hardware that allows
phase detection and frequency modulation is now available for all TappingModecapable microscopes in the form of Digital Instruments Extender Electronics
Module. (Microscopes without the Extender addition cannot utilize phase detection; for more information, contact Digital Instruments.) Phase detection and fre-

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quency modulation detection are superior methods for magnetic force imaging,
offering greater ease of use, better signal-to-noise ratios, and reduced artifact content as compared to amplitude detection. If extensive MFM imaging is planned, the
Extender Electronics module is strongly recommended.

13.2.1. Procedure
1. Mount a NanoProbe magnetic probe on the scanner or tip holder. The tip should
be magnetized with a strong permanent magnet before installing the tip holder on
the AFM head. Tips are usually magnetized with the field aligned along the tip axis
(perpendicular to the sample surface). The MFM then senses force gradients due to
the perpendicular component of the sampless stray field. Tip magnetizers are provided with MFM probes purchased from Digital Instruments.
2. Set up the AFM as usual for TappingMode operation. In all Channel panels, the
Highpass and Lowpass filters should be Off. Set the Rounding parameter in the
Microscope / Calibrate / Scanner window to zero (0.00).
3. The procedure to tune the cantilever drive frequency and amplitude depends on
whether you are using phase detection or amplitude detection. Both cases rely on
automatic Cantilever tune just as when preparing for TappingMode; see Chapter 8
of the product instruction manual. MFM cantilevers have resonant frequencies
between 50 and 100 kHz. If using the AutoTune feature, these values can be used
as bounds for the frequency sweep. With the Extender option, two curves appear in
the Cantilever Tune box: the amplitude curve in white, and the phase curve in yellow (Fig. 229-3). Microscopes without the Extender Electronics Module display
only the amplitude curve.

Setting a Drive Frequency for Phase Detection

The Drive frequency should be set to the center of the cantilever resonance, as
shown in Figure 13.3. This will be done automatically if using AutoTune.

Phase
Detection

MFM / EFM

Figure 13.3. Cantilever Tune for phase detection and frequency modulation.

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To correctly track the cantilever phase, the Phase offset parameter must be
adjusted. This is automatically done in AutoTune; alternatively, Zero Phase can be
selected from the menu bar above the Cantilever Tune frequency sweep window.
The phase curve should appear as in Figure 13.3, decreasing with increasing frequency, and crossing the center line (corresponding to a 90 phase lag) at the peak
frequency. The phase curve then measures the phase lag between the drive voltage
and the cantilever response. Again, vertical gradients in the magnetic force cause a
shift f0 in the resonance frequency. In this case, resonance shifts give rise to phase
shifts which then give an image of the magnetic force gradients; see figure 13.4.

Notes
The Extender electronics give a measure of the phase lag of the cantilever oscillation relative to the piezo drive. This measurement is monotonic versus frequency as is the true phase lag in degrees. The Extender measurement; however,
has slightly different nonlinear characteristics vs. frequency. The measurement
technique allows optimal signal-to-noise ratios; however, absolute values of
phase data should be taken as approximate. Users requiring quantitative measures of force gradient are advised to use frequency modulation (See
Section 13.2.2). Proceed to Step #4 below.
.
180

Phase (deg)

F0

90

Drive Frequency

Figure 13.4. Shift in phase at fixed Drive frequency.

Amplitude
Detection

MFM / EFM

Setting a Drive Frequency for Amplitude Detection

Set the Drive frequency to the left side of the cantilever resonance curve, as
shown in Figure 13.5. This can be done by using the AutoTune feature to first
find the resonance peak, then using Offset under the Cantilever Tune menu
bar to manually move the drive frequency to the side of the resonance. For

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maximum sensitivity, set the Drive frequency to the steepest part of the resonance curve. As the tip oscillates above the sample, a gradient in the magnetic
force will shift the resonance frequency f0; (see Figure 13.6). Tracking the variations in oscillation amplitude while in LiftMode yields an image of the magnetic force gradients.
Proceed to Step #4 below.

Figure 13.5. Cantilever Tune for amplitude detection.

Amplitude

F0

Drive Frequency
Figure 13.6. Shift in amplitude at fixed drive frequency.
4. Adjust the Drive Amplitude so that the RMS voltage response of the photodetector is approximately 2 volts. (Somewhat larger values may be beneficial if using
amplitude detection.) This can be done with Auto Tune by selecting an appropriate
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Target Amplitude (in this case, 2V) before tuning, or by exiting Cantilever Tune
and manually adjusting the Drive Amplitude parameter under Feedback Controls.
Quit Cantilever Tune and return to Image Mode. Under Interleave Controls set
the Lift start height to 0 nm, and Lift scan height to 100 nm. (The lift height can
be optimized later.) Set the remaining Interleave parameters (Setpoint, Drive
Amplitude, Drive frequency, and gains) to the Main Controls values. This can be
done by setting the flags left of the Interleave Control column to off (grayed
bullets).
5. Under Scan Controls, set the Scan size to 5 m and Scan rate to 12 Hz. For
the left image, set the Z range to 75 nm and the Line direction to Retrace. Engage
the AFM and make the necessary adjustments to obtain a good topographical image
while displaying height data. Use the maximum possible Setpoint to ensure that the
tip is contacting the surface only lightly. The image should be similar to the topographic image shown on the left of Figure 13.7. The surface is fairly flat with lubrication nodules of various sizes. A good image of the nodules provides a check that
the tip is sharp.

Figure 13.7. Topographic (left) and magnetic force gradient image (right) of
metal evaporated tape at 100 nm Lift scan height.
6. The MFM data can be shown on Channel 2; however, the parameter settings are
different depending on whether Phase Detection or Amplitude Detection is being
used

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Phase
Detection

Part IV: Interleaved Imaging Techniques

Phase Detection
Set the Channel 2 image Data type to Phase, Z range to 3 degrees, and Line
direction to Retrace.

MFM / EFM

Notes
It is important that the Scan direction be set to Retrace for both the main and
interleave scans. If instead it is set instead to Trace, a band may appear along
the left side of the images due to the time taken for the tip to move between the
surface and the lift scan height.
Amplitude
Detection

MFM / EFM

Amplitude Detection
Set the Channel 2 image Data type to Amplitude, Z range to 1 nm, and Line
direction to Retrace.
7. Change Interleave mode to Enable to invoke LiftMode. Set the Channel 2 Scan
line to Interleave to display the interleaved data. (This can only be done after
Interleave mode is Enabled.) A magnetic force gradient image similar to that
shown on the right of Figure 13.7 should appear as the Channel 2 image. The alternating dark and light stripes represent the recorded magnetic information, and signify a varying resonant frequency and hence magnetic force gradient on the tip. As
usual, keep the Setpoint as large as possible while consistent with a good image.
Wider scans (> 25 m) will reveal separate tracks in which the magnetic stripes are
at different angles.

13.2.2. Frequency modulation.

With the Extender Electronics Module, it may be desirable to use frequency modulation. This activates a feedback loop which modulates the Drive Frequency to
keep the cantilevers phase lag at 90 degrees relative to the drive, corresponding to
resonance. The frequency Data Type displays the resulting shift in Drive Frequency in Hz, and gives the most direct, quantitative image of force gradients.
To enable frequency modulation, follow the procedure above for obtaining an MFM
image with phase detection, but switch the Channel 2 image Data type to Frequency. Try a Z range (frequency shift) of approximately 10 Hz. Select Other
Controls, then adjust the frequency modulation gains. Setting both frequency modulation Integral gain and Proportional gain to 100 is a good starting point. As
with the topography gains, the scan can be optimized by increasing the gains to
maximize feedback response, but not so high that oscillation sets in. With 225 m
MFM cantilevers, gains are usually in the range of 100250.

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13.3. Troubleshooting Suggestions

13.3.1. MFM image verification.
The procedure described above should produce a good magnetic force gradient
image of the videotape sample. If there is a problem, check that the Interleave
Mode is set to Lift, that Interleave is Enabled and that the Scan Line is set to
Interleave. Check also that the Interleave values of Drive Amplitude and Drive
Frequency are initially set equal to the main Scan Controls values.

13.3.2. Saturation in amplitude detection

If using amplitude detection, the magnetic force image can saturate (appear completely featureless) if the Interleave Drive Amplitude is significantly different
than the Drive Amplitude in the main scan. Adjust the Interleave Setpoint to
restore the image. (Note that the Interleave Setpoint has no physical effect in LiftMode since there is no surface feedback during the lift pass.

13.3.3. Optical interference.

Amplitude

Detection
When using Amplitude Detection, optical interference may sometimes appear in
the Lift (magnetic force gradient) image when imaging highly reflective samples.
Optical interference appears as evenly spaced, sometimes wavy lines with ~12 m
MFM / EFM
spacing superimposed on the lift image. This occurs when ambient laser light (i.e.,
light passing around or through the cantilever, then reflecting off the sample) interferes with laser light reflecting from the cantilever. Interference can be alleviated by
moving the beam spot up the cantilever away from the tip; about one-third of the
cantilever length works well. The adjustment can be refined by carefully moving
the beam spot laterally a small distance on the cantilever while scanning until interference fringes are minimized. Be careful not to move the beam off the cantilever or
feedback may be lost.

Notes

Optical interference is essentially eliminated by using phase detection or

frequency modulation.)

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13.4. Advanced Topics

13.4.1. Lift scan height and magnetic imaging resolution.
The most important parameter affecting imaging resolution is the Lift scan height.
The range of 10200 nm is most useful. In general, MFM resolution is roughly
equal to the lift height: smaller Lift Scan heights give better resolution; conversely,
magnetic features smaller than the Lift Scan height may not be resolved. The tip
also experiences stronger fields close to the surface, giving improved signal-tonoise ratios.
For example, the image of metal-evaporated tape in Figure 13.7 has a resolution
limited by the 100 nm Lift Scan height. To improve the resolution, try reducing the
Lift scan height to ~ 25 nm. Ensure that the tip does not strike the surface on the
low point of its swing in the Lift image. Tip strikes appear as black or white spots,
or even noisy, high-contrast streaks crossing the image. If the tip begins to strike the
surface, reduce the Interleave Drive Amplitude. (In general, MFM tips are not
damaged by intermittent tip strikes, except in extreme cases of very large amplitude
and small lift heights.) An example of an image of the metal-evaporated tape taken
with a Lift scan height of 30 nm is shown in Figure 13.8. Note the fine magnetic
structure that is not visible in Figure 13.7. When imaging a sample for the first time,
begin with moderate Lift scan heights (50 nm or greater), then adjust downward.
On relatively smooth samples (e.g., hard disks), lift heights down to 0 nm can be
used, as long as the drive amplitude is adjusted accordingly. (Lift scan heights of 0
nm still correspond to a non-zero mean tip-sample distance. See the section on Setpoint below.) It is usually not beneficial to use Lift scan heights much smaller than
the surface roughness. Users are encouraged to experiment for the best images on
their samples.
The ultimate resolution of MFM with the NanoScope III is near 20 nm. Resolution
is affected by properties of the tip, including mechanical sharpness and magnetic

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structure. When in good condition, NanoProbe magnetically coated tips routinely

give 50 nm resolution, and many achieve 30 nm or better.

Figure 13.8. High-resolution magnetic force gradient image of

metal evaporated tape at 30 nm Lift scan height.

13.4.2. Fine Tuning Interleave Controls

Certain scanning parameters found under Interleave Controls can be set to values
in the Interleave (Lift) scan that differ from the values in the main scan. These
parameters are enabled by clicking on the circular flag to the immediate left of the
desired Interleave control, toggling its state from off (gray bullet) to on (green
bullet). When the flag is set to off, the main scan control parameter setting takes
precedence. When the flag is set to on, the displayed Interleave scan value is
active, overriding the main scan value.
Drive amplitude
For MFM, of particular use is the Interleave Drive Amplitude. This parameter can
affect a magnetic force image in a variety of ways.

Increasing the Drive Amplitude can improve the signal-to-noise ratio when
using phase detection or frequency modulation. This is because intrinsic, lowlevel noise interferes less when measuring the phase of a larger cantilever
oscillation amplitude and hence stronger photodetector output. As an

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illustration, try setting the Interleave Drive Amplitude to 0; the resulting phase
image will be pure noise because measuring the phase of a non-oscillating
cantilever is meaningless.
In LiftMode, the Interleave Drive Amplitude can often be set to a value larger
than in the main scan, thus giving optimal signal-to-noise. In some cases this is
beneficial as long as the Drive Amplitude is not increased to the extent that the
tip strikes the surface on the low point of its swing. The signatures of tip-sample
contact are white and black spots in the image, or, in extreme cases, noisy, highcontrast streaks across the whole image. It is usually safe to increase the Drive
Amplitude until the first signs of tip strike are noticed, then reduce the amplitude slightly.
CAUTION: Before enabling the Interleave Drive Amplitude, check that its value
is not much larger than the main Drive Amplitude value to prevent possible damage to the tip.
ATTENTION: Lors dun travail en mode intercal (Interleave Mode), vrifier que
la valeur de tension applique loscillateur pizo-lectrique est infrieure celle
applique loscillateur en mode imagerie (Main Drive Amplitude). Le non
respect de cette procdure peut entraner la destruction de la pointe.
WARNHINWEIS: Bevor Sie im Interleave-Mode die Interleave Drive-Amplitude einschalten, vergewissern Sie sich bitte, da der dort eingetragene Wert nicht
wesentlich grer ist, als der Wert der Main Drive-Amplitude, um evtl. Beschdigungen der Spitze vorzubeugen.
Amplitude
Detection

MFM / EFM

When using amplitude detection, variations in Drive Amplitude affect

sensitivity and image contrast as well as signal-to-noise ratio. This is because
changes in the oscillation amplitude change the slope of the amplitude vs.
frequency curve, and hence the effective sensitivity; see Figure 13.6. With
phase detection and frequency modulation, changes in amplitude produce no
change in contrast, and results are thus more reproducible than with amplitude
detection.

Notes

On some microscope models, there is a lowpass filter in the scanning electronics

that prevents fast switching of the Drive Amplitude between main and
Interleave scanning. This can interfere with very fast rates (> a few Hz).
Setpoint
For the most reproducible results, it is best to use a consistent setpoint. In LiftMode, the total tip-sample distance htot is the sum of the average tip-sample distance in TappingMode hT, and the lift scan height hlift (see Figure 13.9). In
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TappingMode, the average tip-sample distance hT is equal to the oscillation amplitude, which is determined by the setpoint. Large variations in setpoint can thus
change the total tip-sample distance in Liftmode, sometimes with visible results in
the magnetic image. For this reason, reproducible results are most easily obtained
by using consistent setpoints. Note that a lift scan height of 0 nm still gives a mean
tip-sample distance of hT in LiftMode.

Lift pass
TappingMode pass
htot =
hT + hlift

hlift

hT

Figure 13.9. Tip heights and oscillation amplitudes in TappingMode and

LiftMode.
The relationship between setpoint voltage and oscillation amplitude is known as the
sensitivity. Its value can be determined with Force Calibration; see Chapter 11 in
the product instruction manual. For 225 m MFM cantilevers, the sensitivity is typically in the range 15-20 nm/V. A 1V Setpoint typically corresponds to hT ~15-20
nm.

13.5. Installation of Extender Electronics Module

In the Spring of 1994, Digital Instruments began making available its Extender
Electronics Module (sometimes referred to as phase box or phase extender) for
customers wanting phase detection and frequency modulation MFM. Hardware
changes, different for each system type, are required to retrofit Dimension Series
systems or MultiMode systems originally shipped without the Extender Electronics
module.
For MultiMode systems, the Extender is installed using a 37-to-37 pin ribbon cable
between the NanoScope III or IIIA SPM controller and the Extender Electronics
Module, and a 37-to-25 pin ribbon cable from the Extender to the microscope. The
hardware change consists of replacing a circuit board in the base of the microscope
(this may be done by either the customer or a factory representative). Detailed
installation instructions are provided with the new hardware when shipped. For
more information, contact Digital Instruments.
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13.5.1. Setting the Extender Electronics for Dimension or MultiMode

The Extender Electronics box is equipped with a slider switch for switching internal electronics between Dimension-series and MultiMode SPM signals. This
switch may be accessed through a hole on the underside of the box. In the drawing
below, the switch is set to MultiMode.

Dimension

MultiMode
For MultiMode SPMs, it should always be set to MultiMode. Use a pencil to
access the switch through the hole.
WARNING: Do not insert a conducting object (e.g., screwdriver) into the Phase
Extender box while it is engergized.
ATTENTION: Ne pas insrer d objet conducteur (par exemple: un tournevis)
dans le botier dextension de phase (Phase Extender Box) quand celui-ci est sous
tension.
WARNUNG: Stecken Sie keine leitfhigen Teile (zum Beispiel Schraubenzieher)
in die Phase Extender Box, whrend diese eingeschaltet ist.

13.5.2. Microscope parameter files.

There are two parameter (par) file contexts that are used with the Extender Box:
Extended AFM and Extended STM. The former of these two contexts is used for
the following operational modes: contact AFM, TappingMode AFM, LFM, MFM,
force modulation, electric field measurement and others. The latter context is for
use only with STM.
For each scanner intended to be used with the Extender, there must be a PAR file
for the context required. For example, if there are three scanners, all intended for
both STM and AFM use, a total of six PAR files are required.

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Notes

Due to the many Digital Instruments microscope systems available, the variety
of scanners, when the system was purchased, and the systems history of
software updates, not all systems will have PAR files with the same name or
naming scheme. You can determine the exact name of the PAR file to be
modified by using the DOS EDIT file editor to list the contents of the file /
SPM/SYSTEM.PAR. The name of the most recent PAR file in use will be
on the line that starts with the words \Microscope file:.
CAUTION: When closing the System.par file after viewing it, if you are
asked to SAVE the file or to SAVE CHANGES, be sure to say No.
ATTENTION: A la fermeture du fichier System.par, lorsque lordinateur
demande SAUVEGARDER (SAVE) ou SAUVEGARDER LES CHANGEMENTS (SAVE CHANGES), rpondre toujours NON.
WARNHINWEIS: Falls Sie sich mit einem Editor die Datei system.par
anschauen und beim Verlassen des Editors gefragt werden, ob Sie die Datei speichern (SAVE) bzw. die nderungen speichern wollen (SAVE CHANGES), antworten Sie bitte mit Nein (No).
To modify the PAR files on a MultiMode or Dimension system, locate the proper
PAR file in the /SPM/EQUIP directory on your computer. Use a text editor to
modify the file. The text must be saved as plain ASCII (standard DOS text). DI recommends using the DOS EDIT file editor. (Microsoft Word or other similar desktop-editors normally save files with embedded formatting commands causing the
par files to be unreadable by the NanoScope software.) Using the EDIT program,
modify the file to include a new line at the bottom of the file. For example:

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If the line

\Is FM: No
is present in the file, then change the line to read:

\Is FM: Yes

If the line

\Is FM: No
is not present, add the line:

\Is FM: Yes

Then locate the line:

\In Polarity: Reverse

and change it to read:

\In Polarity: Forward

Then locate the line:

\In Polarity: AUX D: Reverse

Change it to read:

\In Polarity AUX D: Forward

Repeat the above procedure for each scanner (i.e. PAR file) in use. After the cables
are connected, power up the NanoScope controller and start the microscope control
program.

13.5.3. Important points.

1. Extender-compatible microscope electronics are required to permit operation of
the phase detection extender option. Standard electronics on these microscopes
require hardware upgrades. Consult your Digital Instruments sales representative
for details.

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Magnetic Force Imaging (MFM)

2. Turn off the power to the NanoScope controller whenever connecting or disconnecting the Extender.
3. In LiftMode, the best performance is obtained if the RMS amplitude is kept
below 7.0 volts, the limit of the RMS outputs linear operation.

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THIS IS A BLANK PAGE.

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Chapter 14

Electric Force (EFM) Imaging

Chapter Table of Contents

14.1
14.2
14.3

14.4

14.5
14.6
14.7

Electric Force Microscopy Overview 2

14.1.1 Electric Field Gradient Imaging Overview 4
14.1.2 Surface Potential Imaging Overview 4
Electric Field Gradient DetectionTheory 5
Electric Field Gradient DetectionPreparation 7
14.3.1 Jumper Configurations for Systems Without the Extender
Electronics Module 9
A: Voltage Applied to the Tip 10
B: Voltage Applied to the Sample 11
C: External Voltage Source Applied to the Tip 12
D: External Voltage Source Applied to the Sample 13
14.3.2 Jumper Configurations For Microscopes With the Extender
Electronics Module 14
E: Voltage Applied to the Tip 15
F: Voltage Applied to the Sample 16
G: External Voltage Source Applied to the Tip 17
H: External Voltage Source Applied to the Sample 18
Electric Field Gradient DetectionProcedures 19
14.4.1 Phase Detection 20
14.4.2 Amplitude Detection 23
With Extender Electronics Module 23
Without Extender Electronics Module 23
Surface Potential DetectionTheory 25
Surface Potential DetectionPreparation 26
14.6.1 Applying Voltage to the Sample Directly 27
14.6.2 Applying Voltage to the Sample Through Piezo Cap 28
Surface Potential ImagingProcedure 29
14.7.1 Troubleshooting the Surface Potential Feedback Loop 32

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14.1. Electric Force Microscopy Overview

This chapter describes how to perform electric force microscopy (EFM) imaging on
a MultiMode SPM system. Similar to magnetic force microscopy (MFM)and
sharing many of its procedural techniquesthis mode utilizes the Interleave and
LiftMode procedures discussed in previous chapters. Please read those chapters
prior to attempting electric force measurements.
All standard MultiMode SPMs are capable of EFM imaging using amplitude detection techniques. By adding an Extender electronics module (see Figure 14.2), the
MultiMode SPM may also be used for frequency modulation or phase detection,
giving improved results. Amplitude detection has largely been superseded by frequency modulation and phase detection. This hardware unit is required for surface
potential imaging, and is strongly recommended for electric field gradient imaging.
Two types of electric force microscopy are available using the MultiMode SPM
system: 1) electric field gradient imaging; and, 2) surface potential imaging.
Each of the electric field measurement techniques are based on a two-pass LiftMode measurement. LiftMode allows the imaging of relatively weak but longrange magnetic and electrostatic interactions while minimizing the influence of
topography (see Figure 14.1). Measurements are taken in two passes (each consisting of one trace and one retrace) across each scanline. First, topographical data is
taken in TappingMode on one trace and retrace. The tip is then raised to the final
scan height, and a second trace and retrace performed while maintaining a constant
separation between the tip and local surface topography. Both methods of electric
force measurement are explained in this chapter.

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Electric Force (EFM) Imaging

3
Force Gradient Scope Data
(Interleave scan)

1
1521

Electric Fields
1
2
3

Topographic Scope Data

(Main scan)

Cantilever measures surface topography on first (main) scan.

Cantilever ascends to lift scan height.
Cantilever follows stored surface topography at the lift height above sample
while responding to electric influences on second (interleave) scan.
Figure 14.1. EFM LiftMode principles.

Figure 14.2. Extender Electronics Modulerequired for frequency

phase detection MFM and EFM.

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Figure 14.3. EFM probe tip holder, top and bottom view (left to right).

14.1.1. Electric field gradient imaging overview.

Electric field gradient imaging is a technique which measures variations in the electric field gradient above a sample. The sample may be conducting, nonconducting,
or mixed. Since the electric field gradient is also shaped by the surface topography
(e.g. sharp points on the surface concentrate the field gradient), large differences in
topography can make it difficult to distinguish electric field variations. In general,
the best samples for electric field gradient imaging are samples that have applied
voltages of roughly 1 volt or more, samples with fairly smooth topography, or samples with trapped charge. Samples with insulating layers (passivation) on top of
conducting regions may also be good candidates for electric field gradient imaging.

14.1.2. Surface Potential Imaging Overview

Surface potential imaging measures the effective surface voltage of the sample by
adjusting the voltage on the tip so that it feels a minimum electric force from the
sample. (In this state, the voltage on the tip and sample is the same.) Samples for
surface potential measurements should have an equivalent surface voltage of less
than 10 volts, and operation is easiest for voltage ranges of 5 volts. The noise
level of this technique can be as low as a few mV. Samples may consist of conducting and nonconducting regions, but the conducting regions should not be passivated. Samples with regions of different materials will also show contrast due to
contact potential differences. Semi-quantitative voltage measurements can be made
on samples if the system is carefully calibrated on a sample at a known voltage.
This method requires the Extender Electronics Module and version 3.1 or later of
the NanoScope software.

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14.2. Electric Field Gradient DetectionTheory

Amplitude

Electric field gradient imaging is analogous to standard MFM, except that gradients
being sensed are due to electrostatic forces. In this method, the cantilever is
vibrated by a small piezoelectric element near its resonant frequency. The cantilevers resonant frequency changes in response to any additional force gradient.
Attractive forces make the cantilever effectively softer, reducing the cantilever
resonant frequency. Conversely, repulsive forces make the cantilever effectively
stiffer, increasing the resonant frequency. A comparison of these force additives is
shown in Figure 14.3.

F0

Amplitude

Frequency
Attractive gradient equivalent to additional spring in tension attached
to tip, reducing the cantilever resonance frequency.
F0

Frequency
Repulsive gradient equivalent to additional spring in compression attached
to tip, increasing the cantilever resonance frequency.
Figure 14.4. Comparison of attractive and repulsive forces
to action of a taut spring attached to the tip.
Changes in cantilever resonant frequency can be detected in one of the following
ways:

Phase detectionwith Extender Electronics Module only.

Frequency modulation (FM)with Extender Electronics Module only.
Amplitude detectionnot recommended due to artifacts.
All of the above methods rely on the change in resonant frequency of the cantilever
due to vertical force gradients from the sample. Figure 14.4 shows a diagram of
how the Extender Electronics module provides the signal enhancement and feedback allowing gradient detection. The best candidates for electric field gradient
imaging are samples that have large contrasts in the electric force gradient due to

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material differences or regions at substantially different potentials (voltage differences of 1.0 or more). For other samples having rough surface topography or small
voltage variations, this technique may be undesirable because topographic features
will appear in the LiftMode image.

Cantilever Deflection Signal

Photodiode signal
Conditioning

RMS Detector
Phase Detector

Laser
Beam

Amplitude Signal

Phase Signal

Signals to
NanoScope

Servo Controller

Reference
Signal

(Feedback loop
adjusts oscillation
frequency until
phase lag is zero)

Frequency
Frequency Signal

Control lines

Photodetector

High Resolution
Oscillator
Tapping
Piezo

Oscillator Signal

Extender Electronics Module

Sample

Figure 14.5. Diagram of Extender Electronics Module in phase and

frequency measurement mode.
Topographic features appear in the LiftMode image because local force gradients
are heavily influenced by surface structure. That is, sharp features on sample surfaces concentrate the local force gradient. This happens on all roughness scales, so
the local force gradient will also vary in much the same way as does the surface
topography. Thus, electric field LiftMode images measured by amplitude, phase or
frequency detection often show contrast that is very similar to the surface topography. Samples with rough surface topography or with smaller potential variations are
more successfully imaged by the surface potential measurement method described
below.

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Notes
In most cases, it is necessary to apply a voltage across the tip or sample to
achieve a high-quality image. Various methods for applying voltages to the tip
and sample are included in the sections that follow. Samples with permanent
electric fields may not require the application of voltage.

14.3. Electric Field Gradient Detection

Preparation
This section explains how to conduct electric field gradient imaging by applying a
voltage to the tip or sample to generate electric fields. If the sample being imaged
has a permanent electric field which does not require the external application of
voltage, the steps below are not required and you can proceed to Section 14.4.
Before attempting to reconfigure the jumpers, carefully read the following Jumper
Configuration sections.
When it is necessary to apply voltage to the tip or sample, minor changes must be
made to the jumpers in the microscopes baseplate and the toggle switches on the
Extender Electronics Module (if equipped). Original jumper configurations and
jumper changes are dependent on the microscope being used and the measurements
desired. Section 14.3.1 provides jumper configuration instructions for basic microscope models operating without the Extender Electronics Module (See: Jumper
Configuration Sections A, B, C, D.). Section 14.3.2 provides jumper configuration
instructions for basic microscope models operating with the Extender Electronics
Module (See: Jumper Configuration Sections E, F, G, H.)
The location and orientation of the jumpers in the baseplate of the MultiMode is
shown below in Figure 14.5. To change the jumpers, it should not be necessary to
remove the baseplate; they can easily be changed through the rectangular opening
in the bottom of the baseplate using a pair of non-conducting tweezers. For non-

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EFM applications and surface potential operation, jumpers are usually left in their
original positions or returned to their original positions.
Jumpers, inside baseplate
window

To
er
ntroll
pe Co tronics
o
c
S
o
c
Nan
r Ele
tende
or Ex Module

Figure 14.6. Diagram of MultiMode baseplate showing

location and orientation of jumpers.
1. Carefully examine the following figures and identify which jumper configuration, if any, is appropriate for your application.
2. Power down the NanoScope III controller and turn off all peripherals. Unplug the
NanoScope III power cable from the microscopes controller electronics box.
3.Ensure the tip is not engaged on the sample. Disconnect and remove the microscope head and the scanner.
4. Carefully tilt the MultiMode so that the baseplate is oriented as shown in
Figure 14.5. Locate header and jumpers. As shipped from the factory, jumpers on
systems without the Extender Electronics Module should appear as shown in
Figure 14.6, whereas jumper systems with the Extender Electronics option should
appear as in Figure 14.11.If the microscope is to be used for EFM imaging in cases
where voltage is applied to the tip or sample, it is necessary to change the jumpers.
5. Depending upon whether voltage is to be applied to the tip or sample, and the
amount of voltage to be used, reconfigure jumpers on the baseplate header using the
jumper configuration as shown in the appropriate sections below.
6. After the jumpers are correctly configured, apply power to the microscope and all
peripherals. Boot the computer and start the NanoScope software.
7. If the jumpers are configured to use an external voltage source, click on the
Microscope / Calibrate / Detector option to display the Detectors Parameters
window. Switch the Allow in attenuation field to Allow.
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8. Imaging can now be accomplished using the procedures in Section 14.4.

14.3.1. Jumper configurations for systems without the Extender

Electronics Module
As shipped from the factory, the jumper configuration on a MultiMode SPM without the Extender Electronics Module should appear as shown in Figure 14.6 below.
Ground
Piezo Cap
Analog 2
Gain Select
Analog 2
To AFM Tip
Auxiliary D (to NanoScope III controller)
STM
Indicates jumpers

Figure 14.7. Normal jumper configuration for systems without the Extender
Electronics Module as shipped from factory.

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A: Field Gradient ImagingVoltage Applied to the Tip

The jumper configuration in Figure 14.7 connects the Analog 2 signal from the
NanoScope III controller ( 12 VDC range) to the tip.

Notes
In all configurations which apply voltage to the tip, an E-field cantilever holder
is required. Contact Digital Instruments for more information.
Enabling the Analog 2 Voltage Line:
The Analog 2 voltage line is normally used by the NanoScope to control the
attenuation (1x or 8x) of the main feedback signal. This application of EFM imaging uses the Analog 2 signal for EFM data. Therefore, input attenuation must be
disabled for the duration of the EFM experiments. To do this, click on the Microscope / Calibrate / Detector option to display the Detectors Parameters window.
Switch the Allow in attenuation field to Disallow. Return to the main Feedback
Controls panel; the Analog 2 field should now be enabled. This signifies that voltage is now being supplied via the Analog 2 pin located on the baseplate header.
Remember to restore (Allow in attenuation) upon completion of EFM imaging.
Ground

Tip
Piezo Cap
Analog 2

Analog 2

Sample
Gain Select
Analog 2
To AFM Tip
Auxiliary D (to NanoScope III controller)
STM
Indicates jumpers

Figure 14.8. Jumper configuration for application of voltage to tip

(for systems without the Extender Electronics Module).

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B: Field Gradient ImagingVoltage Applied to the Sample

The jumper configuration in Figure 14.8 connects the Analog 2 signal from the
NanoScope III controller ( 12 VDC range) to the sample chuck.
Enabling the Analog 2 Voltage Line
The Analog 2 voltage line is normally used by the NanoScope to control the attenuation (1x or 8x) of the main feedback signal. This application of EFM imaging uses
the Analog 2 signal for EFM data. Therefore, input attenuation must be disabled for
the duration of the EFM experiments. To do this, click on the Microscope / Calibrate / Detector option to display the Detectors Parameters window. Switch the
Allow in attenuation field to Disallow. Return to the main Feedback Controls
panel; the Analog 2 field should now be enabled. This signifies that voltage is now
being supplied via the Analog 2 pin located on the MultiMode baseplate header.
Remember to restore (Allow in attenuation) upon completion of EFM imaging.
Ground

Tip

Piezo Cap
Analog 2

Sample
Analog 2

Gain Select
Analog 2
To AFM Tip
Auxiliary D (to NanoScope III controller)
STM
Indicates jumpers

Figure 14.9. Jumper configuration for application of voltage to sample

(for systems without the Extender Electronics Module).

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C: Field Gradient ImagingExternal Voltage Source Applied to the

Tip
In some cases, it may be advantageous to use voltages greater than 12 VDC, or to
use a pulsed power supply. If an external source of voltage is to be applied to the
tip, configure jumpers as shown in Figure 14.9.

Notes

In all configurations which apply voltage to the tip, an E-field cantilever holder
is required. Contact Digital Instruments for more information.
Ground

Tip

Piezo Cap
Analog 2

Sample

Gain Select
Unused
To AFM Tip
Auxiliary D (to NanoScope III controller)
STM

>10 M

(+)

(-)

External Voltage
Source

Indicates jumpers

Figure 14.10. Jumper configuration for applying external voltage to tip

(for systems without the Extender Electronics Module).
A current-limiting resistor (e.g., 10100 M) should be placed in series with the
external voltage supply as shown to protect the tip and sample from damage. Current-limited power supplies may also be used. Voltage leads should be connected to
pins on the header using soldered, push-on connectors. Do not solder leads directly
to the header pins, as the heat may cause damage and/or make jumpering the pins
difficult. The connection to ground can be made to the AFM chassis or externally.

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D: Field Gradient ImagingExternal Voltage Source Applied to the

Sample
In some cases, it may be advantageous to use voltages greater than 12 VDC, or to
use a pulsed power supply. If an external source of voltage is to be applied to the
sample, configure jumpers as shown in Figure 14.10.
()

Ground

External Voltage
Source

Piezo Cap
Analog 2
Gain Select

(+)
>10 M

Tip

Unused
To AFM Tip

Sample
Auxiliary D

+
>10 M

STM

Indicates jumpers

Figure 14.11. Jumper configuration for applying external voltage to sample

(for systems without the Extender Electronics Module).
A current-limiting resistor (e.g., 10100 M) should be placed in series with the
external voltage supply as shown to protect the tip and sample from damage. Current-limited power supplies may also be used. Voltage leads should be connected to
pins on the header using soldered, push-on connectors. Do not solder leads directly
to the header pins, as the heat may cause damage and/or make jumpering the pins
difficult.

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14.3.2. Jumper Configurations For Microscopes With the Extender

Electronics Module
REMINDER: Power down the microscope and turn off all peripherals. Unplug the
NanoScope III control and power cables from the system before attempting to
adjust jumper configurations.
As shipped from the factory, systems with the Extender Electronics option, should
have an original baseplate jumper configuration as shown in Figure 14.11.
Ground
Piezo Cap
Analog 2
Unused
Analog 2
To AFM Tip
Auxiliary D (to NanoScope III controller)
STM
Indicates jumpers

Figure 14.12. Normal jumper configuration as shipped from factory for

MultiMode SPM with Extender Electronics Module installed.

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Electric Force (EFM) Imaging

E: Field Gradient ImagingVoltage Applied to the Tip

Notice that the jumper configuration in Figure 14.12 connects the Analog 2 signal
from the NanoScope III controller ( 12 VDC range) to the tip, and is exactly the
same as the jumper configuration shown in Figure 14.11, the standard configuration
as shipped from the factory.

Notes

In all configurations which apply voltage to the tip, an E-field cantilever holder
is required. Contact Digital Instruments for more information.
Enabling the Analog 2 Voltage Line
The Analog 2 voltage line is normally used by the NanoScope to control the
attenuation (1x or 8x) of the main feedback signal. This application of EFM imaging uses the Analog 2 signal for EFM data. Therefore, input attenuation must be
disabled for the duration of the EFM experiments. To do this, click on the Microscope / Calibrate / Detector option to display the Detectors Parameters window.
Switch the Allow in attenuation field to Disallow. Return to the main Feedback
Controls panel; the Analog 2 field should now be enabled. This signifies that voltage is now being supplied via the Analog 2 pin located on the MultiMode baseplate header.
Remember to restore (Allow in attenuation) upon completion of EFM imaging.
Ground

Tip
Piezo Cap
Analog 2

Analog 2

Sample
Unused
Analog 2
To AFM Tip
Auxiliary D (to NanoScope III controller)
STM

Indicates jumpers

Figure 14.13. Jumper configuration for application of voltage to tip

standard configuration of systems with the Extender Electronics
Module as shipped from factory.

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F: Field Gradient ImagingVoltage Applied to the Sample

The jumper configuration in Figure 14.13 connects the Analog 2 signal from the
NanoScope III controller ( 12 VDC range) to the sample.
Enabling the Analog 2 Voltage Line
The Analog 2 voltage line is normally used by the NanoScope to control the
attenuation (1x or 8x) of the main feedback signal. This application of EFM imaging uses the Analog 2 signal for EFM data. Therefore, input attenuation must be
disabled for the duration of the EFM experiments. To do this, click on the Microscope / Calibrate / Detector option to display the Detectors Parameters window.
Switch the Allow in attenuation field to Disallow. Return to the main Feedback
Controls panel; the Analog 2 field should now be enabled. This signifies that voltage is now being supplied via the Analog 2 pin located on the baseplate header.
Remember to restore (Allow in attenuation) upon completion of EFM imaging.
Ground
Piezo Cap

Tip

Analog 2
Unused

Sample
Analog 2

Analog 2
To AFM Tip
Auxiliary D (to NanoScope III controller)
STM
Indicates jumpers

Figure 14.14. Jumper configuration for application of voltage to sample

(for systems with the Extender Electronics Module).

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G: Field Gradient ImagingExternal Voltage Source Applied to the

Tip
In some cases, it may be advantageous to use voltages greater than 12 VDC, or to
use a pulsed power supply. If an external source of voltage is to be applied to the
tip, configure jumpers as shown in Figure 14.14.

Notes

In all configurations which apply voltage to the tip, an E-field cantilever holder
is required. Contact Digital Instruments for more information.
Ground

Tip
Piezo Cap

Analog 2

Sample
Unused

Unused
To AFM Tip
Auxiliary D (to NanoScope III controller)
STM

>10 M

(+)

(-)

External Voltage
Source

Indicates jumpers

Figure 14.15. Jumper configuration for applying external voltage to tip

(for systems with the Extender Electronics Module).
A current-limiting resistor (e.g., 10100 M) should be placed in series with the
external voltage supply as shown to protect the tip and sample from damage. Current-limited power supplies may also be used. Voltage leads should be connected to
pins on the header using soldered, push-on connectors. Do not solder leads directly
to the header pins, as the heat may cause damage and/or make jumpering the pins
difficult.

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H: Field Gradient ImagingExternal Voltage Source Applied to the

Sample
In some cases, it may be advantageous to utilize voltages greater than 12 VDC, or
to utilize a pulsed power supply. If an external source of voltage is to be applied to
the sample, configure jumpers as shown in Figure 14.15.
()

Ground

External Voltage
Source

(+)

Piezo Cap

>10 M
Analog 2
Unused

Tip
Unused
To AFM Tip
Auxiliary D

Sample

+
>10 M

STM

Indicates jumpers

Figure 14.16. Jumper configuration for applying external voltage to sample

(for systems with the Extender Electronics Module).
A current-limiting resistor (e.g., 10-100 M) should be placed in series with the
external voltage supply as shown to protect the tip and sample from damage. Current-limited power supplies may also be used. Voltage leads should be connected to
pins on the header using soldered, push-on connectors. Do not solder leads directly
to the header pins, as the heat may cause damage and/or make jumpering the pins
difficult.

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Electric Force (EFM) Imaging

14.4. Electric Field Gradient Detection

Procedures

Notes

Amplitude detection is the only procedure described here that can be done
without the Extender Electronics Module; however, this method is no longer
recommended (see Section 14.4.2).
1. Locate the two toggle switches on the backside of the Extender Electronics box
(Figure 14.16), then verify that they are toggled as shown in Table 14.1.

Mode

Tip or Sample
Voltage

FM/Phase

Gnd/Surface Potential

Surface Potential
To
Mi
cro
s

To

Analog 2

cope

S
Nano

co

pe

Figure 14.17. Toggle switches on back of Extender Electronics Module.

Mode
FM/Phase
TappingMode
Contact AFM
MFM

Tip or Sample Voltage

Surface
Potential

Apply voltage to
tip or sample (Use
for electric field
gradient imaging;
tunneling AFM)

Analog 2

Surface Potential

GND/Surface
Potential

Table 1.1. Extender Electronics Module toggle switch settings.

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Notes

The toggle switch combination of Surface Potential = ON and

Analog2 = ON is not recommended and can produce erratic, undefined results.
2. Electrically connect the sample by mounting it to a standard sample disk or stage
using conducting epoxy or silver paint. Ensure the connection is good; a poor connection will introduce noise.
3. Mount a metal-coated NanoProbe cantilever into the electric field cantilever
holder. MFM-style cantilevers (225 m long, with resonant frequencies around 70
kHz) usually work well. It is also possible to deposit custom coatings on model
FESP silicon TappingMode cantilevers. Make sure that any deposited metal you use
adheres strongly to the silicon cantilever.
4. Set up the AFM as usual for TappingMode operation. In the Channel panels, be
certain all Highpass and Lowpass filters are Off. Set the Rounding parameter in
the Microscope / Calibrate / Scanner window to zero (0.00).
5. Select View / Cantilever Tune.
6. Follow the instructions below for the type of electric force imaging desired,
Phase Detection or Amplitude Detection.
Phase
Detection

MFM / EFM

Phase Detection
Phase Detection is only available when the Extender Electronics Module has been
correctly configured into the system.

In the Cantilever Tune window, set Start frequency and End frequency to
appropriate values for your cantilever (e.g., for 225 m MFM cantilevers, set
Start frequency to 40 kHz and End frequency to 100 kHz). Select Autotune.

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Two curves appear on the Cantilever Tune graph: the amplitude curve in white,
and the phase curve in yellow. (In Figure 14. 17, the phase curve is the dashed
line and the amplitude curve is the solid line.).

Figure 14.18. Phase detection Cantilever Tune

(Extender Electronics Module installed).
The phase should decrease with increasing frequency and cross the center line
(90 point) at the peak frequency. The phase curve then correctly reflects the
phase lag between the drive voltage and the cantilever response. Again, gradients in the electric force will cause a shift F0 in the resonance frequency. In this
case, resonance shifts give rise to phase shifts which can then give an image
of the electric force gradients; see Figure 14.18.
180

Phase (deg)

F0

90

Drive Frequency
Figure 14.19. Shift in phase at fixed Drive frequency.

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Under Interleave Controls set the Lift start height to 0 nm, and Lift scan
height to 100 nm. (The lift height can later be optimized.) Set the remaining
Interleave parameters (Setpoint, Drive amplitude, Drive frequency, and
gains) to the main Feedback Controls values. This can be done by setting the
flags (left of the Interleave Control column) to off (grayed bullets).

Quit Auto Tune and return to Image Mode

Engage the AFM and make the necessary adjustments to obtain a good
topography (Height) image on Channel 2.

Select the Interleave Controls panel. Set the Setpoint, Drive amplitude,
Drive frequency to Main (off grayed bullets). Verify that Interleave scan is
set to Lift.

Choose a Lift scan height of 100 nm. This will be optimized later. Set the
Channel 1 image Data type to Phase and choose Retrace for the scan Line
direction on both Channel 1 and 2 images.

Switch Interleave mode to Enable to start LiftMode. Set the Channel 1 Scan
line to Interleave to display interleave data. This screen should now display the
cantilever phase change due to electrical force gradients from the sample in the
left image and topography in the right image.

Optimize the Lift height. For high-resolution, make the Lift scan height as
small as possible without crashing the tip into the surface. If the tip crashes into
the surface it creates bright or dark streaks across the image. Also, if the Lift
scan height is set extremely low, the tip may continuously tap on the surface
during the LiftMode scan. Check this by toggling between the Interleave and
main scan lines for the phase image. The two images will look very similar if
the tip is continuously tapping on the surface during the LiftMode scan. In this
case, increase the Lift scan height until the Interleave scan image abruptly
changes, indicating that it is now oscillating above the surface and not
continuously tapping.

Adjust the sample or tip voltage to confirm that contrast is due to electrical force
gradients. On very rough samples, contrast in LiftMode images may be from
air damping between the tip and surface. It is often useful to look at the phase
data in Scope Mode while adjusting the tip or sample voltage up and down.
Contrast due to electrical force gradients should increase or decrease as the tipsample voltage is changed.

For more quantitative results, switch the to the frequency Data Type for
Channel 1. This technique provides a direct measure of the change in resonant
frequency felt by the cantilever. It may be necessary to optimize the FM
(frequency modulation) gain to properly track the shifts in resonant frequency.
This is described in detail in Chapter 13 of the appropriate product instruction
manual.

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Electric Force (EFM) Imaging

14.4.1. Amplitude Detection

Amplitude
Detection

14.4.1.1. With Extender Electronics Module.

MFM / EFM
To set up for Amplitude Detection field gradient imaging on systems with the
Extender module installed, follow the instructions in Section 14.4.1, Phase Detection, with the exception that the Channel 1 Data Type should be set to Amplitude.)

14.4.1.2. Without Extender Electronics Module.

Notes

This imaging method, although described here, is not recommended without the
Extender Electronics module due to the presence of artifacts.
Amplitude Detection, unlike Phase Detection, is available with or without the
optional Extender Electronics Module. This section describes the differences in
software set up and imaging for EFM systems without the Extender module. When
EFM imaging without the Extender module, changes in the cantilever amplitude
provide an indirect measure of shifts in the cantilever resonance frequency as
shown in Figure 14.19.

Amplitude

F0

Drive Frequency
Figure 14.20. Shift in amplitude at fixed Drive Frequency
(Extender Electronics Module not installed).

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Set the Drive frequency to the left side of the cantilever resonance curve, as
shown in Figure 14.20 below.

Figure 14.21. Amplitude detection Cantilever Tune

(Extender Electronics Module not Installed).

For maximum sensitivity, set the Drive frequency to the steepest part of the
resonance curve. As the tip oscillates above the sample, a gradient in the
magnetic force will shift the resonance frequency F0; (see Figure 14.19).
Tracking the variations in oscillation amplitude while in LiftMode yields an
image of the electric force gradients. Either side of the resonance may be used,
though we have obtained slightly better results on the low side, as shown in
Figure 14.19.

When using Amplitude Detection, optical interference may sometimes appear

in the lift (magnetic force) image when imaging highly reflective samples.
Optical interference appears as evenly spaced, sometimes wavy lines with
about 12m spacing superimposed on the lift image. This occurs when
ambient laser light (i.e., light passing around or through the cantilever, then
reflecting off the sample) interferes with laser light reflecting from the
cantilever. Interference can be alleviated by moving the beam spot up the
cantilever away from the tip; about one-third of the cantilever length from the
tip usually works well. On the MultiMode head, the adjustment can be refined
by carefully moving the beam spot laterally on the cantilever while scanning
until interference fringes are minimized.

Notes

Optical interference is essentially eliminated by using phase detection or

frequency modulation, available only with the Extender Electronics Module.

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Electric Force (EFM) Imaging

14.5. Surface Potential DetectionTheory

Notes

Surface potential detection EFM is only possible using the Extender Electronics
Module. This section does not apply to microscopes which are not equipped
with the Extender Electronics Module.
The Extender Electronics Module allows measurement of local sample surface
potential. This is similar to techniques called Scanning Maxwell Stress Microscopy
and Kelvin Probe Microscopy. Surface potential detection is a two-pass system
where the surface topography is obtained in the first pass and the surface potential
is measured on the second pass. The two measurements are interleaved, that is, they
are each measured one line at a time with both images displayed on the screen
simultaneously.
A block diagram of the surface potential measurement system is shown in
Figure 14.21. On the first pass, the sample topography is measured by standard
TappingMode. In TappingMode the cantilever is physically vibrated near its resonant frequency by a small piezoelectric element. On the second pass, the piezo that
normally vibrates the cantilever is turned off. Instead, to measure the surface potential, an oscillating voltage V ac cos t is applied directly to the cantilever tip. This
creates an oscillating electrostatic force at the frequency on the cantilever. The
oscillating force has the following amplitude:
dC
F = ------- V dc V ac
dz
dC
where ------- is the vertical derivative of the tip/sample capacitance.
dz

V dc = V tip V sample , the dc voltage difference between the tip and the sample,

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and V ac is the amplitude of the oscillating voltage applied to the cantilever tip.
Cantilever Deflection Signal
Photodiode Signal
RMS Detector

Amplitude Signal

Lock-in
Amplifier
Reference
Signal

Laser
Beam
Photodetector

Tapping
Piezo

To
Tip

Servo Controller

DC Voltage

Sum
AC

Signals to
NanoScope

(Feedback loop
adjusts DC tip
voltage to zero lockin signal)

Potential Signal
Sample
Oscillator Signal
GND

High Resolution
Oscillator

Extender Electronics Module

Figure 14.22. Simplified block diagram of extender electronics module

in surface potential mode.
The key here is that the force on the cantilever depends on the product of the ac
drive voltage and the dc voltage difference between the tip and the sample. And,
when the tip and sample are at the same dc voltage (Vdc=0), the cantilever will feel
no oscillating force. The Extender Electronics Module uses this fact to determine
the effective surface potential on the sample, Vsample. The Extender determines
the local surface potential by adjusting the dc voltage on the tip, Vtip, until the
oscillation amplitude becomes zero. At this point the tip voltage will be the same as
the unknown surface potential. The voltage applied to the cantilever tip Vtip is
recorded by the NanoScope III to construct a voltage map of the surface.

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14.6. Surface Potential DetectionPreparation

It is often desirable to apply a voltage to one or more areas of a sample. This may
be done in two ways: by connecting a voltage to the sample mounting chuck, or by
making direct contact to the sample. In both cases, jumper configurations in the
bottom of the microscope must be changed to match the environment desired.

Notes

In addition to any reconfigured jumpers, remember to connect the common or

negative terminal of an external power supply to the MultiMode ground or the
AFM chassis.
1. Power down the NanoScope controller and turn off all peripherals. Unplug the
NanoScope power cable from the microscopes electronic box.
2. Locate the jumpers on the electronic board, visible in a window on the bottom
of the MultiMode per Figure 14.5. As shipped from the factory, the baseplate jumpers should appear as shown in Figure 14.22.
Ground
Piezo Cap
GND/OSC + DC
Unused
GND/OSC + DC
To AFM Tip
Auxiliary D (to NanoScope III controller)
STM
Indicates jumpers

Figure 14.23. Normal jumper configuration as shipped from factory for

MultiMode SPM with Extender Electronics Module installed. Sample is
held at ground.

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3. Depending upon whether voltage is to be applied to the sample directly or indirectly, reconfigure jumpers if indicated.

14.6.1. Applying Voltage to the Sample Directly

When voltage is applied directly to the sample, there is no need to reconfigure the
jumpers. They should remain jumpered as shipped from the factory (Figure 14.22),
and the sample should be electrically insulated from the chuck.
Connect the external voltage source directly to the sample by attaching fine gauge
wire to appropriate contacts (e.g., on integrated circuits connect electrical leads
directly to pads). For normal operation, the sample chuck is held at ground; be certain to carefully any electrical connections from the sample chuck.
>10 M
External Voltage
Source

Sample
Electrical Insulator
Sample Chuck

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14.6.2. Applying Voltage to the Sample Through Piezo Cap

When voltage is to be applied to the sample via the sample piezo cap for indirect
surface potential imaging, configure the jumpers as shown in Figure 14.23.
()

Ground

External Voltage
Source

(+)

Piezo Cap

>10 M
GND/OSC + DC
Unused
GND/OSC + DC
To AFM Tip
Auxiliary D
STM

Indicates jumpers

Figure 14.24. Jumper configuration for application of voltage to sample via

sample chuck.
A current-limiting resistor (e.g., 10100 M) should be placed in series with the
external voltage supply to protect the tip and sample from damage. Current-limited
power supplies may also be used. Voltage leads should be connected to pins on the
header using soldered, push-on connectors. Do not solder leads directly to the
header pins. Heat may cause damage and/or make jumpering the pins difficult.
The sample should be electrically connected directly to the chuck or a standard
sample puck using conductive epoxy or silver paint as shown below:
Conductive Epoxy
or Paint
Sample
Sample Chuck

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14.7. Surface Potential ImagingProcedure

1. Locate the two toggle switches on the backside of the Extender Electronics box
(Figure 14.24), then verify that they are toggled as shown in Table 14.2.

Mode

Tip or Sample
Voltage

FM/Phase

Gnd/Surface Potential

Surface Potential
To
cro
sc

To
e
Scop
Nano

Analog 2

Mi

op

Figure 14.25. Toggle switches on back of Extender Electronics Module.

Mode
FM/Phase
TappingMode
Contact AFM
MFM

GND/Surface
Potential

Analog 2

Surface Potential

Apply voltage to
tip or sample (Use
for electric field
gradient imaging;
tunneling AFM)

Tip or Sample Voltage

Surface
Potential

Table 1.2.Extender Electronics Module toggle switch settings for

surface potential imaging.

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Notes

The toggle switch combination of Surface Potential = ON and Analog2 = ON is

not recommended and can produce erratic and undefined results.
2. Mount a sample onto the sample holder. Make any external electrical connections that are necessary for the sample.
3. Mount a metal-coated NanoProbe cantilever into the electric field cantilever
holder. MFM-style cantilevers (225 m long, with resonant frequencies around
70 kHz) usually work well. It is also possible to deposit custom coatings on model
FESP silicon TappingMode cantilevers. Verify that all deposited metal adheres
strongly to the silicon cantilever.
4. Set up the AFM as usual for TappingMode operation.
5. Use Cantilever Tune: AutoTune (as described in Section 14.4.1) to locate the
cantilevers resonant peak. Remember, however, that the Extender box has been
reconfigured so that the phase detection circuitry now acts as a lock-in amplifier.
Any procedures that are normally used to view or adjust the phase signal will now
affect the lock-in signal instead (see Figure 14.21).
In this case, two curves should appear in the Cantilever Tune box: the amplitude
curve in white and the lock-in curve in yellow. In the event you find more than one
resonance, select a resonance that is sharp and clearly defined, but not necessarily
the largest. It is also helpful to select a resonant peak where the lock-in signal also
changes very sharply across the peak. Multiple peaks can often be eliminated by
making sure the cantilever holder is clean and the cantilever is tightly secured.
6. Engage the AFM and make the necessary adjustments for a good TappingMode
image while displaying height data.
7. Select the Interleave Controls command. This brings up a new set of scan
parameters that are used for the interleaved scan where surface potential is measured. Different values from those on the main scan may be entered for any of the
interleaved scan parameter. To fix any of the parameters so they are the same on the
main and interleave scans, click on the green bullets to the left of particular parameter. The green bullet changes to off (gray) and the parameter value changes to
the main Feedback Controls value. Set the interleave Drive frequency to the main
feedback value. Enter an interleaved Setpoint of 0 V. Set Interleave scan to Lift.
8. Enter an Interleave Controls Drive amplitude. This is the ac voltage that is
applied to the AFM tip. Higher Drive amplitude produces a larger electrostatic

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force on the cantilever and this makes for more sensitive potential measurements.
Conversely, the maximum total voltage (ac + dc) that may be applied to the tip is
10 V. So a large Drive amplitude reduces the range of the DC voltage that can be
applied to the cantilever. If the sample surface potentials to be measured are very
large, it is necessary to choose a small Drive amplitude, while small surface potentials can be imaged more successfully with large Drive amplitudes. To start choose
a Drive amplitude of 5 V.
9. Set the Channel 2 image Data type to Potential. Set the scan Line direction for
the main and interleave scans to Retrace. Remember to choose the Retrace direction because the lift step occurs on the trace scan and data collection occurs on the
retrace.
10. Choose a Lift start height of 0 nm and a Lift scan height of 100 nm. The Lift
scan height can be readjusted later.
11. Switch Interleave mode to Enable to start LiftMode. Now, when the microscope completes a topographic scan line (trace and retrace) the system turns off the
TappingMode piezo and switches the oscillator signal to the cantilever. The cantilever is driven electrostatically according to the interleave Drive amplitude that has
been selected. Also, when Potential is selected as the Data type for the Channel 2
image, a feedback circuit is enabled in the Extender box which adjusts the dc voltage on the tip to maintain the cantilever oscillation amplitude at zero. To do this, the
feedback circuit uses the lock-in signal of the cantilever oscillation and tries to keep
this value at zero volts. As detailed in the Section 14.5 above, when the cantilever
oscillation amplitude has returned to zero, the dc voltage on the tip and sample are
the same. The NanoScope records the dc voltage applied to the tip and this signal is
displayed in the Potential data type.
12. Adjust the FM gains. The feedback loop that is used by the Extender Electronics
for surface potential measurements is the same as the one used in Frequency Modulation (FM) for magnetic and electric force gradient detection, as described previously. The feedback loop should be tuned in a similar manner to the FM setup.
Select Other Controls and adjust the FM gains. Setting both FM Integral gain and
FM Proportional gain to 15.0 is a good starting point. As with the topography
gains, the scan can be optimized by increasing the gains to maximize feedback
response, but not so high that oscillation sets in. The gains often need to be much
lower for potential measurements than for standard FM measurements. More information on tuning the feedback loop is given in the Troubleshooting section below.
13. Optimize the Lift heights. Set the Lift scan height at the smallest value possible
that does not make the Potential feedback loop unstable or cause the tip to crash
into the sample surface. When the tip crashes into the surface during the Potential
measurement, dark or light streaks appear in the Potential image. In this case,
increase the Lift scan height until these streaks are minimized.
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14. For large sample voltages or qualitative work, select Data type = Phase instead
of Potential. When the Extender box has been configured for surface potential
measurements, the phase signal is actually the cantilever amplitude signal, as
measured by a lock-in amplifier. If the feedback loop is not enabled by selecting the
Data type = Potential, the lock-in cantilever amplitude depends on the voltage difference between the tip and sample in a roughly linear fashion. (The lock-in amplifier produces a voltage that is proportional to the cantilever amplitude.) Qualitative
surface potential images can be collected using this lock-in signal. Also, if the sample has a surface potential that exceeds 10 V (greater than the range of the Potential signal), it is possible to use the lock-in signal to provide qualitative images that
reflect the sample surface potential. To view the lock-in signal with the reconfigured Extender box, select the Data type = Phase.

14.7.1. Troubleshooting the surface potential feedback loop.

The surface potential signal feedback loop can be unstable. This instability can
cause the potential signal to oscillate or become stuck at either +10 V or -10 V. Here
are some tips to see if the feedback loop is working properly with no oscillation:

Go into Scope Mode and look at the Potential signal. If oscillation noise is
evident in the signal, reduce the FM gains. If oscillations persist even at very
low FM gains, try increasing the Lift scan height and/or reducing the Drive
amplitude until oscillation stops. If the tip crashes into the surface the Lock-in
signal becomes unstable and can cause the feedback loop to malfunction.
Increasing the Lift height and reducing the Drive amplitude can prevent this
problem. Once oscillation stops, the FM gains may be increased for improved
performance.
In Scope Mode, if the Potential signal is perfectly flat and shows no noise even
with a small Z-range, the feedback loop is probably stuck at 10 V. (You can verify
this by changing the value of Real-time planefit to None in the Channel 1 panel.)
Reduce the Scan rate and watch the display monitor which indicates the cantilever
amplitude. On the topographic trace, the voltage displayed should be the setpoint
selected for the Main scan. On the Potential trace, this voltage drops close to zero if
the cantilever oscillation is being successfully reduced. If the value on the display
monitor instead goes to a large nonzero value, the feedback loop is probably not
working properly. In this case, try reducing the Drive amplitude and increasing the
Lift scan height. It may also be helpful to momentarily turn the Interleave mode
to Disabled, then back to Enabled. Also try reducing any external voltage that is
being applied to the sample to stabilize the feedback loop, then turn the voltage
back up.

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MultiModeSPM Instruction Manual

Chapter 15 Calibration Procedures,

Troubleshooting and Maintenance

This chapter provides detailed instructions for the fine calibration of Digital Instruments MultiMode SPMs. Additionally, the latter part of the chapter focuses on
problems commonly encountered during operation of the microscope and then concludes with maintenance procedures for the MultiMode SPM adjustment screws.
Operators should establish a three-month service schedule for mainentance and calibration. Check the SPMs measuring accuracy periodically to ensure that images
are dimensionally represented within acceptable limits of error. If measuring accuracy is critical, or if environmental factors (e.g., humidity, temperature) impact the
SPM significantly, this may require a quick check at the start of each imaging session.

15.1. SPM Calibration TheoryOverview

Digital Instruments employs a software-guided calibration procedure for all its
microscopes. The procedural particulars of how calibration is executed using NanoScope software are beyond the scope of this document and include proprietary
methods exclusive to Digital Instruments. The theory, however, is straight forward
and consists of the steps listed below.

Scan a calibration reference having surface features of precisely known

dimensions.

Compare known dimensions on the calibration references surface with those

estimated by the SPM software.

Adjust calibration parameters until the SPMs dimensions accord with the true
dimensions of the reference.

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The Capture Calibration and Autocalibration routines are designed to optimize

measuring accuracy over the entire measuring range of the scanner. In order to
obtain the finest accuracy possible for a given scan size, the scanner calibration
parameters can be manually fine-tuned. This may prove useful in applications
where measuring accuracy must be better than 1 percent.

15.1.1. Theory behind calibration

For purposes of calibration, the NanoScope software employs various derating and
coupling parameters to model scanners nonlinear characteristics. By precisely
determining points along the scanners sensitivity curve, then applying a rigorous
mathematical model, full-range measuring capabilities can be made accurate to better than 1 percent.
Consider the sensitivity curve represented here:

Voltage

440 V

110 V
0
0

Scanner Movement (nm)

This curve typifies scanner sensitivity across the full range of movement. The vertical axis denotes voltage applied to the scanner. The horizontal axis denotes scanner
movement. At higher voltages, the scanners sensitivity increases (i.e., more movement per voltage applied). At zero volts, the scanner is motionless. Plotting each
point along the curve describes a second-order, exponential relationship which provides a rough approximation of scanner sensitivity.
Unfortunately, things are more complicated. Because piezo materials exhibit hysteresis, their response to increasing voltage is not the same as their response to
decreasing voltage. That is, piezo materials exhibit memory, which causes the
scanner to behave differently as voltages recede toward zero. The graph below represents this relationship.

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Scanner
Voltage

Scanner
Movement

Time
To produce the sharp, linear movements (triangular waveform) required for accurate back-and-forth scanning, it is necessary to shape the applied voltage as shown
on the top graph above. Moreover, the applied voltage must compensate for scan
rate and scan size. As scan rate slows, the applied voltage must compensate for
increased memory effects in the piezo material. As scan size is decreased, the piezo
exhibits more linearity. These effects are further complicated by X-Y-Z coupling
effects (the tendency for one axis to affect movement in other axes).
Through rigorous quality control of its scanner piezos, Digital Instruments has
achieved excellent modeling of scanner characteristics. Two calibration points are
typically used for fine-tuning: at 150 and 440 volts. (A third point is assumed at 0
nm/volts.) These three points yield a second-order sensitivity curve to ensure accurate measurements throughout a broad range of scanner movements.
Because scanner sensitivities vary according to how much voltage is applied to
them, the reference must be thoroughly scanned at a variety of sizes and angles.
The user then tells the software the distance between known features on the references surface, and a parameter is recorded to compensate the scanners movements. The X, Y and Z axes may be calibrated in any sequential order; however, the
linearization adjustments (Section 15.4) must be performed before any calibrations
are attempted (otherwise, they will be undone by the linearity adjustments).

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15.2. Sensitivity and Scanner Calibration

Background Information
Scanners serve as the movers and shakers of every scanning probe microscope.
Typically, they consist of a hollow tube made of piezoelectric material such as PZT
(lead zirconium titanate). Piezo materials contract and elongate when voltage is
applied, according to whether the voltage is negative or positive, and depending
upon the orientation of the materials polarized grain structure. Scanners are used to
very precisely manipulate sample-tip movement in order to scan the sample surface. In some models (e.g., Small Sample MultiMode) the scanner tube moves the
sample relative to a stationary tip. In other models (e.g., Dimension SPMs) the sample is stationary while the scanner moves the tip.
Not all scanners react exactly the same to a voltage. Because of slight variations in
the orientation and size of the piezoelectric granular structure (polarity), material
thickness, etc., each scanner has a unique personality. This personality is conveniently measured in terms of sensitivity, a ratio of piezo voltage-to-piezo movement. Sensitivity is not a linear relationship, however. Because piezo scanners
exhibit more sensitivity (i.e., more movement per volt) at higher voltages than they
do at lower voltages, the sensitivity curve is just thatcurved. This non-linear relationship is determined for each scanner crystal and follows it for the life of the
scanner. As the scanner ages, its sensitivity will decrease somewhat, necessitating
periodic recalibration.

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The diagram below represents scanner crystal voltage versus photodiode voltage. In
this instance, detector sensitivity is given as volt per volt, a parameter provided in
the Force Calibration screen.
Photodiode voltage
Laser

Photodiode
array

Cantilever
-220 VDC

0 VDC

+220 VDC

Scanner

Photodiode Voltage

+3.0

Detector Sensitivity

-3.0
-220

0
Scanner Voltage

+220

The Microscope / Calibrate / Scanner function displays the Scanner Calibration

dialog box, allowing users to enter the sensitivity of their scanners X-Y axes. Here,
sensitivity is measured in terms of lateral displacement for a given voltage (nm/
volt). In addition, other parameters measure the scanners X-Y coupling and other
effects.

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15.3. Calibration References

As described above, each scanner exhibits its own unique sensitivities; therefore, it
is the task of the user and software to precisely measure these sensitivities, then
establish software parameters for controlling the scanner. This task is accomplished
with the use of a calibration reference.

180 nm deep
10 m

10 m

Figure 15.1. Section of Digital Instruments platinum-coated,

silicon calibration reference.
One such calibration reference is shown in Figure 15.1 above. This calibration reference consists of a silicon substrate having a regular series of pits, each 180 nm
deep, which is plated with platinum. Pits are spaced apart on 10 m centers. Other,
similar surfaces are available having different dimensions. Atomic-scale calibrations are generally carried out with mica or graphite, which exhibit very regular
atomic lattices. Calibration references serve as the primary tool by which SPMs are
calibrated. They serve as measuring sticks with which to gauge scanner displacement for a given voltage.
The SPM should be capable of measuring a calibration reference with an accuracy
of 2 percent or better while scanning at the maximum Scan size setting. By using
fine calibration techniques, it is possible to calibrate the SPM to much better than
this.

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15.4. Linearity Correction Procedure

For applications which demand good linearity, the following procedure can be used
to optimize the linearity correction parameters for individual scanners. As discussed
previously, linearity correction is especially important for long-range scanners
(such as the J and K).

15.4.1. Check scanner parameter values

If the system's original scanner parameters have been deleted, the scanner parameters can be copied from the software backup disk which is sent with every system.
Individually purchased scanners are shipped with a head/scanner disk which contains the backup files, or a hard copy of the scanner parameters. In the event that
files are not found, fax or call Digital Instruments for scanner calibration records.

15.4.2. Align calibration reference

Load the silicon calibration reference into the SPM. The reference will need to be
aligned with the microscope scanner so that the tip scans parallel to the references
features with the Scan angle set at 0 degrees.

Scan angle = 0

For D and E scanners, use a 1-micron pitch reference. For G, J, and K

scanners, use a 10 micron pitch height reference. Align the reference within about 2
degrees of perpendicularity to the scan axes.

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15.4.3. Set Real Time parameters

Set parameters in the control panels to the following values:

Panel

Parameter

Setting

Scan Controls

Scan Size

440 V

X offset

0.00 nm

Y offset

0.00 nm

Scan angle

0.00 deg

Scan rate

2.44 Hz

Other Controls
Channel 1

Number of samples

256

Slow scan axis

Enabled

Z limit

440 V

Units

Volts

Data type

Height

Z range

~ 20 Va

a. Adjust the Z range parameter to obtain the best contrast.

15.4.4. Set up SPM for contact AFM.

Set up the microscope for contact AFM imaging: set the AFM mode to Contact.
(The microscope can also be calibrated using STM; however, this example will utilize contact AFM.) Set the Scan angle to 0 degrees. Adjust Real-time parameters to
obtain a good-quality, maximum Scan size image. The Scan rate should be set to a
value of 2.44 Hz and the Number of samples parameter should be set at 256.
With the sample engaged, check the scanning line relative to the references features; the scan should be orthogonal to the pits on the reference. If the reference
requires rotation, Withdraw and rotate the sample to improve orthogonality
between sample and scan line. Repeat until features are oriented orthogonally with
the scan frame.

15.4.5. Check sample orthogonality.

Check the sample scan for orthogonality along both the X- and Y-axes. If the scan is
aligned along one axis of the scan but not another, it may be necessary to adjust the
microscopes Orthogonality parameter in the Scanner Calibration panel. To measure a captured images orthogonality, view it using the Off-line / View / Top View
function. On the display monitor, click on the Angle command, then use the mouse
to draw a cursor between the edges or centers of widely spaced pits (see left figure

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below). The angle should be measured with the vertex near the center of the image
and the vertices in the upper-right or lower-left quadrant. The angle will be displayed on the white status bar at the bottom of the display monitor. Use the mouse
to drag the cursor until it is oriented correctly,

Figure 15.2. Left image: non-orthogonal image. Notice how pits are aligned
with the vertical (slow) axis but skewed with the horizontal (fast) axis.
Right image: a corrected, orthogonal scan.
then read the angle off the status bar. If the angle differs by more than a half degree,
a correction will be required; otherwise, skip ahead to the step below.

15.4.6. Adjust sample orthogonality.

To adjust the orthogonality of the scan, click on Real Time / Microscope / Calibrate / Scanner to access the Scanner Calibration panel. The Orthogonality
parameter is displayed on the bottom-right corner of the panel. Enter the difference
between 90 degrees and the angle measured in the Top View image. (For example,
if the angle measured in the Top View image was 92.5 degrees, enter a value of -2.5
degrees into the Orthogonality parameter.) Click the Ok button to exit the Scanner Calibration panel, then capture another image and re-measure the angle.
Repeat correction of Orthogonality until the scanned image shows less than 0.5
degrees of error. After a major change to the orthogonality parameter, it may be
necessary to physically realign the calibration standard to the image frame.

15.4.7. Adjust mag0 and arg0

Select Microscope / Calibrate / Scanner to display the Scanner Calibration dialog box. Set mag0 and arg as follows:
When adjusting linearity, it is essential to keep in mind which part of the scan is the
beginning and which is the ending. When the Line direction is set to Trace, the
beginning of the fast scan is on the left, as indicated by the arrow base. When viewing up or down scans, be careful to check the image against itself, not the residual
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image from the previous scan. Also, be careful to compare only the part of the scan
drawn since the last parameter change.
Because the display monitor screen itself is not linear, the best way to check mag0
and arg is with the Real-time Zoom box.
A. Adjusting Fast mag0
After engaging, click on Microscope / Calibrate / Scanner. This will invoke the
Scanner Calibration window. As parameters values are changed, the effects will
be seen on the display monitor. Now move the mouse cursor to the display monitor
and select Zoom Out. This will produce a box whose size and position can be
changed by alternate clicks on the left mouse button. Adjust the box until it is about
one-third the size of the scan. Click once on the right mouse button to park the box
and free the cursor, which will jump to Execute. (Clicking twice will execute a
Zoom, which we don't want to do.)
Select (highlight) the scanner parameter to be modified. The first one to do is Fast
mag0. Now move the zoom box to the start of the fast scan (on the left if the Line
direction is set to Trace). Move and size the zoom box until the beginning third of
the scan's features are exactly aligned with the zoom box. The beginning third of the
scan will be the standard for judging almost all of the linearity values. It is a good
technique to ignore the set of features near the edges of the scan since these may be
distorted slightly. Now move the zoom box to the ending third of the scan. Align
one side of the zoom box with some features and observe how well the other side
aligns with the features under it.
Compared to the beginning third of the scan, if the features in the ending third of
the scan are too big to fit the same number of them inside the zoom box, type a
smaller number for Fast mag0. If the features are too small, increase Fast mag0.
Change mag0s by about 0.1 to 0.3 units at a time. Remember, every time a parameter is changed, the entire scan axis is affected, so after every change it is necessary
to resize the zoom box at the beginning third of the scan and re-compare the ending.

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B. Adjusting Fast arg

Now that the beginning third of the scan is equal to the ending third, the center may
need adjusting. Just as before, if the center features are too big for the box, reduce
the Fast arg. If the features are too small, increase the Fast arg. Change args by
0.2 to 0.5 units at a time. Remember, changes affect the whole scan, so keep resizing the zoom box after changes.

Center Compressed

Center Expanded

Figure 15.3. X scan linearizationcompression vs. expansion.

Notes

After an adjustment in Fast arg is made, Fast mag0 may need to be readjusted.
Continue steps A and B until the rulings are evenly spaced across the Fast-axis.
(If using a one-dimensional reference, it may be desirable to do step E
{Adjusting Fast mag1} before proceeding; because adjusting the slow linearity
will require the one-dimensional reference to be physically rotated 90 degrees.
After finishing step E, return to here.)
After Fast mag0 and Fast arg have been set, insert these values for Slow mag0 and
Slow arg. These will serve as close starting points before adjusting the slow linearities.
C. Adjusting Slow mag0
Follow the same instructions as for Fast mag0. Setting the slow linearities requires
a lot of time because after making a parameter change it is necessary to wait until a
fresh third of a scan has begun with the new parameters before the zoom box can be
resized. Move the resized box to the ending of the scan and be prepared to measure
the ending quickly. If the user is quick enough, a new parameter value can be typed

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in before the scan starts again. Be careful not to confuse scan top and bottom with
beginning and ending, since the scan direction alternates. Adjust the zoom box to fit
the beginning third of the scan and check the ending third. If the features at the ending third are too big for the box, reduce the parameter. If the features are too small,
increase. Be careful to compare only parts of the current scan, not the previous one.

Center Compressed

Center Expanded

Figure 15.4. Y scan linearizationcompression vs. expansion.

D. Adjusting Slow arg
Follow the same instructions as for Fast mag0. Adjust the zoom box to fit the
beginning and ending of the scan, then check the center. If the features in the center
are too big, reduce the Slow arg. If the features are too small, increase.
After an adjustment of Slow arg, Slow mag0 may need to be readjusted. Continue
to follow steps C and D until the rulings are evenly spaced along the slow axis.
E. Adjusting Fast mag1
Initial Adjustment
Close the Scanner Calibration window by selecting OK. (Selecting Restore will
reset the parameters to the values when the box was opened.) Change the Scan size
to 150 volts. Select View / Scope Mode. On the display monitor, select Dual
Trace. If the two scope traces do not overlap, Fast mag1 needs to be adjusted. On
the control panel, select Slow scan axis. When some tall features appear on the
scope trace, tap the keyboard's right or left arrow key to toggle Slow scan axis to
Disabled. Select Microscope / Calibrate / Scanner to open the Scanner Calibration box. Select Fast mag1. Use the left and right arrow keys to change the value
until the two traces are aligned. (The yellow retrace line will shift in the same direction as the arrow.) When done, select OK to close the Scanner Calibration box.
Set Slow scan axis back to Enabled. Select View / Image Mode.

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Fine Adjustment
Initial adjustment is usually adequate; however, if more precision is desired, adjust
Fast mag1 using the same procedure as in step A (see Adjusting Fast mag0). As
before, set the Zoom box for the beginning of the scan and then check the ending.
(Because the scan is small, it may be necessary to use a Zoom box up to one-half as
large as the scan). If the ending of the scan is bigger than the beginning, reduce
Fast mag1. If the ending is too small, increase the value.
F. Adjusting Slow mag1
With the Scan size still set to 150 volts, select Microscope / Calibrate / Scanner.
Select Slow mag1 and input the value from Fast mag1. For medium-sized scanners
(C to F), it is probably worth stopping here, because the Slow mag1 value is usually
100-120 percent of the Fast mag1 value. However, if more precision is desired,
adjust Slow mag1 using the same procedure as in step C (see Adjusting Slow
mag0). As before, set the Zoom box for the beginning of the scan and then check
the ending. (Because the scan is small, it may be necessary to use a Zoom box up to
one-half as large as the scan). If the ending of the scan is bigger than the beginning,
reduce Slow mag1. If the ending is too small, increase the value.
Wait one complete frame with the new value before readjusting the Slow mag1
value.
This completes the linearity adjustments. Check the final result by capturing an
image and checking it with the Off-line / Modify / Zoom window. The scanner is
now ready for calibration of the X and Y parameters.

15.5. X-Y Calibration using Capture Calibration

Scanners are calibrated by setting parameters in the NanoScope software using the
Capture Calibration command. This basic step must be performed before fine calibration. The basic procedure using version 4.XX software and a 10-micron calibration reference (Figure 15.1) is described in this section. Earlier versions of
NanoScope software are similar. Note that D and E scanners require a 1micron cross-ruling.
1. With the Scan rate set at 2.44 Hz and Number of samples parameter at 256, a
full Capture Calibration will require about 70 minutes. Increasing the Number of
samples, or decreasing the Scan rate will significantly increase the required time.

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2. Using the mouse, click on Real-time / Capture / Calibration. The Capture

Calibration dialog box will be displayed:
Capture Calibration
File Name Prefix: calibrat
cxx
sfx
dfx
cyy
sfy
dfy
dxx
ssx
dsx
dyy
ssy
dsy
Withdraw when completed
Capture

Quit

The Capture Calibration dialog box lists twelve parameters used in the calibration
procedure. If this is a first-time calibration, or if the microscopes calibration has
not been checked within the last three months, verify that all parameters are
selected. Click on the Capture button to initiate the automatic calibration routine.

Notes

The microscope will begin an automatic series of scans on the reference which
require about one hour total to complete. During each scan, the scanner moves
the piezo using carefully calculated movements. Many of these movements are
unusual, giving rise to a variety of images which do not look like the normal
reference. For example, pits may resemble trenches and features may be
presented at various angles.
3. As each routine is executed, the user may need to adjust the scan slightly to optimize the calibration image. This is accomplished using the Capture Control dialog
box, which is displayed on the control monitor throughout the calibration routines.
Capture Control
Capturing at 311V, 45
Setpoint:

0.00 V

Adjust Y offset

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Up

Down

Skip

Abort

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Note the status bar at the bottom of the control monitor. The capture status will
start at skip 2meaning that the program will skip the current scan and one more
before capturing an image for later calibration. (This allows hysteresis and drift to
settle out when the scan changes direction and size between images.) If the scan has
not settled out by the time the capture status changes to On, click on the Skip button to increment the capture to skip 1, skip 2, or skip 3. Do not click on Abort
unless you want to stop the entire Capture Calibration program.
Features should extend across as much of the displayed image as possible. If portions of features are missing, or if the image is blank, click repeatedly on the
Adjust Y offset / Up or Down button to adjust the scan until more of the features
are imaged. When the image looks optimized, allow the software to capture the
image without disturbing it. The software will then automatically index to the next
image.

28.37 m

Figure 15.5. Use the Adjust Y offset / Up or / Down buttons to improve a

partial calibration image (left). Calibration image at right is improved
and may be used to measure distances between features.
After the first four images with the diagonal stripe pattern have been captured, the
user can usually leave the system unattended while the program continues to completion. Some of the next images may seem stretched in one dimension; however,
this is normal.
When all calibration images have been obtained, the software will prompt the user
that it is finished.
4. Go to the Capture directory (!:) where all Capture Calibration files have been
saved. Click on Off-line / File / Browse (or the Browse icon) to review all Capture
Calibration files.
5. Verify that all calibration images contain features spanning the full width and
height of the image frame. (See right Figure 15.5 above as an example.)

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Notes

All images unsuitable for calibration must be recaptured. Record the file name
extensions of any unusable files (e.g., .cxy, .dyy), then delete them. Reengage
the reference surface and select Capture Calibration again. Verify that the file
name prefix is identical to that of the usable files, then deselect all usable file
name extensions from the last capture (click on their box to remove the X).
Finally, click on the Capture button to recapture the selected files.

15.6. Off-line / Utility / Autocalibration

After the Capture Calibration routine is completed, the user measures surface features contained within each image and enters their dimensions into the software.
The software compares its estimates with the actual (user-entered) dimensions to
make final corrections. This portion of the calibration is carried out using the Offline / Utility / Autocalibration command.
To utilize the Off-line / Utility / Autocalibration command, do the following:
1. Select any of the captured calibration images in the Capture (!:) directory. Click
on the Off-line / Utility / Autocalibration command. The control monitor will display the X-Y Piezo Calibration dialog box:
X-Y Piezo Calibration
File Name Prefix: calibrat
Ssx & Dsx & Cxy & Dxy
Ssy & Dsy & Cyx & Dyx
Sfx & Dfx
Cxx & Dxx
Sfy & Dfy
Cyy & Dyy
Calibrate

Quit

Verify that the file name prefix assigned to the captured files from the Capture Calibration routine described in Section 15.5 above is correct.
2. For normal calibration, verify that all parameters are selected in the dialog box,
then click on Calibrate to execute the routine.

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The software will sequentially present various calibration images on the display
monitor while prompting the user to draw either a vertical line or a horizontal line.
The control monitor will simultaneously display various dialog boxesone for
each imagerequesting that a distance be entered.
3. Use the mouse to draw a line on the image. The line should be drawn to span as
many features as possible, preferably connecting like edges. For example, consider
the following:

Autocalibration

Draw a vertical line

In this example, a line is drawn from the bottom edge of one feature to the bottom
edge of another feature four rows awaya distance of 40 microns. The control
monitor simultaneously displays a dialog box for entering the distance indicated by
the white line:
MMAFMJ.PAR Xs-Xf coup der
New distance in m:
Cancel

35.95
Ok

The distance displayed in the box (in this example, 35.95 m) is the softwares estimate (based on current calibration values) of the length of the line drawn on the
image. If the line length is different from the value shown, it will have to be
changed. (In this example, the user would enter a value of 40.)
4. Enter the distance covered by the white line drawn on the image. If a 10-micron
reference is being employed, like portions of features are spaced 10 microns apart
(e.g., between bottom edges, left sides, etc.).

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Please Note: Features must be measured without regard to how they appear in calibration images. Remember, features may be represented as having stretched, distorted, or angled appearances due to the unusual movements employed during
Capture Calibration scanning. Regardless, features are separated by the same
(e.g., 10-micron) spacings.
5. Continue drawing lines and entering measured distances until all Capture Calibration images have been measured. When the software is finished, it will prompt
the user that it is done.
If Capture Calibration and Autocalibration routines have been completed correctly, the SPM should be calibrated within 1-2 percent accuracy over most of the
scanners measuring range. Should it be necessary to obtain still better accuracy, the
SPM can be fine-tuned to obtain maximum measuring accuracy. This is accomplished through the use of calibration parameters discussed in the next section.

15.7. Fine-tuning for X-Y Measuring Accuracy

Fine-tuning is usually performed at two Scan size settings: 150 and 440 volts. Both
horizontal and vertical measurements of sample features are made, then compared
with actual distances. Based upon this comparison, computer parameters are fine
tuned. To fine tune your SPM for maximum X-Y measuring accuracy, review each
of the steps below.

Notes

If you are using an A scanner to image atomic-scale features, it will necessary

to substitute graphite or mica for the silicon calibration reference. See Section
15.9 below for directions in atomic-scale calibration of the X- and Y-axes.

15.7.1. Prepare system for fine-tuning.

1. Set the Scan size parameter on the Scan Controls panel to the maximum value
(440 volts). Verify that the Scan angle is set at 0.00 degrees. Mount a calibration
reference into the SPM and begin imaging. This may consist of a generic (e.g., 10micron, silicon) reference, or a sample having features of known dimensions (e.g.,
grating, etc.). Optimize the image quality.
Please note: Your calibration and fine-tuning procedures are no better than the procedures and references used. Choose both carefully!

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15.7.2. Measure horizontally at 440 V scan size.

1. Set the Scan size parameter on the Scan Controls panel to the maximum value
(440 volts). Verify that the Scan angle is set to 0.00 degrees. Engage the surface.
2. Select two widely-spaced features on the sample image of known separation,
then use the mouse to draw a horizontal line between them. (For example, on a 10micron, silicon reference, draw the line from the left side of one pit to the left side
of another pit as far away as possible.) The screen will display the measured distance between pits next to the line.
Now check to see whether the microscopes measured distance agrees with the
known horizontal distance. If there is significant disagreement between the two,
fine tuning will be required; go to step #3 below. If the displayed distance agrees
with the known distance, skip to Section 15.7.3.
3. Based upon the results in step #2 above, perform the following calculation:
Known distance between features
----------------------------------------------------------------------------------------------------SPM-calculated distance between features

That is, divide the known distance by the distance displayed next to the line drawn
in step #2 above. Record this quotient.

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4. Click on the Real time / Microscope / Calibrate / Scanner option. The Scanner
Calibration dialog box will be displayed:
Scanner Calibration
X fast sens:
X fast derate:
X slow sens:

230 nm/V
0.230

nm/V2

267 nm/V

Y fast derate:
Y slow sens:

228 nm/V
0.218 nm/V2
257 nm/V

Y slow derate:

0.270 nm/V2

XsXf coupling:

0.548

nm/V2

YsYf coupling:

0.569 nm/V2

XsXf coup der:

0.027 pm/V3

YsYf coup der:

0.222 pm/V3

XsYf coupling:

0.078 nm V2

YsYf coupling:

0.134 nm V2

XsYf coup der:

-0.04 pm/V3

YsYf coup der:

0.0668 pm/V3

X slow derate:

0.286 nm/V2

Y fast sens:

Fast mag0:

1.40

Slow mag0:

1.47

Fast mag1:

1.05

Slow mag1:

0.860

3.00

Slow arg:

Fast arg:
Fast cal freq:

2.44 Hz

Slow cal freq:

Piezo cal:

440 V

Rounding:

Allow rotation:

Allow

Orthogonality:

Ok

3.00
4.77 Hz
0.00
0.00 deg

Cancel

Multiply the quotient obtained in step #3 above by the X fast sens value shown on
the Scanner Calibration panel, then enter the new value. The new value will adjust
the scanners fast axis to more closely match calculated distances with actual feature distances. The new sensitivity setting will take effect as soon as it is entered. To
save it to the computers hard disk, click on the Ok button.This will also close the
Scanner Calibration panel.

15.7.3. Measure vertically at 440 V scan size

1. Return to the image of the calibration reference. Clear the horizontal line drawn
in Section 15.7.2 above (click the right mouse button, or click on Clear), then draw
a vertical line between features. After waiting for at least three full scans (to allow
the piezo to stabilize), select two widely spaced features and draw the line from like
portions of features (top edge-to-top edge, etc.). The SPM will display the calculated distance between features.
2. Check to see whether the microscopes calculated distance agrees with the
known vertical distance. If there is significant disagreement between the two, fine

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tuning will be required; go to step #3 below. If the displayed distance agrees with
the known distance, skip to Section 15.7.4 below.
3. Based upon the results in step #2 above, perform the following calculation:

Known distance between features

----------------------------------------------------------------------------------------------------SPM-calculated distance between features

That is, divide the known distance by the distance displayed next to the line drawn
in step #2 above. Write this value down.
4. Click on the Real time / Microscope / Calibrate / Scanner function to display
the Scanner Calibration dialog box. Select the Y slow sens parameter.
5. Write down the Y slow sens value shown on the Scanner Calibration panel.
Multiply the quotient obtained in step #3 above by the Y slow sens value shown on
the Scanner Calibration panel, then enter the new value. This should adjust the
scanners slow axis to more closely match calculated distances with actual feature
distances. To save the new parameter value, click on the Ok button.

15.7.4. Measure horizontally at 150 V scan size

1. Set the Scan size parameter on the Scan Controls panel to one-third the maximum (150 volts). Verify that the Scan angle is set to 0.00 degrees, and that Units
(Other Controls panel) is set to Volts. Select two widely-spaced features on the
sample image of known separation, then use the mouse to draw a horizontal line
between them. (For example, on a 10-micron, silicon reference, draw the line from
the left side of one pit to the left side of another pit as far away as possible.) The
microscope will display the measured distance next to the line.
Now check to see whether the microscopes measured distance agrees with the
known horizontal distance. If there is significant disagreement between the two,
fine tuning will be required; go to step #3 below. If the displayed distance agrees
with the known distance, skip to Section 15.7.5.
3. Adjustments may be made in one of two ways. The first method uses to trial and
error to dial in in the correct value. The second method calculates a precise correction.

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Trial and error method Go to the Real time / Microscope / Calibrate /

Scanner function to display the Scanner Calibration dialog box. Select the X
fast derate parameter (or Y fast derate for Y-axis adjustment). If the measured
distance is less than the actual distance, decrease the X fast derate parameter
slightly (or Y fast derate for Y-axis adjustment) and re-measure image features.
Adjust deratings up or down until measurements accord with known feature
distances.

Calculation method Perform the following calculation:

a
s ---- [ s d ( 440 v ) ]
m

-------------------------------------------------------------440 v

Where s is the Sens value; a is the actual distance; d is the derating value; m is the
measured distance; and, v is the Scan size in volts.
4. Click on the Real time / Microscope / Calibrate / Scanner function to display
the Scanner Calibration dialog box. Select the X fast derate parameter.
5. Write down the X fast derate value shown on the Scanner Calibration panel.
Multiply the value obtained in step #3 above by the X fast derate value shown on
the Scanner Calibration panel, then reenter the new X fast derate value. This
should adjust the scanners fast axis to more closely match calculated distances
with actual feature distances. To set the new parameter value, click on the Ok button.

15.7.5. Measure vertically at 150 V scan size

1. Select two widely-spaced features on the sample image of known separation,
then use the mouse to draw a vertical line between them. (For example, on a 10micron, silicon reference, draw the line from the top edge of one pit to the top edge
of another pit as far away as possible.) The microscope will display the measured
distance next to the line.
Now check to see whether the microscopes measured distance agrees with the
known vertical distance. If there is significant disagreement between the two, fine
tuning will be required; go to step #3 below. If the displayed distance agrees with
the known distance, no further calibration is required.
2. If the displayed distance does not agree with the known distance, perform the
calculation shown in Step #3 above to make a correction.
3. Click on the Real time / Microscope / Calibrate / Scanner function to display
the Scanner Calibration dialog box. Select the Y slow derate parameter.

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4. Write down the Y slow derate value shown on the Scanner Calibration panel.
Multiply the value obtained in step #2 above by the Y slow derate value shown on
the Scanner Calibration panel, then enter the new value. This should adjust the
scanners slow axis to more closely match calculated distances with actual feature
distances. To set the new parameter value, click on the Ok button.

15.7.6. Change Scan angle and repeat calibration routines

As a final step, change the Scan angle on the Scan Controls panel to 90 degrees,
then repeat steps 15.7.215.7.5 above for the following parameters: Y fast sens, X
slow sens, Y fast der, and X slow der. This will ensure the scanner is calibrated
along both the X- and Y-axis.

15.8. Calibrating Z
With respect to obtaining accurate Z-axis measurements, users should be aware that
while it is generally not difficult to obtain accurate X-Y calibration references, it is
much more difficult to obtain accurate Z-axis results. Users should be aware that Zaxis calibration is very sample-dependent. It is not easy to control Z piezo dynamics because the Z-axis does not move at a constant rate, as the X- and Y-axes do during scans. Furthermore, offsets can effect the piezo over a period of minutes. The
platinum-coated, silicon calibration references distributed by Digital Instruments
have 180 nm vertical features which are accurate to within 3 percent and are used
throughout the examples provided within this section. If greater accuracy is desired,
an appropriate calibration standard must be selected, and/or a metrology head
employed using a Digital Instruments Dimension Series microscope.

15.8.1. Engage surface and begin imaging

Set up the microscope for contact AFM imaging. Engage the surface and adjust
Real-time parameters to obtain a good-quality, maximum Scan size image. The
Scan rate should be set to a value of 2.44 Hz and the Number of samples parameter should be set at 256 or 128.
Verify that the Z Center Position value shown next to the image display hovers
around 0 volts. If the Z Center Position value is non-zero, use the Real Time /
Motor / Tip Up and Tip Down buttons to adjust.

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15.8.2. Adjust Scan size

Depending upon the type of scanner employed, adjust the Scan size parameter to
include part of a pit, or up to 1 pit, within the image, along with portions of the surrounding flat area. The image should include Z-axis depths from the highest to the
lowest elevations.
A scanners, when set at their maximum Scan size (440 volts), may image only a
small portion of one pit. Adjust the sample and/or microscope stage until one side
of a pit is visible, along with portions of the flat, rim area around the periphery of
the pit.
Since it may be difficult and/or time consuming to locate a pit in the sample using
an A scanner, an alternate method of locating a pit is to use the Scope mode
option in real time imaging. After engaging on the surface of the sample, set both
Realtime Planefit and Offline Planefit to offset. Go to Scope mode. Watching the
Scope trace diagram, slowly turn the X-Y stage adjustment screws on the AFM
microscope. (Do not turn more than a 1/2 turn in each direction.) When the scanner
tip encounters a pit the Scope trace diagram will display a step in the normally flat
line, see Figure 15.6. Be sure that the Z center position is fairly close to zero (50
V).

Scope Trace
Z range
35nm/div

Scan

Figure 15.6. Scope Trace screen will display a step when the tip encounters
a pit in the reference sample.
After finding the step in the Scope mode screen, click back to Image mode. The
image should now encompass a portion of one pit.
Scanners larger than A can image an entire pit. It is not necessary to change the
Realtime and offline planefits for these scanners.

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15.8.3. Capture and correct an image

Capture an image by clicking on Capture in the Real Time screen, or use the Capture icon. When the image is captured, go to the Off-line screen.
It will be necessary to remove all tilt and scan line errata from the image before
continuing. To remove scan line errata, select Off-line / Modify / Flatten Manual.
The Flatten order parameter in the dialog box should be set to 1. Go to the display
screen, then draw a stopband over the pit as shown here:

If the image encompasses one pit, or a portion of one pit (if you are using an A
scanner), cover as much of the pit as possible with a stopband while leaving the
remainder of the top surface exposed. Click on Execute to complete the flattening
procedure, then Quit the dialog box.

15.8.4. Measure vertical features

With the image corrected, its vertical features may now be measured. This is performed using Bearing analysis so that more data points are utilized.
Select the Off-line / Analyze / Bearing command. Go to the display screen and
draw a cursor box over the entire image.

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To commence Bearing analysis, click on Execute in the display monitors top

menu bar. Height data within the drawn cursor box will be graphed on the display
monitor, and should show two, prominent spikes. These spikes correspond to two
elevations on the surface: the bottom of each pit and the top surface.

Cursor

Depth Scale

Hist Cursor

Stopband

Depth Ref

Zoom

Execute

Clear

Depth [nm]
0.50

124.12 m2
82.266 nm
78.049 m2
62.891
138.24 nm
4.361 m3
4.008 m2
3.229
182.69 nm

200

Box area
Center line av
Bearing area
Bearing ratio
Bearing depth
Bearing volume
Hist area
Hist%
Hist rel depth

Depth [nm]

100

0.25

Bearing Analysis

Cursor: Box

Depth: Auto

2.50 5.00
Hist%

Ref: Peak

7.50

50
Bearing area%

100

Scale: Full

Use the mouse to slide the top (red) line cursor on the Hist% graph to the centerline of the top data spike as shown in the example above. Select Hist Cursor / On
to generate another (green) line cursor; position this one on the centerline of the
bottom data spike. The distance between the two cursors is given at the Hist rel
depth field inside the data box. (Depending upon whether the red cursor is positioned over the top or bottom data spike, the Hist rel depth value may be either
positive or negative. It doesnt matter; take the absolute value.)
If a 10-micron, silicon calibration reference from Digital Instruments has been
used, the Hist rel depth value should be very close to 180 nm. Its variance from
this value gives a good indication of the microscopes measuring error in the Z-axis.
If the value is more than 2% from 180 nm, it will be necessary to make adjustments
(see Section 11.8.5 below); write down the Hist rel depth value now.
To exit the Bearing dialog box, click on Quit.

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15.8.5. Correct Z sensitivity

If the depth of the pit on the 10-micron silicon calibration reference deviates significantly from 180 nm, it will be necessary to correct the Z sensitivity parameter in
the Z Calibration dialog box. Corrections here do not change the voltage applied
to the scanners Z-axis piezo crystal, but affect scaling applied throughout the Zaxis measuring range.
Transfer to the Z Calibration dialog box by clicking on Real Time / Microscope /
Calibrate / Z. The Z sensitivity parameter is listed at the top-left and should be
highlighted. Write this value down now.
Perform the following calculation:
180 nm
----------------------------------------------Hist rel depth value

That is, divide the actual depth of features (180 nm for the 10-micron calibration
reference) by the measured depth (indicated in Bearing analysis by the Hist rel
depth value). Multiply this quotient by the Z sensitivity value in the Z Calibration
dialog box, then replace the value with the product. Click on the Ok button to enter
the new Z sensitivity value.

Note

The numerator value above (180 nm) is for Digital Instruments 10-micron
silicon reference. For other calibration references, set the numerator equal to the
depth of features measured by Bearing analysis. Ideally, calibration references
used should have features with heights comparable to those being imaged and
measured on samples.

15.8.6. Recheck Z-axis measuring accuracy and correct

After steps 15.8.115.8.6 above have been completed, it will prove useful to
recheck the Z-axis measuring accuracy of the SPM. Repeat steps 15.8.415.8.5
above until the required accuracy is obtained.

Note

SPMs leaving Digital Instruments are normally calibrated to within 2 nm of

accuracy using the 10-micron silicon reference. This corresponds to an accuracy
of 1 percent. If greater accuracy is required, use a very high-precision
calibration height standard with features comparable to those being imaged on
samples.
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15.8.7. Calculate Retracted and Extended offset deratings

Note

It is not necessary to perform this procedure on A scanners.

Piezoelectric materials exhibit greater sensitivity at higher voltages. In steps
15.8.115.8.6 above, the Z-axis was calibrated while scanning near the middle of
its voltage range (i.e., Z Center Position ~ 0 V). In this section, the Z-axis piezo
will be calibrated while extended and retracted to offset the increased sensitivity.
1. Engage the surface as described in Sections 15.8.115.8.2.
2. Use the Real Time / Motor / Tip Up button until the Z Center Position reads
100 V.
EXPLANATION: By using the motor to move the tip up, the feedback loop forces
the Z-axis piezo to extend to continue its tracking of the surface.
3. Refer to steps 15.8.315.8.4 above to determine the measured depth of the calibration standard with a 100 volt Z Center Position.
Record the measured depth; it should read 180 nm on a Digital Instruments 10 m
silicon calibration reference (model STS-1800). If the depth measured by the
extended piezo is in error by more than two percent, an adjustment will be required.
4. Click on the Real Time / Microscope / Calibrate / Z option to display the Z
Calibration panel, then click on the Extended offset der parameter.
Perform the following calculation:
(1 + current offset der)

180nm
1
meas. depth

For example, if current offset = 4% and measured depth = 175nm, then:

(1 + .04) 180nm 1 = .0697
175nm
5. Enter 6.97 for the External offset derating % menu item.
6. The procedure for calculating and setting the Retracted offset der is exactly the
same as for the Extended offset der; however, the piezo must be retracted by 100 V.
Repeat steps #2-6 above in this section; however, start by using the Motor Control
panel and the Tip Down button to retract the piezo to a Z Center Position of -100
Volts.
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15.9. Calibration of A Scanners for Atomicscale Measurement

The A scanner is the smallest scanner, with a total travel of approximately 0.4 m
along each axis. Its compact design lends excellent stability for atomic scans, and
requires slightly modified X-Y calibration procedures. These are treated in this section. The procedure for X-Y calibration described below is essentially the same as
those described in Sections 15.7.215.7.3 of this manual; however, they substitute
graphite or mica atoms for the pits seen on silicon calibration references. A similar
procedure is outlined in Chapter 9 of this manual for STM imaging of graphite.
Please note that this procedure applies only to X-Y calibration of atomic-scale
imaging. The Z-axis is calibrated in the normal way using a silicon calibration reference as described in Section 15.8 above.

15.9.1. Prepare sample.

The calibration may be conducted with either highly ordered pyrolytic graphite
(HOPG) or mica. Mica should be used for contact AFM; HOPG for STM. Both
mica and HOPG need to be cleaved to obtain a good flat surface. Cleaving is
accomplished by adhering tape to the surface and pulling it off; this produces a
fresh surface of atoms having a regular lattice.
Place the sample to be used on a puck, then attach to the scanner cap.
2. To obtain contact AFM atomic-scale images, try the following Real Time parameter settings:

Panel
Scan Controls

Feedback Controls

Parameter

Setting

Scan Size

12 nm

X offset

0.00 nm

Y offset

0.00 nm

Scan angle

0.00 deg

Scan rate

61.00 Hz

Number of samples

512

Slow scan axis

Enabled

Z limit

440 V

Integral gain

12.00

Proportional gain

4.00

LookAhead gain

0.00

Setpoint

0V

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Panel

Parameter

Setting

Other Controls

AFM mode

Contact

Input attenuation

1x

Interleave Controls

Interleave mode

Disabled

Channel 1

Data type

Height

Highpass filter

34

Lowpass filter

Part V: Utilities

3. Engage the surface and adjust the Integral gain and Setpoint to obtain a good
image. The Setpoint should be kept low if possible, and the Z Center Position
should be close to 0 V. Notice that the Scan rate is set much higher (~ 61 Hz) for
atomic-scale images, this to defeat some of the noise due to thermal drift.
If difficulty is experienced obtaining an image, Withdraw and try a different site on
the surface, then Engage again. Many users find it easiest to obtain good images
measurements if the sample is rotated until atoms are oriented vertically.
4. Once a satisfactory image is obtained, Capture it. The image should appear similar to the image of graphite shown below. The captured image will be used for the
calibration procedure described in the next several steps.

Figure 15.7. Typical atomic scan of graphite. Note the highly regular lattice
of the atoms. The cursor line describes a distance of 6.66 .

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5. Go to the Off-line / View / Top View option and measure the spacings between
atoms using the mouse. Depending upon whether the sample is graphite or mica,
the spacings should measure as shown below.
A
C
A = 0.519 nm
B = .900 nm
C = 1.37 nm

Atomic spacing for mica.

A
C
A = 0.255 nm
B = .433 nm
C = .666 nm

Atomic spacing for graphite.

Record the spacings between at least ten atoms observed in the captured image. It
will prove useful to take several samples of each measurement and average them to
ensure accurate results. (This can be done quickly by alternatively walking the
cursor line from atom to atom; the average distance will be shown on the bottomright corner of the display monitors status bar.) If the measurements vary by more
than 2 percent from the dimensions shown above, a correction should be made.
6. Correction of the X- and Y-axis is essentially the same procedure as described in
Sections 15-7.215-7.3 of this support note and will not be repeated here. The
only significant difference is that the known distances must be adjusted for the
smaller, atomic spacings of the atoms. Furthermore, only the sensitivity parameters
are adjusted for atomic-scale imaging; namely:

X fast sens at 0 Scan angle

Y slow sens at 0 Scan angle
Y fast sens at 90 Scan angle
X slow sens at 90 Scan angle

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The derating parameters are not adjusted for atomic-scale imaging, including:

X fast derate
X slow derate
Y fast derate
Y slow derate
Retracted offset der
Extended offset der

As referenced in Section 15.7.9, the sensitivity parameters must be calibrated with

the Scan angle set at both 0 degrees and at 90 degrees.
7. Z-axis calibration is done in the normal way, using a silicon calibration reference. Refer to Section 15.8 for instructions on calibrating the Z-axis.

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15.10. Troubleshooting the MultiMode SPM

Depending on the operating mode being used, the symptoms and subsequent resolution may vary. For this reason, problems listed in this section are divided into contact AFM and TappingMode. STM problems are described in Chapter 9 of this
manual.
Some of the problems and cures associated with contact AFM are also relevant to
TappingMode. If problems occur, it may be helpful to read through the Contact
AFM problems and vice-versa. The most common problem while operating in TappingMode is due to unusual resonance peaks in the Real Time / View / Cantilever
Tune command. Double peaks in the resonance curve can be caused by improper
seating of the cantilever or a fracture in the cantilever. In general, bad cantilevers
produce strange resonance curves, so the first thing to do when an unusual resonance curve occurs is to clean the groove on the cantilever mount and reseat the
cantilever. If this does not improve the resonance curve, install a new cantilever.

15.10.1. Contact AFM: False engagement

The main cause of false engagement is optical interference on the photodiodes,
which causes the vertical deflection (A-B) voltage to slowly move toward the setpoint voltage. Once the vertical deflection voltage reaches the setpoint voltage, the
feedback loop assumes the tip has contacted the sample.
The source of the optical interference comes from either: i) the reflective gold coating on the cantilever, allowing some of the laser spot through and onto the sample
surface; or, ii) stray laser light from the main beam interacting with the surface
directly, causing optical path length related interference. The direct substrate reflection is more of an issue with reflective substrates that have large steps or topography. These effects can cause scattered light to be reflected onto the photodiode
assembly along with the reflected beam from the back of the cantilever. The scattered light causes changes in the vertical deflection (A-B) voltage as the AFM head
is lowered to the sample during engagement.
IMPORTANT! If a false engagement occurs, it can be detected easily by adjusting
the Setpoint and observing the Z Center Position change. Increasing the Setpoint
voltage by 1 volt should cause the Z Center Position to change by 15 volts. If
the Z Center Position changes by a large amount (1020 volts), the system is
false engaged.
It is a good habit to watch the vertical deflection (A-B) differential voltage while
the tip is engaging. The voltage should ideally jump (not drift slowly) from some
negative value to the setpoint voltage. If it drifts slowly it means that reflected light
is affecting the photodiode voltage. If this is the case, the engagement process can
be aborted with the Esc key. The photodiode position should be adjusted to make

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the Vertical Deflection voltage more negative than the setpoint voltage before trying
the engage sequence again.
Sources of false engagement include:

Incorrect optical alignment of laser spot on cantilever. This alignment will cause
a greater amount of laser light to reflect off of the sample.

The sample has a region on it that touches the cantilever before the tip does.
Foreign material stuck on the cantilever beam that is lower than the tip.
Check the cabling between the computer and the controller, and between the
controller and the microscope. Any discontinuity in the microscope signals can
cause an immediate engage.

The Setpoint may be set more negative than the vertical deflection (A-B)
voltage (this applies only to contact AFM modes). This false engagement is
immediate and the computer will not show any motor travel or time delay after
one gives the command. To correct for this condition, select Withdraw and
check that the vertical deflection voltage reads a voltage more negative than the
setpoint voltage.

15.10.2. Contact AFM: Head appears engaged but does not track
surface features
Occasionally, the head appears to be engaged but surface features do not appear on
the display monitor. This usually results from false engagement (see Section 15.1.1
above), poor laser alignment, or something other than the tip coming in contact
with the sample surface.
An easy way to check for laser alignment problems is to check the laser beam using
a magnifier or slip of paper. Click on the Withdraw command to remove the cantilever from the surface and recheck alignment with the magnifier or paper method
(see Chapter 5). When satisfied with the alignment, readjust the top-bottom differential signal before re-attempting engagement.
Occasionally, when the optical head is not leveled properly, something other than
the cantilever tip (usually the corner of the substrate or the cantilever clip) will contact the surface during engagement. The system may engage, but the image will not
contain any features. Testing the SUM signal after withdrawing the tip several times
is a good test for this failure mode. Generally, the SUM signal will be far from its
original value if something other than the tip contacts the surface. The head should
be leveled and the laser realigned if this has occurred.

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15.10.3. Contact AFM: Head does not engage

The complementary problem to false engagement is not engaging at all. Here are
some common causes of this problem:

The tip may have started too far from the sample. Lower the tips height above
the sample surface by using the coarse alignment screws, then repeat the
engagement procedure.

The laser may be misaligned and/or the cantilever may be broken. When this
occurs, replace the cantilever substrate, realign the laser, and repeat the
engagement procedure.

15.10.4. Contact AFM: Head engages immediately

If the microscope engages immediately after the Engage icon is selected, the problem may be one the following: 1) The Setpoint may be lower than the feedback
voltage. Select Withdraw a few times and verify that the upper DVM reads a negative voltage of -1.0 to -4.0 Volts. Adjust the Setpoint to zero or slightly above and
try to engage again. If the microscope still engages immediately, check the cabling
between the computer and the NanoScope controller and also between the controller and the microscope. Any discontinuity in the voltage feedback will cause an
immediate engage.

15.10.5. Contact AFM: Displacement of material

This is generally caused by too much tracking force. Use the Force Calibration
window after engagement for setting the correct tracking force.
The AFM can be tuned to operate in the attractive region of the force curve. This
will take advantage of the fluid layer which captures and holds the tip to the sample.
This effectively reduces the tracking force. Be aware of the fact that this means the
tip is pulling away from the sample. This operating condition might cause the tip to
pop off of the sample surface.

15.10.6. Contact AFM: Lines in the image

Lines can be caused by:

AFM tip picking up contamination. The tip will effectively become longer and
this will cause the feedback loop to raise the tip to keep the same tracking force.
The contamination can come off of the tip which will cause another level shift in
the image. This problem will show up as large bands in the captured image.

Friction. Some samples have a stronger frictional interaction with the tip than
others. The cantilever will bend and straighten due to the tip sticking and
slipping as it is dragged across the surface of the sample. The result is a line-by-

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line level shift in the captured image. The trace and retrace scan directions can
actually be inverted from each other if the friction is high enough. A good
practice is to use the scope image mode in dual trace display. The trace and
retrace directions should be close to each other. Trace and retrace can invert if
there is friction present between the tip and the sample surface.

15.10.7. Contact AFM: Problems with silicon nitride cantilevers

Sometimes nitride cantilevers can be a problem due to lateral warping or torquing
of the nitride beams. This causes the reflected light to spill off to the side as the tip
begins to engage the sample. Warping or torquing of the cantilever is associated
with some older cantilever wafers. If engagement does not work the first time, try
changing the actual lever used, i.e., go to the next lever on the same chip. Usually,
the wide 200 m-long lever has the most lateral warping. If this is the case, try the
wide, short cantilever next to it. Generally, the narrow-legged silicon nitride cantilevers (both of which are on the same side of the chip) will have difficulties with the
laser optics due to laser beam spillage over the side of the cantilever. This effect is
more pronounced for samples which are highly reflective.
Using a microscope that has an interferometric objective lens, it is possible to
observe five or more contour lines following the length of the legs of the cantilever
on a warped cantilever probe. Cantilever probes which are not warped will have
contour lines parallel to the substrate edge. Nikon sells interferometric objective
lenses for their Optophot and similar microscopes (such as the MPlan 40(x) DI 0.5
210/0). This is a recommended lens for observing contour lines on the cantilever for
diagnostic purposes. It is beneficial to use a bandpass color filter with this lens.
Please consult Nikon for further information.

15.10.8. Contact AFM: Image vertical dimensions are not correct

1. When invoking the Highpass filter, height information will not be accurate. The
Highpass filter removes the DC component of scan information. This will invalidate
the height information in the image.
2. The Sensitivity parameter must be calculated (as described in Chapter 6) or
deflection data will be inaccurate.

Note

The gains must be set low to reduce movement of the Z piezo when acquiring
deflection data used in height measurements.

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15.10.9. Contact AFM: Z Center Position goes out of range

The Z Center Position voltage is a measure of the average voltage to the Z electrode. The image will disappear when the Z center position reaches either the fully
extended or the fully retracted ends of the Z center indicator. Possible causes
include:

Having the Z limit too low.

Tilted sample. The sample should be as level as possible, particularly for larger
scans, because tilt in the sample can cause the Z scan to run out of range.

Mechanical drift will cause the sample-to-tip distance to change slowly bringing
them apart completely, or too close together. If this is the case, the Z center will
show either +220 (extended) or -220 (retracted), respectively.

Drift in the optical path

Differentiating between optical path or mechanical drift is the first step in eliminating this problem. The force curve is a very useful tool for this purpose. Go to the
force curve immediately after engaging. The force curve has two main regions: the
sloping regions when the sample is in contact with the tip, and the flat region when
the tip is free. Intersection of these two regions is what is important. Watch the
force curve and determine whether the curve drifts vertically or horizontally; vertical drift is indicative of optical path drift, while a horizontal drift is due to a
mechanical change in tip-to-sample separation.
Use the following as first steps in correcting drift:

Verify that the sample, tip and stage are all stabilized. There should be no free
movement between any of these components

Recheck that the cantilever is firmly seated in its place and that there are no dirt
particles wedged beneath it. Check that everything is tight and secure. Once this
is checked, there may still be some drift. Using the Tip Up and Tip Down
command can bring the sample back into range. (This may have to be done due
to any number of factors.)

Check for thermal stability. The SPM should not be located directly in the path
of heating or air conditioning ducts; also, avoid locating the SPM near large
windows which trap solar heat. Thermally caused drift due to thermal expansion
of SPM components is the most common cause of mechanical drift. The
MultiMode tends to heat up and drift when used with the acoustic isolation hood
because it traps heat produced by electronics in the base and head.

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15.10.10. Contact AFM: Poor image quality

If the tip is engaged with the upper DVM reading a stable, near-setpoint value and
the Z center position is not overly sensitive to small changes in Setpoint, then laser
alignment is probably good and the tip is scanning the sample. If image quality is
poor with distorted shapes and low contrast, try adjusting the gains first, then optimize the scan direction to take advantage of the best tip shape to improve image
quality. Vary the Scan angle parameter in the Scan Controls panel and see if this
will help clean up the image. There is some variation in the shape of tip from substrate-to-substrate and the tip shape can affect the engagement process. (For example, a blunt tip may tend to engage falsely.) Therefore, changing the angle at which
the tip scans some surfaces may have a significant effect.
Other scan parameters may also have a significant effect on the image quality. Varying the Scan rate, X and Y offsets, filtering, feedback gains and ranges all may
improve the image (or make it worse!). Once engaged, adjust parameters in the
Scan controls panel to improve the image quality. It is unlikely that adjusting the
parameters will damage the tip unless the feedback gains are set too high, causing
severe oscillations of the tip. In general, the Scan rate should be lower for large
scans and for samples having tall features. The Scan rate can be increased on flat
samples.
The offsets and zoom commands should be used to locate good clean regions on the
sample. Filtering can improve atomic-scale images, but it is usually better to go
without filtering on larger scans. Highpass filtering will distort the height information in all but atomic scans. For height data, the Integral and Proportional gains
should be high but not high enough to cause oscillations. For deflection data, the
feedback gains should all be low (close to zero). LookAhead gain should only be
used for samples with regular features oriented along the slow axis. The user is
encouraged to review the descriptions of all the parameters in the Command Reference Manual and to experiment with parameters on a known sample.
Selecting a large Scan size and a high scan rate for a few scans can sweep an area
clear. Decreasing the Scan size to image within the swept area can improve the
quality of atomic images.
Finally, adjust the force exerted on the sample. Engagement requires a positive
deflection of the cantilever, but the microscope will operate at much lower forces
and lowering the force sometimes improves the image quality. Either use the force
calibration to set the force or lower the Setpoint in small increments.

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15.10.11. Contact AFM: Force Calibration command does not seem to

work
Most often, the Force Cal. command will not provide a meaningful display, when
first invoked. Z scan start and Z scan size as well as Setpoint affect the position
and shape of the curve, and will probably require adjustment to achieve a useful
display. The negatively sloped sensitivity line should, however, always be straight
for a proper force curve.

15.10.12. Contact AFM: Image vertical dimensions are not correct

When collecting deflection data or invoking the Off-line / Highpass filter, height
information may not be accurate. The Highpass filter removes low frequency information from the scan. This can distort the height information in the image. The
Sensitivity parameter must be calculated properly or deflection data will be inaccurate. The gains must also be low to reduce Z-axis movement of the piezo. Even with
the sensitivity properly calibrated and the gains as close to zero as possible, height
data is more accurate than deflection data if the feedback gains are properly
adjusted.

15.10.13. Contact AFM: Z Center Position goes out of range

The sample should be as level as possible, particularly for larger scans, because tilt
in the sample can cause the Z scan to run out of vertical range.

15.10.14. Contact AFM: Image goes white

If, when using an A scanner, the image goes white after a couple of scans and the
Z center voltage is still within range, check the Real Time Planefit parameter on
the active Channel panel. When using an A scanner, it should usually be set to
Line or Offset. In general, this will be a problem anytime there is a significant
amount of drift in the Z center voltage, but drift is especially prevalent with A
scanners.

15.10.15. TappingMode: Streaks on the trailing edge of surface features

Streaks are an indication of the tip not tracking the surface due to either: 1) insufficient tapping force; 2) an excessively fast scan rate; or, 3) gain values set too low.
Streaking may also result from any combination of these factors.
Try the following procedures to eliminate this condition:

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Reduce the setpoint voltage. This increases the amount of tapping force on the
surface. This is probably the thing that will be most effective. Be careful when
doing this on soft samples. The sample surface can still be disturbed even
though the forces are very small.

Reduce the scan rate. The scan rate needs to be slower in TappingMode than in
contact AFM. Typically it should be around 1-3Hz.

Increase the integral and proportional gains. This will speed up the response
time of the Z piezo transducer.

15.10.16. TappingMode: Lines across the image

Lines oriented in the fast scan direction can be caused by the tip sticking to the surface. This condition may be remedied by increasing the RMS voltage. Working
with a larger RMS has the effect of giving the tip more energy to pull off of the surface. To correct this condition, try the following approach:
1. Use arrow keys (p) to increment the Setpoint voltage positively. Do this while
monitoring the Z Center Position voltage on the display monitor. Increase the Setpoint voltage until the Z Center Position voltage jumps to the fully retracted position.
2. Note the current Setpoint voltage value. This value is just slightly greater than
the RMS voltage currently used.
3. Increase the Setpoint voltage another 2 volts.
4. Use arrow keys to increase the Drive amplitude (press 2-3 times). This will
increase the RMS voltage output from the microscope. (Increasing the RMS voltage means the cantilever is oscillated harder, making it less subject to capture by a
sticky surface.)
5. Use arrow keys to reduce the Setpoint voltage until the Z Center Position voltage begins to move away from the retracted position. Continue to reduce the Setpoint voltage until the topographic image on the display monitor pops into clear
view.

15.10.17. TappingMode: Rings around features on the surface.

This effect might also be described as the image looking as though it is half submerged beneath water. This is caused by operating with a drive frequency too close
to cantilever resonance.
Use the arrow keys to increment the drive frequency a little lower. Do this while
watching the Real Time scan. Be aware that the RMS voltage might also reduce.

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Repeat the steps in the lines across the image troubleshooting description to
adjust the RMS voltage.

15.10.18. TappingMode: Multiple or repeating patterns

The tip is probably chipped. This is usually caused by using too much tapping force
on the surface, or because the tip encountered a feature too high to successfully
traverse. Solution: change the tip.

Notes

Operating with a smaller difference between the RMS voltage and the Setpoint
voltage means that less tapping force is being used. This may damage the tip
because the tip may not be following the surface, allowing it to crash into
vertical features.

15.10.19. TappingMode: Image goes white or black

If the image goes white or black after a few scans and the Z Center Position voltage is still within range, check the Off-line Planefit sub-command on the control
monitor. Off-line Planefit is normally set to Full. (See full description of the Offline Planefit command in Digital Instruments Command Reference Manual.

15.10.20. Fluid Imaging: Image drifts.

Occasionally, there may be some image drift due to the o-ring (used to contain
fluid) sliding across the sample surface. To reduce movement of the o-ring, the fluid
cell needs to be set up such that there is minimal lateral movement of the SPM head
with respect to the sample once the o-ring is installed. This is best accomplished by
keeping the head level and positioning the tip as closely as possible to the surface
before installing the o-ring so that the lateral movement of the tip during engagement is minimized. Also, moving the positioning screws at the bottom of the optical
head should also be minimized once the o-ring is installed. Further suggestions for
solving this problem consist of the following:

Use the fluid cell without the o-ring as described in Chapter 7 of this manual.
This technique works best on hydrophobic surfaces. If you have a surface that
does not allow a liquid drop meniscus to form or stabilize (e.g., mica), a water
repellant marker may be used to outline a boundary for holding the drop. This
type of marker, the PAP PEN, can be purchased from the The Binding Site,
5889 Oberlin Drive #101, San Diego, CA 92121; 1-800-633-4484; Fax: 619453-9189.

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Notes
For applications where fluid flow is necessary, this option should not be used.
Be certain to check for leaks and wipe up any spilled fluid as soon as possible to
avoid damage to the scanner.

The new vertical engage scanners allow the tip to approach the sample without
the lateral movement caused by the stepper motor. Thus, lateral stress on the oring is absent. Vertical engage scanners are available in the 125-micron (J),
and 10-micron (E) sizes. Contact Digital Instruments for more information.

Lightly coating the area of the o-ring which contacts the sample surface with
white petrolatum or vacuum grease will allow the o-ring to slide across the
surface, minimizing lateral stress. This also forms a better fluid-tight seal
between the o-ring and sample. Be aware that some solvents (e.g., non-polar
organic solvents) may dissolve some lubricants into the fluid.

Replace the o-ring with a slice of thin-walled glass, plastic, or stainless steel
tubing. The diameter and thickness of the ring of tubing should be chosen to
prevent contacting the inner or outer walls of the curcular groove in the glass
cantilever holder. This gives the head more room to move laterally during
engagement and for positioning the tip over the sample surface. The height of
the ring of tubing must be chosen so that it is not too tall to prevent the tip from
reaching the sample surface, or so short that the ring does not reach the bottom
of the glass cantilever holder before engagement. Glue the ring of tubing to the
steel sample puck or to the sample to prevent leaks.

Notes
When using the ring of tubing in the fluid cell, fluid cannot be circulated
through the cell as when using the supplied o-ring.

When positioning the o-ring on the surface, adjust the positioning knob at the
base of the head to move it slightly forward. This will counter some of the
lateral stress on the o-ring due to the head shifting rearward during engagement.
To prevent leaks when using the supplied o-ring, it is best to place the o-ring on
the sample before placing the head on the scanner.

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15.11. MultiMode SPM Adjustment Screw

Maintenance Procedure
This section covers maintenance procedures for adjustment screws used on Digital
Instruments Small Sample microscopes. These screws are used to support and position the head relative to the scanner, and must be cleaned periodically to ensure
smooth operation. Instructions for the removal, cleaning, lubrication and replacement of adjustment screws are included in this section. A schedule of inspection
and service is recommended at least every three months.
If adjustment screws are inspected and cleaned regularly, they should last the life of
the scanner without replacement. Contamination of the screws with grit depends
heavily upon the operating environment, types of material(s) being scanned, and
operator handling.

15.11.1. Inspection
Small Sample SPMs utilize fine-pitch (1/4-80) adjustment screws; in some scanners, two of them are manually turned, and a third (rear) screw is turned by a motor
located in the microscope base. The Vertical Engagement JV scanner has just one
adjustment screw. The diagram below illustrates a screw and adjacent hardware
installed on later-model (post-August 1993) microscopes. Earlier models have their
brass threaded inserts installed at the top of the scanner body (rather than the bottom) and feature a Teflon bushing. Inspection and service is similar for all types.
(top)
(Scanner body)

Ball Bearing

Setscrew (applies
pressure to bushing)
Plastic bushing

Brass threaded insert

Screw

Screw hole (on 3-screw models)

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Adjustment screws are threaded into brass inserts, which are affixed to the scanner
body with epoxy. Although screws are not heavily lubricated, a light film of oil is
applied to them at the factory to prevent galling. This allows sufficient lubrication
for fine adjustment, while minimizing drift (i.e., loosening) between the screws and
scanner body due to the slow displacement of lubricant from screw threads.
Problems develop whenever screws become fouled with fine grit: screws may be
difficult to turn and/or exhibit any of the following symptoms:

Eccentric, rotational limp (i.e., alternatively easy, then difficult to turn).

Faint, crunching or grinding noises when rotated.
Microscope cannot engage sample surface, i.e., motor is unable to rotate rear
adjustment screw.
If any of these conditions are noted, screws should be backed out and cleaned as
described below.

Notes

If screws are frozen (i.e., cannot be rotated), DO NOT attempt to force them!
Return the scanner body and screws to Digital Instruments for repair.
The user should inspect screws at least every three months, more often if possible.
It is a good practice to check screws whenever the scanner body is removed by turning manually and feeling for resistance. This is especially true of the rear, motoractuated screw, which may be fouled without the users notice.

15.11.2. Remove adjustment screws.

To remove adjustment screws, do the following:
1. Remove SPM head and disconnect the scanner body from the Small Sample base
by pulling its cable connector straight up. Hold the scanner body firmly in your
hand.
2. Gently turn each screw to check for resistance. Turn counterclockwise until
backed out of its screw hole. If resistance is experienced in turning the screw, stop,
rotate briefly in the opposite direction, then retry. If resistance is experienced on
later-model scanners, loosen the setscrew which applies pressure to the plastic
bushing (see diagram above), then try again.
3. If screws are frozen (i.e., cannot be rotated at all), DO NOT attempt to force
them. Return the entire scanner body and screws to Digital Instruments for repair.

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15.11.3. Inspect for physical damage.

Adjustment screws are made of hardened stainless steel; threaded inserts are made
of a much softer brass. If a screw becomes fouled with hard grit it may bind against
the threaded insert. If the bound adjustment screw is forcefully rotated, the screw
will almost always destroy the brass insert: threaded inserts may become crossthreaded, or stripped entirely of threads. If this occurs, they will have to be pressed
out and replaced; return to Digital Instruments for repair.
1. Once screws are removed from the scanner body, they may be washed using
methanol. Do not use strong solvents such as methyl chloride, MEK, benzene, etc.
Use a fine brush or swab to remove grit from between threads and shoulder.
Observe caution around rubberized knob surfaces; certain solvents may dissolve
them! Be sure to remove all grit from surfaces; air dry.
2. Use a swab stick (e.g., Q-tip, Puritan swab, etc.) to carefully clean grit from the
threaded brass inserts. Be sure to remove all grit from threads; air dry.
CAUTION! Do NOT splash solvent on the scanner tube or wiring at the center of
the scanner bodycertain components (e.g., wiring insulation) may be dissolved,
causing scanner failure!
ATTENTION! Ne pas clabousser le tube en cramique pizo-lectrique ou le
montage lintrieur du tube avec un solvant. Certains composants pourraient tre
dissous, entranant une dfaillance du tube.
WARHINWEIS! Verwenden Sie keine Lsungsmittel auf dem Scanner-Rhrchen
oder den Kabelanschlssen am Piezo - manche Komponenten (z.B. Isolation der
Anschludrhte) knnten sich auflsen und eine Fehlfunktion des Scanners nach
sich ziehen.
3. Carefully inspect surfaces for signs of wear or damage. If small burrs are visible
inside of the threaded brass inserts, they may removed by gently sanding with fine
emory cloth, then recleaned using a swab and solvent. If threads are cross-threaded
or stripped, the unit will have to returned to Digital Instruments for repair.

15.11.4. Clean guide bushings.

Plastic guide bushings are installed to stabilize screws and increase rigidity. Tolerances between screws and bushings are very tight, necessitating removal of all grit.
Use a swab and methanol as described above to clean bushings thoroughly.

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Notes

It is not necessary to remove setscrews from the scanner base to clean bushings.
(Setscrews are used only to apply pressure to the shoulder of each adjustment
screw; see diagram above.) If setscrews are removed, they should be retorqued
to approximately 4 in/oz., or until the adjustment screw can be turned snugly
without binding.

15.11.5. Lubricate.
Apply a very fine layer of lubricant to each adjustment screw. Lubricant may consist of high-vacuum grease, optical coupling grease, or equivalent. Screws should
exhibit a slight sheen and no more, indicating that they have been finely coated.

Notes

Excessive use of oil and grease on screws can cause the head to drift slightly.
This is due to a slow displacement of lubricant between the screw and threaded
insert. As lubricant is slowly squeezed out between the screw and threaded
insert, the screw settles, causing the head to lower itself (and the tip) toward the
sample. This is especially apparent during atomic-resolution imaging.

15.11.6. Reinstall.
1. Verify that all screws, threaded inserts and plastic bushings are free of grit.
2. Replace adjustment screws in their threaded inserts. Carefully turn them down
clockwise until the shoulder of the screw engages the plastic bushing, and the
screws ball bearing appears at the top of the scanner body.

Notes

If screws bind during reinstallation, stop immediately. Back the screw out again,
reclean as described above, then redo installation. Recheck that the setscrew is
properly torqued at the plastic bushing. If screw still cannot be installed without
binding, return to Digital Instruments for repair.
3. Verify that each screw turns freely in both directions, but feels snug. (Adjustment
screws should turn freely while exhibiting sufficient rigidity to stabilize the head.)

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15.12. Vertical Engagement ScannersInstallation, Use, and Maintenance

Digital Instruments now offers E and J scanners which permit vertical engagement without significant lateral movement. The vertical scanners feature the following:

Completely motorized tip-sample engage.

Fully vertical engage head does not tilt.
Easy to locate tip on desired scan area.
0.5 m lateral repeatability on subsequent engages.
Accommodates samples up to 8.0 mm thick.
Integrated fluid seal at top of scanner resists fluid spillage.
Retaining springs mount permanently to scanner body.

Your vertical scanner should come shipped with the following:

MMAFMJ.PAR (J scanners) or MMAFME.PAR (E scanners) parameter

file on diskette1.

Stabilizing screw, P/N AFM-SCN-579

Stabilizing screw, P/N AFM-SCN-580
In addition, you will require a calibration reference, such as a P/N STR10-180.

15.12.1. Hardware Installation

Installation of the vertical scanner is very similar to earlier models. To install the
vertical scanner, do the following:

15.12.2. Remove old scanner.

If the SPM is engaged, disengage the sample by clicking on the Withdraw icon
several times. Unplug and remove the SPM head from the microscope. Remove the
sample, then unplug and remove the old scanner body.

1. Parameter file name may be labeled with scanners serial number (e.g., 1234JV.PAR).

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15.12.3. Install vertical scanner.

Set the vertical scanner atop the MultiMode AFM or LFM support ring with the
scanners leadscrew at the back. The leadscrew should slip into the flexible coupling. If the leadscrew does not seat completely into the coupling, toggle the Tip
Up-Down switch on the microscope base; this will rotate the coupling until the
leadscrew seats.
Plug the vertical scanner cable into the receptacle on the left-rear edge of the support ring.
Secure the scanner to the ring using one of two screws supplied (see Figure 223-1
below).

Figure 15.8. Stabilizing screw for securing the vertical scanner to the
support ring. MultiMode AFM screw (left), and screw for other SPMs
(right).
One screw is supplied with a longer shoulder (P/N AFM-SCN-580); this screw
should be used with all MultiMode SPM bases. Use the short-shouldered screw
(P/N AFM-SCN-579) for all other SPM models. The screw is inserted through a
small hole on the front-underside of the support ring. Turn the screw until snug; do
not overtighten.
IMPORTANT! The use of a fastening screw is necessary to ensure optimal system
resolution and noise-free operation. DO NOT attempt to operate the scanner atop
the support ring without a fastening screw!

15.12.4. Install parameter file.

The vertical scanner is shipped with a diskette containing its corresponding parameter file; this parameter file must be loaded into the computers EQUIP directory.
To load the file, exit the NanoScope software, then place the diskette into the floppy
disk drive. Locate the EQUIP directory on the computers hard drive, then transfer
to it (e.g., CD \EQUIP).

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NOTE:
There may be more than one \EQUIP directory, especially if the SPM uses more
than one version of the NanoScope software. If so, copy the file to ALL directories
and sub-directories labeled EQUIP.
The parameter file may be copied with any name, as long as it includes a .PAR
extension. Make certain the vertical scanners parameter file name is not the same
as a preexisting file; otherwise, it will overwrite the preexisting file. The parameter
file is copied using a DOS command. For example, for a J scanner:
COPY B:\MMAFMJ.PAR C:\EQUIP\1234JV.PAR
Once the parameter file is copied, reboot the NanoScope software to resume.

NOTE:
The vertical scanner parameter files are identical to all other J and E scanner
parameter files except for the Motor sensitivity parameter. On vertical scanners
this parameter value is larger than older models. A summary of Motor Sensitivity
parameter values is provided below.
Motor Sensitivity parameter value
(Tip travel per half step)
AFM, LFM,
TipView STM

MultiMode AFM

Vertical Scanners

80

110

3-screw Scanners

19

26

15.12.5. Select scanner.

Transfer to the Real Time / Microscope / Select panel. Click on the J or E
button within the Scanner selection box, depending upon whether a J or E
scanner is to be installed. If another J or E scanner parameter file already exists
in the \EQUIP directory, both choices will be presented. Select the newly copied
parameter file, then click on the panels Ok button to exit.

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15.12.6. Inspect scanner.

Load a calibration reference (e.g., P/N STR10-180) on the MultiMode SPM,
engage the surface and obtain an image. Verify that the scanner is working properly,
and take a series of measurements on the calibration reference to ensure accuracy.
If the calibration reference is not measuring accurately, it may be necessary to calibrate software parameters to ensure measuring accuracy. This calibration procedure
is detailed in the latest revision of Support Note 217, Calibration Procedures. Follow instructions provided in this document to properly recalibrate your vertical
scanner.

15.13. Troubleshooting
15.13.1. Scanner is not properly calibrated.
Verify that the scanners parameter file has been properly copied to each of the
computers \EQUIP directories. Check the parameter file name; it should include a
.PAR extension (e.g., JVSCANR.PAR). Try to reselect the scanner using the Real
Time / Microscope / Select panel.
If the parameter file is correctly selected but measures inaccurately, it may be necessary to calibrate the scanner. This calibration procedure is detailed in the latest
revision of Support Note 217, Calibration Procedures.

15.13.2. Sample will not move (Tip Up/Down switch doesnt work).
If the vertical scanner is adjusted to its maximum tube height, the leadscrew may
disengage from the motor coupling on the MultiMode base. (This is a built-in feature to prevent motor burn-out.) To reengage the leadscrew, remove the scanner
from the support ring, then manually back the screw out several turns. Replace the
scanner on the support ring and reattempt motorized movement.
If the leadscrew becomes fouled with grit, rotation may become difficult or impossible. To inspect, remove the scanner from the support ring and turn the leadscrew
manually while feeling for resistance. If the leadscrew resists rotation, it will have
to be backed out, cleaned with solvent and lubricated. (DO NOT attempt to clean
the leadscrew while in the scanner body; solvents will ruin the scanner circuitry!) A
leadscrew cleaning procedure is detailed in Support Note 216 available from Digital
Instruments.

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NOTE:
If screw is frozen (i.e., cannot be rotated), DO NOT attempt to force it! Return the
scanner body and screw to Digital Instruments for repair.

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THIS IS A BLANK PAGE.

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Index

A
Adjustment Screws
maintenance 15-43
Aliasing 11-37
Amplitude 8-19
Amplitude Calibration 8-25
Average count 11-22
B
Bias 9-11
Bias Voltage 9-1, 9-5, 9-6
C
Calibration
standard 15-6
Calibration Procedures 15-33
cantilever substrates 4-1
Cantilever Tune 8-8, 8-158-20
Cantilever Tune
initial settings 8-9
cantilevers 4-1
Cantilevers. See Probe Tips
Capture 9-12, 11-21
Capture Calibration 15-13
Center Frequency 8-9, 8-10
Color contrast 9-13
Color offset 9-13
Color table 9-13
Component List 3-13-2
Contact AFM
detector offsets 6-1
in fluids 7-1
principles of 2-2815-34
Contact Force 6-14, 8-25, 11-18

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Index-1

D
Data type 6-13, 6-14, 8-19, 8-20, 9-11, 13-8
FM 11-34
LFM 10-1
STM 9-49-5, 9-6
Date type 13-8
Deflection 6-13
Dimension 5000
hardware described 1-2
Dimension 5000 1-1
DNA
imaging with TappingMode 8-41
Drive Amplitude 8-24, 11-24
Drive amplitude 8-10, 8-11, 11-29, 11-31, 11-35, 11-36, 11-37
Drive frequency 8-10, 8-18, 8-24, 11-24, 11-33, 13-8
with MFM 13-4, 14-21
E
ECAFM 7-1
Edge Effects 11-37
EFM 12-112-7, 13-9, 14-2
Electric Force Microscopy See EFM 12-1
Electrochemical AFM 7-1
Engage 8-14, 9-11
Engagement
false 15-35
FM 11-34
STM 9-11, 9-12, 9-13, 9-19
TappingMode 8-13
Error Signal Mode 8-19
F
False Engagement 15-35
Feedback Gains
initial settings 6-13
Feedback type 9-5, 9-7
Fluid Cell
preparation 8-278-31
Fluids, imaging in 7-1
FM See Force Modulation
Force Cal
TappingMode in fluids 8-34
Force Cal 6-13, 6-14, 11-111-12
Force Cal
adjustment 11-10
Force Calibration 15-5
Force Calibration 8-218-26, 11-19
Capture 8-23, 11-24
Drive amplitude 8-24, 11-24
Drive Frequency 8-24, 11-24
Sensitivity 8-24, 11-22
Force Curve 11-4
adjustment 11-511-12

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Force Modulation 11-2511-38

edge effects 11-36
operating procedure 11-2911-37
principles of 11-28
Frequency Modulation
with MFM 13-8
Frequency Sweep 8-8
with MFM 13-6, 14-22
Frictional Measurements See Lateral Force Microscopy
G
Graph range 11-24
H
Hardware
components listed 3-13-2
Hardware Description 1-1
Head
adjustment 8-4
laser aiming 6-1
preparation 5-1
Head 3-2
Height 6-13, 8-19, 8-20
Highpass 8-20, 13-4, 14-20
Highpass Filter 6-15
I
Image Mode 10-5
Input attenuation 8-10, 8-13, 11-23
Installation 3-1
Integral gain 2-272-31, 6-13, 8-13, 8-17, 8-19, 9-11, 11-37, 13-8
Interleave Controls 6-5, 12-112-7, 13-11
Lift scan height 12-5
principles of 12-2
L
Laser Aiming
with fluid cells 7-7
Lateral Force Microscopy 10-1
Left Image 6-6
LFM 10-7
principles of 10-1, 10-6
scan angle 10-2
Lift scan height 12-3, 12-4, 12-5, 13-7, 14-22
Lift start height 12-3, 12-4, 13-7, 14-22
LiftMode 12-112-7
principles of 12-3
with MFM 13-313-4
with TappingMode 12-512-7
Line direction 10-1, 10-5, 12-5, 13-7, 15-9
Look Ahead gain 6-13, 8-13, 9-6
Look ahead gain 8-19
Lowpass 8-20, 9-13, 13-4, 14-20

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Index-3

Lowpass Filter 6-15

Lysozyme 8-38
M
Magnetic Force Microscopy See MFM 12-1
Main Controls 6-4
may 14-24
MFM 12-112-7, 13-9, 14-2
operating procedure 13-413-8
principles of 13-313-4
resolution 13-10
Microscope
Calibrate 8-23
Scanner 15-10
Select 5-22
Modify 9-13
Motor
Engage 6-6
Withdraw 8-15
N
Number of samples 2-27, 11-22
O
Offset 8-10
Other Controls 6-5
P
Plot type 9-13
Probe Tips 4-14-12
EFM 13-3
engagement 6-6
FM 11-27, 11-38
force curves 8-22, 11-4
geometry 4-24-7, 4-114-12, 12-5
LFM 10-3
MFM 13-3
NanoProbe 13-3
removal from substrates 4-1, 4-8
selection 6-116-12
silicon 4-14-7
silicon nitride 4-84-12, 15-36
STM 9-3, 9-9
tuning 8-88-12
Proportional gain 2-272-31, 6-13, 8-13, 8-19, 11-37, 13-8
R
Real-time 5-22
Retrace 8-17
Right Image 6-6
RMS Amplitude 8-5
Rounding 10-5, 13-4, 14-20

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S
Samples
biological 7-18-44
minimizing surface forces 11-10
preparation 5-3, 7-2
Scan angle 10-1, 10-2
Scan direction 13-8
Scan rate 2-27, 6-14, 8-17
Scan size 2-26, 6-14, 9-11, 13-7
STM 9-6, 9-12
Scan speed 11-37
Scanner
calibration 15-33
linearity 15-13
parameters 8-188-24, 11-23
piezoelectric crystals 2-7
Scanner Calibration 15-10
Scope Mode 10-5
Sensitivity 6-13, 8-19, 8-24, 11-22
adjustment 8-23
Sensitivity
adjustment 11-9
Setpoint 6-14, 8-11, 8-16, 8-20, 8-24, 11-23, 11-37
defined 6-14
FM 11-34, 11-35, 11-36
Force Modulation 11-29
STM 9-12
Silicon Cantilever Substrates 4-1
Slow scan axis 2-27
Small Sample SPM
adjustment screws 15-43
Spring Constant
specifications 6-12
STM 9-19-30
applications 9-2
hardware 9-3
principles of 9-1
Sweep graph range 8-10, 11-31
Sweep width 8-10, 11-32
T
TappingMode 8-18-26, 11-19
in fluid 8-268-43
principles of 2-322-34
scanning parameters 8-188-24, 11-23
set-up 5-22
Tip Down 8-23, 11-6, 11-21, 11-24
Tip Holder
installation fixture 5-9
preparation 5-6
STM 9-9
Tip Up 8-23, 11-21, 11-24
to 13-7

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Index-5

Trace 8-17
Troubleshooting 15-41
adjustment screws 15-43
calibration 15-33
cantilever tune plot badloose cantilever 8-43
contact force too high 15-35
control loop explained 2-26
drift during fluid imaging 15-41
loss of Z center position 15-37
no engagement 15-35
poor imagelines 15-40
poor imagerepeating images 15-41
poor imagerings around features 15-41
poor imageslines 15-36
poor imagestreaks on trailing edges 15-40
poor imagevertical distortion 15-37
poor imagewhiteness 15-41
probe tips 15-36
TappingMode in fluids 8-35
U
Units 11-22, 11-23
V
Van der Waals Forces 12-7
View
Cantilever Tune 11-30
Image Mode 9-11
Scope Mode 9-6, 9-11, 10-3
W
Wet Samples
TappingMode 8-44
X
X offset 2-26, 9-11
Y
Y offset 2-26, 9-11
Z
Z limit 2-27
Z scan rate 8-22, 11-15
Z scan size 8-21, 8-22, 8-23, 8-26, 11-2, 11-18, 11-22
Z scan start 8-21, 8-22, 8-23, 8-26, 11-2, 11-18, 11-22
Zoom In 8-10, 11-32

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