1

AP 5301/8301
Instrumental Methods of Analysis
and Laboratory
Lecture 3
Microscopy (II): scanning electron
microscopy & scanning probe microscopy

Prof YU Kin Man

E-mail: [email protected]
Tel: 3442-7813
Office: P6422
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Lecture 3: Outline
 Introduction
 Major components and functions of a SEM
─ Electron guns
─ Magnetic lenses
─ Scanning coils
─ Electron detectors
 Electron-specimen interactions
─ Secondary and backscattered electrons
─ Interaction and escape volumes
 Magnification and resolution
 Images: effects due to different parameters
─ Acceleration voltage
─ Objective lens aperture
─ Electron probe diameter
─ Sample charging
 Scanning probe microscopy
─ Scanning tunneling microscopy
─ Atomic force microscopy
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Scanning electron microscope (SEM)

Column

Sample
Chamber

A scanning electron microscope (SEM) is a microscope that uses

electrons rather than light to form an image. There are many
advantages to using the SEM instead of a OM.
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Optical and electron microscopies: a comparison

Probe

Light source Source of

electrons
Condenser
Magnetic
lenses
Specimen
Objective

Projector Specimen
Eyepiece

detector

Optical Transmission electron scanning electron

microscope microscope (TEM) microscope (TEM)
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SEM: advantages
Magnification Depth of Field Resolution

OM 4 – 1000x 15.5 – 0.19mm ~ 0.2mm

SEM 10 – 3000000x 4mm – 0.4mm 1-10nm

 SEM has a large depth of field

─ allows a large amount of the sample to be in focus at one time and
produces an image that is a good representation of the three-
dimensional sample.
 SEM produces images of high resolution, which means that closely
features can be examined at a high magnification.
 SEM usually also equipped with analytical capability: electron probe
microanalysis (energy dispersive x-ray analysis).
 The higher magnification, larger depth of field, greater resolution and
compositional and crystallographic information makes the SEM one of the
most useful instruments in various fields of research.
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Scanning electron microscope

column

Sample
chamber
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Fundamental properties of electrons

ℎ
 Electron wavelength: the de Broglie’s wavelength of an electron is 𝜆 = ,
𝑝
where p is the electron momentum, h is the Planck’s constant.
𝑒𝑚𝑒 𝑣 2
 For an electron accelerated to a kinetic energy of eV, 𝑒𝑉 = and its
2
ℎ 12.27
momentum 𝑝 = 𝑚𝑒 𝑣 = 2𝑚𝑒 𝑒𝑉; electron wavelength 𝜆 Å = ≈
𝑝 𝑉 (𝑣𝑜𝑙𝑡)
1
 Considering relativistic effect (e.g. 100 keV electrons will have 𝑣 > 𝑐):
2
12.27
𝜆 Å ≈
𝑉 (1 + 0.978 × 10−6 𝑉)
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Resolution: electron vs. optical microscopes

0.6𝜆
𝑟𝑒𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 =
𝑛 sin 𝛼

Optical microscope Electron microscope

l~0.5mm 𝜆 Å =
ℎ
≈ 0.068Å (at 30 kV)
𝑝

n=1.5 (glass) n=1.0 (vacuum)

a~70o a~1o
Resoultion~0.2 mm or 2000Å Resolution ~4.1 Å
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Electron-solid interactions
 10

Electron-solid interactions
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SEM: an overview
 The column
─ An electron beam is produced by the electron gun
(thermionic or field emission) and accelerated to
the desired voltage (typically 0.2-40 kV).
─ The beam is focused by one or two condenser
lenses to a spot of ~0.4 to 5 nm
─ The electron beam is deflected by pairs of
scanning coils, rastering the beam in the x- and y-
directions
 The sample chamber
─ Specimens must be of an appropriate size to fit in
the specimen chamber and are generally mounted
rigidly on a specimen holder.
─ Specimens must be electrically conductive to prevent the accumulation
of electrostatic charge at the surface.
─ Nonconductive specimens tend to charge when scanned by the electron
beam, and are usually coated with an ultrathin coating of electrically
conducting material (Au, Al)
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SEM: an overview
 Electron-atom interaction: when the primary
electron beam interacts with the sample, the
electrons lose energy by repeated random
scattering (elastic or inelastic) and absorption
within a teardrop-shaped volume of the
specimen (the interaction volume), extending
from less than 100 nm to ~5 µm into the
surface.
─ Inelastic collision with electrons: energy is
transferred to the other electron and if the
energy transferred exceeds the work function a
secondary electron (SE) will be emitted with
energy typically <50 eV (within a few nm of the
solid).
─ Elastic scattering with atomic nuclei: primary
electrons elastically scattered by nuclei. Most
backscattered electrons (BSEs) have
energies comparable to the primary electron
energy (>>50 eV).
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SEM: an overview
Image formation: SEM images can be formed by either the SEs or BSEs
 SE image: due to their low energy (<50 eV), these electrons originate within a
few nanometers from the sample surface.
─ The SEs are detected by an Everhart-Thornley detector (a scintillator-
photomultiplier system).
─ The amplified signal is displayed as a 2-D intensity distribution that can
be viewed and eventually saved as a digital image.
─ The brightness of the signal depends on the number of secondary
electrons reaching the detector.
─ Using the signal of SEs, image resolution less than 0.5 nm is possible.
 BES image: dedicated BSE detectors are positioned above the sample in a
"doughnut" type arrangement, concentric with the electron beam, maximizing
the solid angle of collection.
─ BSE detectors are usually either of scintillator or of semiconductor types.
─ Since heavy elements backscatter electrons more strongly than light
elements, and thus appear brighter in the image, BSE are used to detect
contrast between areas with different chemical compositions.
 Other types of images: signals from cathodoluminescence and x-ray
microanalysis can also be used to form images giving different information of
the specimen
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SEM: images

SE BSE

SEM images of Fe particles in carbon obtained with secondary

electrons (left) and back-scattered electrons (right). The BSE image
shows the Fe particles with bright contrast

Field emission SEM image of a

AuAuAgAu nanowire, acquired with
backscattered electron detection.
The Ag segment appears darker as
compared to the Au
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SEM: the interior

L. Reimer, “Scanning Electron Microscope”, 2nd Ed.,

Springer-Verlag, 1998, p.2
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SEM: electron gun

Electron guns are used to produce a fine, controlled beam of electrons which
are then focused at the specimen surface.
 Thermionic emission gun:
─ A tungsten filament heated by DC to
approximately 2700K or LaB6 rod heated to
around 2000K in a vacuum of 10-3 Pa (10-4 Pa
for LaB6), producing flux of electrons
─ Electrons are accelerated by an acceleration
voltage of 1-50kV
 Field Emission Gun:
─ The tip of a tungsten needle is made very
sharp (radius < 0.1 mm) so that electric field
becomes very strong (> 107 V/cm) and
electrons emitted due to field emission
─ Ultra-high vacuum (<10-6 Pa) is needed to
avoid ion bombardment to the tip from the
residual gas.
─ Electron probe diameter < 1 nm is possible
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SEM: electron gun
Thermionic Gun
W E: >10MV/cm
T: ~1500oC

Filament (5-50mm)

(5nm)

W and LaB6 Cold- and thermal FEG

Source Brightness Stability (%) Size Energy spread (eV) Vacuum (Torr)
W 3x105 ~1 50 mm 3.0 10-5
LaB6 3x106 ~2 5 mm 1.5 10-6
C-FEG 109 ~5 5 nm 0.3 10-10
T-FEG 109 <1 20 nm 0.7 10-9
Brightness – beam current density per unit solid angle
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SEM components: magnetic lenses

A magnetic lens is a solenoid designed to produce a specific magnetic flux
distribution. Magnetic lenses are used for the focusing or deflection of moving
electrons. They operate by use of the magnetic Lorentz force. Their
strength can often be varied by usage of electromagnets.

𝑭 = −𝑒(𝒗 × 𝑩) Electromagnetic lenses

create a circular magnetic
field that demagnify
(condense) the electron
beam as it passes through.

Lens formula: 1/𝑓 = 1/𝑝 + 1/𝑞

𝑓𝐵𝑜2

f can be adjusted by changing 𝐵𝑜 , i.e. changing the current through coil.

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SEM components: condenser

Condenser lens – focusing
 Controls the spot size and convergence
of the electron beam which impinges
on the sample.
 For a thermionic gun, the diameter of
the first cross-over point ~20-50µm
 To focus the beam to < 10 nm on the
specimen surface, the magnification
should be ~1/5000, which is not easily
attained with one lens (say, the
objective lens) only.
 Therefore, condenser lenses are added
to demagnify the cross-over points.

Demagnification:
𝑀 = 𝑓/𝐿
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SEM components: objective

Objective lens – final probe forming
 Controls the final focus of the electron
beam by changing the magnetic field
strength
 Since the electrons coming from the
electron gun have spread in kinetic
energies and directions of movement,
they may not be focused to the same
objective
plane to form a sharp spot.
 By inserting an aperture, the stray
electrons are blocked and the remaining
narrow beam will come to a narrow
 The cross-over image is finally
demagnified to an ~10nm beam spot
which carries a beam current of
approximately 10-9- 10-12 Å.
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SEM components: scanning coils

Scanning coils in a SEM are used to raster the beam across the sample
for textural imaging
 Two sets of coils are used for scanning the
electron beam across the specimen surface in
a raster fashion over a rectangular area of the
sample surface.
 This effectively samples the specimen surface
point by point over the scanned area.
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SEM components: electron detectors

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SEM components: Everhart-Thornley detector

 A Everhart-Thornley Detector (E-T
detector or ET detector) consists
primarily of a scintillator inside a
Faraday cage inside the specimen
chamber of the microscope
 A low positive voltage is applied to the
Faraday cage to attract the relatively
low energy (<50 eV) secondary
electrons.
 The scintillator has a high positive
voltage (~10 kV) to accelerate the
incoming electrons to it where they
can be converted to light photons
 Can be used in backscattered
electron (>50 eV) mode by either
turning off the Faraday cage or by
applying a negative voltage to the
Faraday cage
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SEM components: backscattered electron detector

Backscattered electrons have energies close to the primary
beam energy and are detected by semiconductor detectors
 High energy (>50 eV to keV) backscattered
electrons (BSEs) incident on the detector
creating electron-hole pairs in the bulk of
the semiconductor.
 The 𝑒 − ℎ pairs are separated and swept to
opposite poles by an applied voltage,
creating a current
 The number of 𝑒 − ℎ pairs are proportional
to the energy of the electrons
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Electron beam microscopy/spectroscopy

The types of signals produced by a SEM include secondary electrons (SEs),
back-scattered electrons (BSEs), characteristic X-rays and photons
(cathodoluminescence) (CL), absorbed current (specimen current) and
transmitted electrons. Both SEs and BSEs are used for imaging

(1-50keV)
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Secondary electrons (SEs)

 Produced by inelastic interactions of high
energy electrons with core electrons (K, L M
shells) of atoms in the specimen, causing the
ejection of the electrons from the atoms. T
 These ejected electrons have energies <50eV.
 SE yield: 𝛿 = 𝑛𝑆𝐸 /𝑛𝐵 >1 independent of Z Bright
 d decreases with increasing beam energy and
increases with decreasing glancing angle of
incident beam Dark

 Due to their low energy, only SE that are very

near the surface (<10nm) can exit the sample
and be examined (small escape depth).
 SE generation depend on the angle of
incidence, thus local variations in the angle of
the surface to the beam (roughness) affects
the numbers of electrons leaving from point to
point. This gives rise to topographic contrast
of the specimen
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Backscattered Electrons (BSEs)
0.6
Primary
49 keV
0.5

10 keV
0.4

𝜼 0.3

0.2

0.1

0
0 10 20 30 40 50 60 70 80 90
 BSE are produced by elastic interactions Z
(scatterings) of electrons with nuclei of atoms
in the specimen and they have high energy SEM images of
and large escape depth. a geological
material taken
 BSE yield: 𝜂 = 𝑛𝐵𝑆 /𝑛𝐵 ~ increases with with 750 V
atomic number, Z electrons.
BSE
The BSE image
 BSE images show characteristics of atomic displays
number contrast, i.e., high average Z minimum
topography but
appear brighter than those of low average Z.
enhanced Z-
 𝜂 increases with tilt giving rise to topological contrast
contrast (but not as well as SEs). SE
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Interaction and escape volume

The combined effect of the elastic and inelastic interactions is to distribute the
beam electrons over a three-dimensional interaction volume. The actual
dimensions and shape of the interaction volume are dependent upon a number
of parameters: accelerating voltage, atomic number and tilt.

 The volume responsible for the

respective signal is called the
escape volume of that signal
 If the diameter of primary electron
beam is ~5nm:
─ Secondary electron:
diameter~10nm; depth~10nm
─ Backscattered electron:
diameter~1mm; depth~1mm
─ X-ray: from the whole interaction
volume, i.e., ~5mm in diameter
and depth
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Interaction volume
The interaction volume increases while the probability of elastic scattering
decrease with accelerating voltage
1 kV 5 kV 15 kV in Fe
0.0 nm 0.0 nm 0.0 nm

2.9 nm 19 nm 115 nm

5.7 nm 38 nm 230 nm

8.6 nm 57 nm 345 nm

11.5 nm 76 nm 460 nm

-8.0nm -4.0nm 0.0 4.0nm 8.0nm -52.9nm -26.5nm 0.0 26.5nm 52.9nm -320nm -160nm 0.0 160nm 320nm

The interaction volume decreases while the probability of elastic scattering

increases with higher atomic number elements.
5 kV in Carbon Iron Gold
0.0 nm 0.0 nm 0.0 nm

52 nm 19 nm 10 nm

103 nm 38 nm 20 nm

155 nm 57 nm 30 nm

207 nm 76 nm 40 nm

-144nm -72nm 0.0 72nm 144nm -52.9nm -26.5nm 0.0 26.5nm 52.9nm -27nm -14nm 0.0 14nm 27nm
 30

Electron interaction volume

Pear shape

5mm

Schematic illustration of electron beam interaction in Ni

Electron interaction volume in
polymethylmethacrylate
(plastic-a low Z matrix) is
indirectly revealed by etching
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Image Formation & Magnification in SEM

𝑴 = 𝑪/𝒙

A 10cm
e-
beam
Detector

10cm
Amplifier

 Beam is scanned over specimen in a raster pattern in synchronization

with beam in CRT.
 Intensity at A on CRT is proportional to signal detected from A on
specimen and signal is modulated by amplifier.
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SEM magnification
 Magnification in an SEM can be controlled over a range of about 6
orders of magnitude from about 10 to 500,000x.
 Image magnification in an SEM is NOT a function of the power of the
objective lens
 Magnification results from the ratio of the dimensions of the raster
on the specimen and the raster on the display device, i.e
controlled by the current supplied to the x, y scanning coils.
Magnification=area scanned on the monitor/area scanned on the specimen

x Low M High M
Large x small x
40mm 7mm

1.2mm 15000x
2500x
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Image Magnification

Example of a series of increasing magnification (spherical lead particles

imaged in SE mode)
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Resolution: spatial
 The resolution is the minimum spacing at which two features of the
specimen can be recognized as distinct or separate.
 Unlike in an optical system, the resolution is not limited by the
diffraction limit, fineness of lenses or mirrors or detector array
resolution.
 The spatial resolution of the
SEM depends on
─ the size of the electron spot,
which in turn depends on both the
wavelength of the electrons and
the electron-optical system that
produces the scanning beam.
─ the size of the interaction
volume.
 The resolution can fall
somewhere between less than 1
nm and 20 nm.
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Resolution: interaction/escape volume

 The interaction volume falls with beam
energy E as ~1/𝐸 5
 If the screen can display 1000 pixels/(raster
line), then there are 1000 pixels on each
raster line on the specimen.
 The resolution is the pixel diameter on specimen surface.
─ If escape volume is larger than the pixel size: resolution decreased since
signal from different pixel will overlap. The image will appeared out of focus.
─ If escape volume equals the pixel size: optimum resolution condition
─ If escape volume is smaller than pixel size: the resolution is still achieved
but signal will be weak and image appears noisy
Effect of probe size on escape volume
BSE x-ray
SE
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Resolution: electron optics limit

 Recall Rayleigh criterion for OM:
0.61𝜆
𝑑𝑚𝑖𝑛 =
(𝑁𝐴)
 For electrons: de Broglie wavelength
𝜆 = ℎ/𝑝 where p is the electron
momentum
ℎ
𝜆=
2𝑚𝑒 (𝐾𝐸)
1.22𝜆
 For electron diffraction: 𝑑𝑑 = ,
𝛼
for a 20-keV beam, 𝜆 = 0.0087 𝑛𝑚 and 𝛼 = 5 × 10−3 𝑟𝑎𝑑, 𝑑𝑑 = 2.1 𝑛𝑚
 SEM resolution is also affected by chromatic and spherical
aberrations (𝐶𝑠 ) of lenses:
1/4
𝑑𝑚𝑖𝑛 = 1.29𝜆3/4 𝐶𝑠
 A SEM fitted with an FEG has an achievable resolution of ~1.0 nm at
30 kV due to smaller 𝐶𝑠 (~20mm) and l.
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Resolution: specimen contrast

Contrast can be defined as (𝑆2 − 𝑆1 )/𝑆2 where 𝑆1 and 𝑆2 are the
background and feature signals, respectively and 𝑆2 > 𝑆1 .
 Topological contrast: the size, shape and texture of three
dimensional objects, dependent upon the number of SEs
and BSEs being emitted from different areas of the
specimen
 Compositional contrast: different numbers of
Excessive contrast
backscattered electrons being emitted from areas of the
sample differing in atomic number

Contrast 𝒅𝒎𝒊𝒏 (nm)

1.0 2.3
Insufficient contrast
0.5 4.6
0.1 23
0.01 230

Optimum contrast & brightness

http://www.charfac.umn.edu/sem_primer.pdf
 38

Resolution of Images
In an extremely good SEM, resolution can be a few nm. The limit is
set by the electron probe size, which in turn depends on the quality of
the objective lens and electron gun.

Pixel diameter on Specimen

Magnification µm nm
10 10 10000
100 1 1000
1000 0.1 100
10000 0.01 10
100000 0.001 1
 39

Effect of acceleration voltage

30 kV 2500 X

5.0 kV 2500 X

The image sharpness and resolution are better at the higher accelerating voltage.
However, using high accelerating voltage cannot reveal the contrast of the
specimen surface structure.
 40

Effect of objective lens aperture

SEM images require not only a fine electron probe, but also a sufficient amount
of signal for forming an image. The objective lens (OL) cannot be reduced
unnecessarily. The OL aperture must be selected with consideration given to the
effect on the image. Electric light bulb filament

Aperture diameter = 600 mm Aperture diameter = 200 mm

Working distance = 10 mm Working distance = 10 mm

Aperture diameter = 200 mm Aperture diameter = 100 mm

Working distance = 38 mm Working distance = 38 mm

The smaller the objective lens aperture diameter and the longer the working
distance (WD), the greater will be the depth of field
 41

Effect of electron probe current

In the SEM, the smaller the electron probe diameter, the higher the magnification
and resolution. However, as the probe diameter is reduced, the probe current is
reduced, affecting image smoothness.
Ceramic
10 kV and 5400 X

1 nA

0.1 nA 10 pA

The smaller the probe current, the sharper is the image, but the image becomes grainy.
 42

Effect of sample charging

Charging is the condition when a material cannot effectively conduct the beam
energy imparted to it. Non-conducting specimen will accumulate charge and the
ensuing image will glow. Typically non-conducting samples are coated with thin
conductive films (Carbon, Gold-Palladium, Platinum etc) to facilitate electron flow.

Image with No Surface Charging Image with Surface Charging

1.0 kV 3200 X 1.3 kV 3200 X

 43

Scanning probe microscopy

(SPM)
 44
Scanning probe microscopy (SPM)
Scanning probe microscopy (SPM) is a branch of microscopy that forms images
of surfaces using a physical probe that scans the specimen.

 SPM was founded in 1981,

with the invention of the
scanning tunneling
microscope by Binnig and
Rohrer. (the Nobel Prize in
Physics in 1986)
 To form images, scanning
probe microscopes raster
scan the tip over the
surface.
 At discrete points in the raster
scan a value is recorded
(depends on the type of SPM),
displayed as a heat map to
produce the final STM images
 45

Different types of SPM

Broadly speaking, there are three main categories of SPM
 Scanning tunneling microscopy (STM): uses an
atomically sharp metallic tip and records the minute
tunneling current (I) between the tip and the surface,
when the tip is hovering so close to the surface that
electrons can move between the surface and the tip. It
maps out the sample topography and electrical
properties.
 Atomic force microscopy (AFM): a cantilever with a
sharp tip - somewhat like the needle of an old record
player - is scanned over the surface. Using the van der
Waals forces or contact forces between a tip and the
sample, the sample topography or mechanical
properties can be measured.
 Scanning near-field optical microscopy (SNOM): a
probe with a small aperture is scanned over the
surface collecting the scattered light coming from
regions much smaller than the wavelength of the light
used.
 46

SPM: advantages and disadvantages

Advantages:
 The resolution of the microscopes is not limited by diffraction, only by the
size of the probe-sample interaction volume (as small as a few pm).
 Able to measure small local differences in object height (like that of 135 pm
steps on <100> silicon).
 Laterally the probe-sample interaction extends only across the tip atom or
atoms involved in the interaction.
 The interaction can be used to modify the sample to create small structures
 Can be measured in any ambient: air or liquid
Disadvantages:
 The detailed shape of the scanning tip is sometimes difficult to determine,
affecting the resulting data especially when the specimen varies in height.
 The scanning techniques are generally slower in acquiring images.
 Result greatly affected by time-domain effects like specimen drift, feedback
loop oscillation, and mechanical vibration.
 The maximum image size is generally small
 Not useful for examining buried solid-solid or liquid-liquid interfaces
 Scanning Tunneling Microscopy (STM)
 STMs use a sharpened, conducting
tip with a bias voltage applied between
the tip and the sample.
 When the tip is brought within about
10Å of the sample, electrons from the
sample begin to "tunnel" through the
gap into the tip or vice versa,
depending upon the sign of the bias
voltage.
 The resulting tunneling current varies d~1 nm

with tip-to-sample spacing, and it is the

signal used to create an STM image.
𝐼 = 𝑉𝑒 −𝐶𝑑
 For tunneling to take place, both the
sample and the tip must be
conductors or semiconductors.
STMs cannot image insulating
Silicon atoms on a A STM image of a
materials. surface via STM gold atom and ion
 48

STM: modes of operation

constant current mode constant height mode

 STMs use feedback to keep the  Tunneling current is monitored as
tunneling current constant by the tip is scanned parallel to the
adjusting the height of the scanner at surface.
each measurement point  There is a periodic variation in the
 the voltage applied to the separation distance between the tip
piezoelectric scanner is adjusted to and surface atoms.
increase/decrease the distance  A plot of the tunneling current vs.
between the tip and the sample tip position shows a periodic
 The image is then formed by plotting variation which matches that of the
the tip height vs. the lateral tip surface structure-a direct "image"
position. of the surface.
 49

STM images

Single-atom Defect in Iodine Adsorbate

Oxygen Atom Lattice on Lattice on Platinum. 2.5nm Scan Mica Surface Atoms,
Rhodium Single Crystal. 5nm Scan
4nm Scan

An STM image of a single-

Cobalt atoms arranged with a
walled carbon nanotube
Atomically resolved graphene lattice. The scanning tunneling microscope
blue and green spheres indicate two carbon
atoms of the unit cell labeled by A and B.
http://www.nanoscience.de/HTML/research/graphene.html
 50

Atomic force microscopy (AFM)

 The atomic force microscope (AFM)
probes the surface of a sample with a
sharp tip, a couple of microns long and
often less than 100Å in diameter. The tip
is located at the free end of a cantilever
that is 100 to 200µm long.
 Forces between the tip and the sample
surface cause the cantilever to bend, or
deflect.
 A detector measures the cantilever
deflection as the tip is scanned over the
sample, or the sample is scanned under Tip
the tip.
 The measured cantilever deflections allow
a computer to generate a map of surface
topography.
 AFMs can be used to study insulators
and semiconductors as well as Cantilever
electrical conductors.
 51

AFM: modes of operation

AFM operation is usually described as one of three modes, according to the nature
of the tip motion: contact mode, also called static mode (as opposed to the other
two modes, which are called dynamic modes); tapping mode, also called
intermittent contact, AC mode, or vibrating mode; and non-contact mode
 52

AFM: modes of operation

 Contact: the tip is "dragged" across the surface of the
sample and the contours of the surface are measured either
using the deflection of the cantilever directly or the feedback
signal required to keep the cantilever at a constant position.
─ High speed but image heavily influenced by frictional and
adhesive forces which can damage samples and distort image.
 Non-contact: the tip does not contact the sample surface.
The cantilever is oscillated with typically a few nm-pm. A
topographic image of the sample surface is constructed by
measuring the tip-to-sample distance at each (x,y) data point.
─ No tip or sample degradation effects, hence it is preferred for
soft samples.
─ Provides lower resolution and can be hampered by the
contaminant layer which can interfere with oscillation
 Tapping: the cantilever is driven to oscillate up and down at
or near its resonance frequency with amplitude up to 200
nm. An image is produced by imaging the force of the
intermittent contacts of the tip with the sample surface.
─ eliminates frictional forces and prevent the tip from being
trapped by adhesive meniscus forces from contaminants.
 53

AFM applications

Contact Mode: Au(111) poly- Non-contact Mode: Si(111) 7x7

Tapping Mode: Arene on graphite
crystalline film on glass.

2D S-layers assembled on mica 3D image of DNA crystals 3D image of Si wafer coated with Ta layer
(Image from Molecular Foundry, LBNL)
 54

STM vs. AFM

STM AFM
Measures local electron density of states, Real topographic imaging
not nuclear positions─not true topographic
imaging
High lateral and vertical resolution –because Lower lateral resolution
of the exponential dependence of the
tunneling current on distance
Exponential dependence between tunneling The force-distance dependence in AFM is
current and distance much more complex
Probe electronic properties (LDOS – Probe various physical properties: magnetic,
including spin states) electrostatic, hydrophobicity, friction, elastic
modulus, etc
Generally applicable only to conducting (and Applied to both conductors and insulators
semiconducting) samples
Writing voltage and tip-to-substrate spacing Writing voltage and tip-to-substrate spacing
are integrally linked can be controlled independently
Advanced SPM Techniques
 Lateral Force Microscopy (LFM)
measures frictional forces between the probe tip and the sample surface
 Magnetic Force Microscopy (MFM)
measures magnetic gradient and distribution above the sample surface
 Electric Force Microscopy (EFM)
measures electric field gradient and distribution above the sample surface
 Scanning Thermal Microscopy (SThM)
measures temperature distribution on the sample surface
 Scanning Capacitance Microscopy (SCM)
measures carrier (dopant) concentration profiles on semiconductor
surfaces
 Nanoindenting/Scratching
measures hardness, and scratch or wear testing to investigate film
adhesion and durability
 Phase Imaging
measures variations in surface properties (stiffness, adhesion, etc.) as the
phase lag of the cantilever oscillation relative to the piezo drive and
provides nano-scale information about surface structure
 56

A 3D variable temperature STM

HS-AFM*1.0 - a High-Speed Atomic Force

Microscope
 57

SEM/SPM: Internet resources

SEM:
http://www.mse.iastate.edu/microscopy
http://www.charfac.umn.edu/sem_primer.pdf
http://cfamm.ucr.edu/documents/sem-intro.pdf
http://virtual.itg.uiuc.edu/training/EM_tutorial
http://science.howstuffworks.com/scanning-electron-microscope.htm/printable
http://www.matter.org.uk/tem/electron_gun/electron_sources.htm
http://www.matter.org.uk/tem/lenses/simulation_of_condenser_system.htm
http://micro.magnet.fsu.edu/primer/java/lenses/converginglenses/index.html
SPM:
http://www.doitpoms.ac.uk/tlplib/afm/tip_surface_interaction.php
http://physics.usask.ca/~chang/course/phys404/STMandAFM.pdf
http://www.eng.utah.edu/~lzang/images/Lecture_4_SPM.pdf
http://leung.uwaterloo.ca/MNS/102/Lect_2013/Lect_26A.pdf
http://www.asylumresearch.com/Gallery/Gallery.shtml