Automated Multipurpose

X-ray Diffractometer
Instruction Manual
This manual describes the correct use of the product as well the usage precautions to be observed. To
obtain full-expected performance from the product, thoroughly read this manual.

Also, store this manual at an easily accessible place so that you can promptly refer to it whenever
it is necessary.

The contents of this manual are subject to change without prior notice.
This manual described in it may not be disclosed to a third party or copied, in whole or in part, without
the written consent of Rigaku Corporation.
In no event will Rigaku Corporation be responsible for the results of the use of this manual.
As a rule, one set of the instruction manual has to be purchased for each product.
If there are any missing or incorrectly collated pages in the delivered instruction manual, please
contact the sales representative who you purchased the instrument from for instruction manual
replacement.
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The names of actual companies and products mentioned herein may be the registered trademarks or
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Before Using the Product
Read this manual cover to cover before attempting to use SmartLab. Carefully read the Guidelines for safe
use of the X-ray diffractometer described in the beginning of this manual.

Copyrights

1. Duplication or reproduction of this manual in whole or in part is strictly prohibited, whether

via hardcopy or electronically. If copies must be made, you must obtain our written approval
before doing so for each specific case.

2. No part of this manual may be disclosed to third parties. If the contents of this manual must be
disclosed to a third party, you must obtain our written approval before doing so for each
specific case.

3. No part of this manual may be cited without our permission. No part of this manual may be
translated or disclosed to a third party without permission. If you must cite or translate any
part of this manual, you must obtain our written approval before doing so for each specific
case.

4. In general, unless special agreements are reached, each product unit is provided with a copy of
this manual.

5. The contents of this manual are subject to change without notice.

Liability

1. Rigaku shall not be held liable for any accidents caused by or resulting from any of the
following.

* Use of the product for a purpose other than the purpose intended
* End of product life
* Unauthorized modifications
* Inadequate maintenance by the user
* Natural phenomena, armed conflicts, civil disturbances
* Use or action in breach of instructions given in this manual
* Installation conditions failing to meet the recommended ambient parameters
* Consumables

2. Rigaku Corporation cannot be responsible for the results of using this manual to operate the
product or the effects of the results of such operation.

Relocation
Please contact Rigaku Corporation before attempting to move the product from the originally installed
location.
Trademarks and registered trademarks
Microsoft and Windows are trademarks or registered trademarks of Microsoft Corporation in the United
States and/or other countries.
Pentium is a registered trademark of Intel Corporation.
Other company names and product names are trademarks or registered trademarks of their respective
companies.
Note that this manual omits the TM (™) and R (®) symbols.
Contents
Overview ............................................................................................................1

Product Features ..............................................................................................3

High-accuracy theta-theta goniometer .....................................................................3
Attachment ...............................................................................................................3
X-ray generator.........................................................................................................3
Cross beam optics (CBO).........................................................................................4
Alignment mechanism (monochromators and analyzers) ........................................4
Receiving analyzer system.......................................................................................4
Incident optics system ..............................................................................................5
Receiving optics system ...........................................................................................5
Optics switching system ...........................................................................................5
Optical device detection ...........................................................................................6
Control software (SmartLab Guidance) ....................................................................6
Two-slit SAXS optics ................................................................................................7
In-plane optics (2080B212) ......................................................................................7
Names of Parts..................................................................................................9
Main unit ...................................................................................................................9
Goniometer.............................................................................................................11
X-ray tube ...............................................................................................................13
Theta_s arm ...........................................................................................................14
Theta_d arm ...........................................................................................................15
Detector mounting bracket .....................................................................................16
Sample stage and attachments ..............................................................................16
Software Configuration ..................................................................................17
Control software .....................................................................................................17
Data processing software .......................................................................................17
Data display software (options) ..............................................................................17
Analysis software (options).....................................................................................17
Turning On and Off SmartLab........................................................................19
Turning on SmartLab ..............................................................................................19
Starting SmartLab Guidance ..................................................................................19
Startup ....................................................................................................................20
Shutdown................................................................................................................21
Exiting SmartLab Guidance....................................................................................22
Turning off SmartLab ..............................................................................................22
Opening and Closing the Door ......................................................................23
Opening the door....................................................................................................23

SmartLab: Automated Multipurpose X-ray Diffractometer i

 Closing the door .....................................................................................................24
Emergency stop switch (EMO) ...............................................................................24
Turning on/off the internal lamp (LAMP).................................................................24
Optics...............................................................................................................25
CBO unit (for Cu target)..........................................................................................25
Incident optics unit (standard incident optics unit)..................................................30
Incident parallel slit adaptor (IPS adaptor) ......................................................30
2-bounce monochromator (option) ..................................................................33
4-bounce monochromator (option) ..................................................................36
CBO-f unit (option: 2220C301) ........................................................................38
Incident slit box.......................................................................................................40
Standard incident slit box.................................................................................40
Collimator holder (option) ................................................................................42
Receiving slit box # 1..............................................................................................46
Standard receiving slit box # 1.........................................................................46
Receiving optics unit # 1.........................................................................................49
Receiving optical device adaptor (ROD adaptor) ............................................49
2-bounce analyzer (option)..............................................................................52
Receiving optics unit # 2.........................................................................................54
Receiving parallel slit adaptor (RPS adaptor)..................................................54
Receiving slit box # 2..............................................................................................57
Standard receiving slit box # 2.........................................................................57
Attenuator ...............................................................................................................59
Standard attenuator .........................................................................................59
Receiving optics unit CALSA (option: 2680K201) ..................................................61
Receiving parallel slit.......................................................................................63
CALSA beam conditioner ................................................................................65
Dtector (D/teX Ultra) ........................................................................................66
Detector ...........................................................................................................67
Detector adaptor.....................................................................................................67
Scintillation counter ................................................................................................69
DBM unit for Cu (option: 2726H112) ......................................................................71
D/teX Ultra (option: 5741A300) ..............................................................................74
DBM unit for Cu for D/teX Ultra (option: 2726P101)...............................................76
PILATUS (option: 5742A101) .................................................................................78
Sample Stage ..................................................................................................79
Standard sample stage...........................................................................................80
β sample stage (option: 2430B101)........................................................................80
ASC-6 (option: 2430H101) .....................................................................................81
For vertical transmission geometry (option: 2455H105)..................................82
AntonPaar sample stage ........................................................................................84

ii SmartLab: Automated Multipurpose X-ray Diffractometer

 Attachments ....................................................................................................85

Sample Plates..................................................................................................87
Height reference sample plate................................................................................87
Transmission SAXS sample plate (option: 2680J111)............................................87
Capillary holder (option: 2430C101).......................................................................88
Wafer sample plates and sample spacers..............................................................88
Installing and removing sample spacers..........................................................91
Installing and removing wafer sample plates...................................................92
Sample Holders...............................................................................................93
Glass sample holder...............................................................................................93
Aluminum sample holder ........................................................................................93
Transmission SAXS sample holder (option: 2680J111)..........................................93
Accessories.....................................................................................................95

Examples of Sample Mounting ......................................................................97

Powder samples .....................................................................................................97
Bulk samples ..........................................................................................................97
Sample for transmission SAXS measurements......................................................97
Wafer-shaped samples...........................................................................................98
Measurements.................................................................................................99
Preparing for measurements ..................................................................................99
Setting the hardware configuration.........................................................................99
Selecting a Package Measurement......................................................................100
Periodic Maintenance ...................................................................................101
Optics maintenance..............................................................................................101
Cooling water........................................................................................................102
Cooling water filter................................................................................................102
Target (2080A211/A411) .......................................................................................102
Filament (2080A211/A411) ...................................................................................102
Ion gauge (vacuum gauge) (2080A211/A411) ......................................................102
Rotary pump (2080A211/A411) ............................................................................102
Troubleshooting............................................................................................103

Cat. No. 2080A211/B211/B212/A411/B411

Manual No. ME11573A04
2010. 11 (Forth Edition)

SmartLab: Automated Multipurpose X-ray Diffractometer iii

 Overview
SmartLab, Automated Multipurpose x-ray Diffractometer, is an x-ray diffraction
system equipped with a high-accuracy theta-theta goniometer featuring a horizontal
sample mount. By changing slits (selection slits), the operator can use the
para-focusing optics to measure polycrystalline samples, the parallel beam optics
incorporating a multilayer mirror suitable for high-precision measurement to
measure polycrystalline and thin film samples, or the SAXS optics to measure
nano-scale samples. A high-resolution optics system provided with a 2- or
4-bounce monochromator on the incident side and a 2-bounce analyzer or CALSA
on the receiving side can be easily installed simply by exchanging units. Adding an
in-plane arm allows various in-plane measurements. SmartLab is capable of
performing a broad range of measurements required for thin film analysis.

Soller slit Ni filter Soller slit Phase ID

Para-focusing analysis/
method
Soller slit Soller slit
Diffracted beam Quantitative
monochromator
analysis

Soller slit PSA Soller slit

Profile analysis
PSA Soller slit Preferred orientation
analysis
Soller slit
Rietveld analysis
+ Structure analysis
CALSA

2-bounce
monochromator
+
SmartLab 2-bounce
Parallel beam Soller slit Soller slit
system analyzer
Film thickness analysis
Soller slit Rocking curve
4-bounce
monochromator Reciprocal space mapping
2-bounce
Soller slit
analyzer

Particle-/Pore-size
SAXS Soller slit Soller slit
distribution analysis

Micro area CBO-ｆ Soller slit D/teX Ultra Micro area

PSC PSA Preferred orientation

Parallel beam measurement
2-bounce In-plane
monochromator
+
PSA measurement
PSC *In-plane arm (option) is required.

CBO unit Incident optics Receiving optics

SmartLab structure and measurement examples

The following five types of SmartLab are described in this manual.

• 2080A211 Rotating anode type

• 2080B211 Sealed tube type
• 2080B212 Sealed tube type with in-plane arm
• 2080A411 Rotating anode type
• 2080B411 Sealed tube type

SmartLab: Automated Multipurpose X-ray Diffractometer 1

 Column
Characteristic x-rays
X-rays are generated by accelerating electrons to very high speeds in a vacuum and directing them against the
anode (target). The x-ray spectra generated by electrons colliding against the target can be divided into two
categories: a continuous spectrum indicating continuous x-rays (white x-rays) and a discrete spectrum for
characteristic x-rays

4000

β α
Characteristic
特性X線
x-rays
Intensity
強度

2000

Continuous
x-rays
連続X線

0
0 0.5 1 1.5 2
Wavelength
波長（Å）(Å)

X-ray spectrum of Cu target

The wavelengths of characteristic x-rays depend on the type of target used. Typical x-ray diffractometry uses Kα
x-rays generated by several types of metal targets, as shown in the following table. Kα x-rays contain Kα1 x-rays
and Kα2 x-rays whose wavelengths are quite close. Although this does not pose serious problems for ordinary
measurement of powder samples for phase identification (ID) analysis, optimal results can be achieved by using
only Kα1 x-rays in certain cases when making measurements for crystal structure analysis with powder samples or
when performing precise measurements of thin film samples. In recent years, it has become possible to use just Kα1
x-rays by employing an incident optical system comprised of a multilayer mirror and a Ge or Si monochromator
crystal.

Table Wavelengths of characteristic x-rays

Target Wavelength (Å)

Atomic Kα2 Kα1 Kβ

Element
number
Cr 24 2.294 2.290 2.085
Fe 26 1.940 1.936 1.757
Co 27 1.793 1.789 1.621
Cu 29 1.544 1.541 1.392
Mo 42 0.7135 0.7093 0.6323
Ag 47 0.5638 0.5594 0.4970
W 74 0.2138 0.2090 0.1844
 Product Features

High-accuracy theta-theta goniometer

A theta-theta goniometer enables omega scans, 2-theta/omega scans, and 2-theta
scans with the sample oriented horizontally (deviation from horizontal
orientation may occur if sample orientation is adjusted). The horizontal
positioning of a sample minimizes the distortion effects caused by weight in the
case of a large wafer while reducing the possibility of a dropped sample.
Additionally, the two axes are equipped with encoders to enable control of each
axis at a resolution of 0.0001º.

Attachment
XY attachment for automated XY mapping or an RxRy attachment for sample
tilt alignment to be conducted before in-plane or reciprocal space map (RSM)
measurement. A newly developed connector allows easy changing of
attachments.

X-ray generator
Even with a horizontal sample mount goniometer with a moving x-ray source,
the product can incorporate a state of the art high-intensity 9 kW rotating anode
x-ray generator. When combined with a multilayer mirror, this x-ray generator
produces a high intensity x-ray beam (approx. 6 to 7 times the intensity provided
by a sealed-tube system) equal to an 18-kW rotating anode x-ray generator,
while reducing power consumption by 50% due to the high-brightness focal spot.
The system also offers lower operating costs compared to earlier models. A 3 kW
sealed tube x-ray generator can also be used with the SmartLab system. The
specifications of each generator are summarized in the following table.

Table Generator specifications

Max. load Max. voltage Max. current Target metal

9 kW rotating anode *1 9 kW 45 kV 200 mA Cu
3 kW sealed tube *2 3 kW 60 kV 50 mA Cu
*1 : 2080A211/2080A411
*2 : 2080B211/2080B212/2080B411

SmartLab: Automated Multipurpose X-ray Diffractometer 3

Product Features

Cross beam optics (CBO)

This unit allows easy switching between the direct beam for para-focusing
(Bragg-Brentano) optics for phase ID analysis and quantitative analysis of
powder samples and a monochromatic parallel beam using a multilayer mirror
for profile analysis of powder samples, measurement of preferred orientation,
measurement of thin film samples, RSM measurement, and rocking curve
measurement, simply by changing a selection slit. Similarly, other selection slits
allow easy switching between small angle x-ray scattering (SAXS) optics for
nano-structural measurements and small aperture optics for micro area analysis.

Alignment mechanism (monochromators and analyzers)

You can select crystal index and type based on the resolution required for
measurement. The 2-bounce monochromators, 4-bounce monochromators, and
2-bounce analyzers have built-in adjustment mechanisms that enable automatic
adjustment via control software (hereinafter referred to as “SmartLab
Guidance”). Crystal adjustment positions are preserved even after the unit is
removed, enabling data measurements without readjustment, simply by
installing the previously adjusted crystal.

Receiving analyzer system

Since the receiving slit box # 2 has a translatable slit position, the following
receiving analyzer systems can be used for different applications simply by
replacing the parts and using the automatic adjustment function of SmartLab
Guidance.

• Double-slit analyzer with two variable slits on receiving side

Para-focusing,, small-angle scattering, and reflectivity measurement
geometries, etc.
• Parallel-slit analyzer (PSA)
Profile measurements of powder samples using parallel beam optics and
requiring high intensity and high precision, thin film measurements, and
measurement of preferred orientation, etc.
• 2-bounce analyzer
Reflectivity measurements requiring high resolution, RSM measurements,
and rocking curve measurements, etc.

4 SmartLab: Automated Multipurpose X-ray Diffractometer

 Incident optics system

Incident optics system

The following mechanisms enable switching between para-focusing optics,
parallel beam optics, 2- or 4-bounce monochromator high resolution optics,
small-angle scattering optics, and micro area measurement optics.
Additionally, for various in-plane measurements, a parallel slit collimator (PSC)
that controls resolution in the in-plane direction can be installed on the incident
parallel slit adaptor and 2-bounce monochromator.

• CBO unit
To select the incident beam.
• Standard incident optics unit
To select Soller slit, 2-bounce monochromator (with Soller slit), or 4-bounce
monochromator.
• Standard incident slit box
Equipped with variable slit and length-limiting slit.

Receiving optics system

The following mechanisms enable selection of a broad range of resolution
characteristics for specific purposes.
A parallel slit analyzer (in-plane PSA) that increases the resolution in the
in-plane direction can be used for various in-plane measurements.

• Standard receiving slit box # 1

For installation of a Kβ x-ray filter for measurements using para-focusing
optics.
• Standard receiving optics unit # 1
For installation of various analyzers.
• Standard receiving optics unit # 2
For installation of parallel slit such as Soller slits.
• Standard receiving slit box # 2
With a slit position alignment mechanism.
• Standard attenuator
For the adjustment of x-ray intensity.

Optics switching system

Optics alignment results are retained by SmartLab Guidance. When you change
optics the previously stored alignment results are used eliminating the need for
realignment.

SmartLab: Automated Multipurpose X-ray Diffractometer 5

Product Features

Optical device detection

SmartLab Guidance can check the conditions of the following optical devices
used for measurement.

• Selection slit in CBO unit

• Type of incident Soller slit or crystal monochromator
• Width of incident slit
• Length of length-limiting slit or type of collimator
• Width of receiving slit
• Type of analyzer
• Type of receiving Soller slit
• Type of detector
• Presence/absence of diffracted beam monochromator, etc.
SmartLab Guidance checks whether the necessary optical devices are installed
and displays a message for the optical configurations suitable for the user’s
intended application. The measurement data file stores parameters for the optical
devices during measurement to improve data reproducibility and traceability.

Control software (SmartLab Guidance)

SmartLab Guidance used to control SmartLab also guides the user through
required measurement procedures and condition-setting processes, in addition to
providing conventional SmartLab control functions. Optical device
configurations, optics alignment methods, sample alignment methods, and
measurement conditions specific to various measurement needs are grouped in
units called Package Measurements. By selecting an appropriate Package
Measurement for the analysis purpose, the user is guided through the procedures
of optics alignment, sample alignment, and data measurement. The program
provides the optimal alignment and measurement conditions for the desired
analysis.
Each Package Measurement was prepared by specialists with expertise in the
specific field of measurement methodology. Even users with limited experience
with x-ray diffraction or x-ray reflectivity measurements can perform
measurements in the same way a specialist would. The software also allows
customization of alignment and measurement conditions for special
measurement needs. Manual control is also possible. The software is designed to
meet a wide range of user needs.

6 SmartLab: Automated Multipurpose X-ray Diffractometer

 Two-slit SAXS optics

Two-slit SAXS optics

The two-slit SAXS optics incorporating a multilayer mirror can perform
measurements with better accuracy and S/N ratios than conventional three-slit
SAXS optics. SmartLab Guidance handles previously difficult adjustments of
small-angle scattering optics. NANO-Solver, the analysis package for pore and
particle size distribution analysis, corrects scattered image distortion resulting
from optics based on the deconvolution of the slit function.

In-plane optics (2080B212)

The use of the in-plane arm and RxRy attachment enables measurements of
in-plane diffraction by maintaining grazing incidence conditions during sample
rotation. This allows the measurement of diffraction from lattice planes
perpendicular to the sample surface. High-precision measurement of orientation,
crystallinity, and distortion of thin films are possible without interference by
x-rays scattered or diffracted from the substrate. Reflection pole figure
measurements using the in-plane geometry eliminate the blind region at the pole
figure edge typically encountered with traditional out-of-plane reflection pole
figure measurements. Complete crystal orientation information is obtained from
the total-area pole figure. Conditions for optics alignment and sample alignment
are set automatically by SmartLab Guidance Package Measurements.

SmartLab: Automated Multipurpose X-ray Diffractometer 7

 Column
Tube voltage and tube current
The intensity of characteristic x-rays is proportional to the n-th power of the difference between tube voltage and
minimum excitation voltage (minimum voltage required for obtaining characteristic x-rays). It is also proportional
to tube current. When the tube voltage is low, the value of n approaches 2. As the tube voltage increases, the value
of n becomes smaller. On the other hand, the intensity of continuous x-rays that appear as a background in the Kβ
filter method is proportional to the square of the tube voltage and is also proportional to the tube current. This
means that an optimum tube voltage value exists for measurements with each target. The following table gives the
optimum voltages for different target types. For measurements using the Kβ filter method, it is a good way to set
the tube voltage so that the P/B ratio (peak-to-background ratio) will become the largest.

Minimum Optimum voltage

excitation (equivalent load) (kV)
Target
voltage
Intensity at P/B ratio at
(kV)
maximum maximum
Cu 8.86 40～55 25～35
Co 7.71 35～50 25～35
Fe 7.10 35～45 25～35
Cr 5.98 30～40 20～30
 Names of Parts
1.

2.

General view of SmartLab

(Left: 2080A211/2080B211/2080A411/2080B411, Right: 2080B212)
Pump for maintaining the vacuum in the x-ray generator.
1. Rotary pump
(2080A211/2080A411）
2. Control PC PC used to control SmartLab.

Main unit
4. 3. 4. 3.

5. 5.

2. 1. 2. 1.

Front view of SmartLab

(Left: 2080A211/2080B211/2080A411/2080B411, Right: 2080B212)

SmartLab: Automated Multipurpose X-ray Diffractometer 9

Names of Parts

1. Main panel Panel used to start and stop SmartLab.

2. Operating panel Panel used to turn the internal light on/off.
This door is opened to change samples and
3. Door
optical devices.
4. X-ray warning lamp Lights when x-rays are generated.
5. Door-lock button Lock/Unlock the door.

11.

10.
12.

6.

8. 9.
7.

Rear view of SmartLab

6. Power input connector External power supply connects here.

The LAN cables used to control SmartLab
7. Connector for control PC
connect here.
The power supply for the rotary pump
8. Connectors for rotary pump connects here.
(2080A211/2080A411)
9. Connectors for water The water circulation pump (short-cut valve)
circulation pump control connects here.
The cooling water pipe of the x-ray generator
10. Pipes for cooling water
connects here.
The rotary pump pipe connect here.
11. Pipes for rotary pump
(2080A211/2080A411)
Circuit breaker for the power supply to the
12. Circuit breaker
main unit.

10 SmartLab: Automated Multipurpose X-ray Diffractometer

 Goniometer

Goniometer

1. 3.

5.

2.
6.

7.
4.

Goniometer

1. Theta_s arm Arm for controlling x-ray beam incident angle.

2. X-ray tube X-ray generating device.
Optical device for achieving desired incident
3. Incident optics
x-ray conditions.
4. Theta_d arm Arm for controlling the x-ray detector angle.
Optical device for achieving desired x-ray
5. Receiving optics
receiving conditions.
6. Detector X-ray detector.
Adjusts the position and orientation of the
7. Sample stage
sample to be measured.
Theta_d arm used for in-plane measurements.
8. In-plane arm
(2080B212)

SmartLab: Automated Multipurpose X-ray Diffractometer 11

Names of Parts

Theta_s arm
• Selection slit

PB, BB, SA, etc.

→CBO unit (for Cu target)

• Incident length-limiting slit

10, 15 (mm), etc.
→Incident slit box

• Incident parallel slit

adaptor/monochromator
Soller slit 5.0 deg、Ge(220)x2 CBO-f etc.
→Incident optics unit (standard incident optics unit)

Theta_d arm
• Kβ filter
→Receiving slit box # 1

• Receiving optical device adaptor/analyzer

• PSA
PSA 0.114 deg, Ge(220)x2 etc.
→Receiving optics unit # 1
• Receiving parallel slit adaptor
• Soller slit/in-plane PSA
Soller slit 5.0 deg, In-plane PSA 0.5 deg etc.
→Receiving optics unit # 2

• Scintillationcounter, D/teX ultra

/diffracted beam monochromator for Cu
→Detector

Sample attachment

• Sample plate
Height reference sample plate,
4-inch sample plate, etc.
→Sample Plates
• Attachment
Standard, XY-4”φ, etc.
→Attachments

• Sample stage
Standard sample stage, β sample stage, etc.
→Sample Stage

12 SmartLab: Automated Multipurpose X-ray Diffractometer

 X-ray tube

X-ray tube
4. 3.

6.
2.

1.
5.

Rotating anode x-ray tube (2080A211/2080A411)

Connect the x-ray generator cooling water
1. Cooling water pipe
pipe.
2. Rotary target X-ray generating source.
3. Shutter Controls x-ray emissions.
4. Filament replacement window Window for replacing the filament.
5. Ion gauge Measures the vacuum in the x-ray generator.
6. Turbo molecular pump (TMP) Vacuates the x-ray generator.

3.

1.

2.

Sealed x-ray tube (2080B211/2080B212/2080B411)

1. Cooling water pipe Connect the x-ray generator cooling water pipe.
2. X-ray tube X-ray generating source.
3. Shutter Controls x-ray emissions.

SmartLab: Automated Multipurpose X-ray Diffractometer 13

Names of Parts

Theta_s arm
2.
3.

4.

1.

Theta_s arm
The control cable of the optical device
1. Incident connector box
connects here.
2. Cross beam optics (CBO) unit Optics unit for switching optics.
Soller units, monochromators, etc. are
3. Incident optics unit
installed here
4. Incident slit box Variable slit on the incident side.

14 SmartLab: Automated Multipurpose X-ray Diffractometer

 Theta_d arm

Theta_d arm
3. 4.

2.

5. 6.
1.

Theta_d arm
The control cables for the optical devices
1. Receiving connector box
connect here.
2. Receiving slit box # 1 Variable slit on receiving side.
Receiving optical devices (analyzer) are
3. Receiving optics unit # 1
installed here.
4. Receiving optics unit # 2 Soller slits, etc. are installed here
5. Receiving slit box # 2 Variable slit on receiving side.
6. Attenuator Adjusts x-ray intensity.

SmartLab: Automated Multipurpose X-ray Diffractometer 15

Names of Parts

Detector mounting bracket

1.

2.

Detector mounting bracket

Used to secure the detector in
1. Base
place.
2. Detector adaptor Used to attach the detector.

Sample stage and attachments

1. 2. 3.

Sample stage and attachments

1. Sample stage Sample attachment unit.

Attachment to be mounted to the
2. Attachment
sample stage.
Plate on which sample holder or
3. Sample plate
sample is placed.

16 SmartLab: Automated Multipurpose X-ray Diffractometer

Software Configuration
Control software
Used to control SmartLab and perform
SmartLab Guidance
measurements.

Data processing software

Performs basic data processing such
Standard data processing as smoothing, background removal,
etc.
PDXL Performs basic data processing.

Data display software (options)

Thin Film data processing Performs a brief analysis of rocking
(9240H162) curve as well as basic data processing.
Superimposes multiple measurement
Profile viewer (9240H162)
data for display.
Displays two-dimensional data such as
3D Explore (9240H403) RSM, pole figure, etc. Performs
simple data processing.

Analysis software (options)

Performs the additional functions
PDXL(9240J702, 9240J703, such as phase ID analysis,
9240J710) quantitative analysis, Rietveld
analysis, etc.
GlobalFit: reflectivity
Performs reflectivity analysis.
analysis (9240H155)
Performs particle size/pore diameter
NANO-Solver(9289H901)
distribution analysis.
Performs analysis of particle
Pore size analysis size/pore diameter distribution of
(9240H231) thin film, accounting for diffuse
scattering from surface and interface.
GlobalFit: extended rocking Performs simulation and analysis of
curve analysis (9240H145) rocking curve.
Performs quantitative analysis of the
QA-Tex(9240H601)
preferred orientation of a sample.
Performs crystallite size distribution
CSDA(9240H651)
analysis.

SmartLab: Automated Multipurpose X-ray Diffractometer 17

 Column
Penetration depth (effective thickness)
The following formula gives the ratio Gx between the intensity of diffracted x-rays from a sample of infinite
thickness and the intensity of diffracted x-rays from a sample with a specific finite thickness of x cm.

x
∫ dI D = 1 − exp⎛ − 2μx ⎞
Gx = ∞0 ⎜ ⎟
∫0 DdI ⎝ sin θ ⎠

Substitute the values for angle θ of the incident x-ray beam and x-ray absorption coefficient μ(/cm) in the following
formula to obtain x cm, the effective thickness.

− ln(1 − G x ) sin θ K x sin θ

x= =
2μ 2μ K x = − ln (1 − G x )
where,

Diffracted x-ray
utilization rate Gx 50 75 90 95 99 99.5
(%)
Kx 0.69 1.39 2.30 3.00 4.61 6.91

The following table shows the results of calculations of the sample thicknesses x cm that give a diffracted x-ray
usage rate of 90% when Kx = 2.30 and θ = 90°.
2
密度ρρ
Density absorption coefficient μ/ρ2(cm
Mass質量吸収係数μ/ρ（cm Thickness for 90% utilization rate (mm)
90%利用率の厚さ（mm)
/g) /g)
Substance
物質 3
（g/cm ) MoKα CuKα CoKα CrKα MoKα CuKα CoKα CrKα
α‐Al2O3 3.97/2 3.34 31.1 48.0 97.6 1.74 0.187 0.121 0.060
Si 2.42/2 6.44 60.6 93.3 189 1.48 0.157 0.102 0.050
α‐SiO2 2.65/2 3.71 34.5 53.1 108 2.34 0.252 0.164 0.080
Powder
CaCO3 2.71/2 8.02 70.9 107 205 1.06 0.120 0.079 0.041
粉末
α‐Fe2O3 5.26/2 27.3 216 42.7 86.5 0.160 0.020 0.103 0.051
ZnO 5.60/2 44.7 50.7 78.2 159 0.092 0.081 0.053 0.026
Ag2O 7.22/2 24.1 204 300 548 0.132 0.016 0.011 0.0058
PbO I(正方）
(tetragonal) 9.53/2 112 216 311 540 0.022 0.011 0.0078 0.0089
Al 2.70 5.16 48.6 74.8 152 0.826 0.088 0.057 0.028
α‐Fe 7.86 38.5 308 52.8 108 0.038 0.0048 0.028 0.014
Metal
金属 SUS(18-8) 7.93 37.9 278 110 106 0.038 0.0052 0.013 0.014
Cu 8.92 50.9 52.9 81.6 166 0.025 0.024 0.016 0.0078
Pb 11.34 120 232 334 579 0.0085 0.0044 0.0030 0.0018
Polymer ポリエチレン
ポリマー
Polyethylene 0.93 0.59 4.0 6.1 12.5 21.0 3.09 2.02 0.989
Vinyl
塩化ビニールchloride 1.41 6.73 62.0 94.2 186.2 1.21 0.132 0.086 0.044
Single crystal Si 2.42 6.44 60.6 93.3 189 0.738 0.079 0.051 0.025
単結晶
substance α‐SiO
2 2.65 3.71 34.5 53.1 108 1.17 0.126 0.082 0.040
Turning On and Off SmartLab
Described below are the procedures for turning on and off SmartLab.

Turning on SmartLab
1 Make sure that the HV ENABLE key on the main panel is unlocked
(the key is in the horizontal position).
If it is locked (the vertical position), turn the key clockwise to unlock it.

Confirm that the key

is unlocked.

Main panel

2 Press the “|” ON button.

3 Make sure the OPERATE lamp lights up in green.

The OPEARATE lamp blinks while SmartLab is starting up and when an error occurs. For
more information, see Appendix Using the OPERATE Lamp.

Starting SmartLab Guidance

1 Click the Start button. Select All Programs → Rigaku → SmartLab
Guidance, then select SmartLab Guidance.

2 The login window will appear. Enter the registered user name and
password in the Login name and Password boxes, and click the OK
button. (When launching the software for the very first time, enter
administrator in the Login name box and click the OK button without
entering a password.)

3 The control axes are initialized after the software is launched.

SmartLab: Automated Multipurpose X-ray Diffractometer 19

Turning On and Off SmartLab

For detailed information on initialization, refer to Section 14 of the “Reference Manual”

Help Topic of the online help section of the SmartLab Guidance software.

Startup
Click Package Measurement under the Task menu and click Startup on the
displayed Package Measurement flow bar.

Startup

When not using the water circulation pump, make sure the cooling water is flowing
properly. If the cooling water is not flowing or the amount, pressure of water are
incorrect, an alarm will be issued and remain active for three minutes after the
startup procedure is initiated. Adjust the water volume to shut off the alarm within
three minutes, then repeat the startup procedure. For information on how to adjust
the water volume, refer to the instruction manual of the water circulation pump.

For the startup procedure, refer to Section 2.1 of the “CBO Maintenance Package
Measurement” Help Topic of the online help section of the SmartLab Guidance software.

20 SmartLab: Automated Multipurpose X-ray Diffractometer

 Shutdown

Shutdown
Click Package Measurement under the Task menu and click Shutdown in the
displayed Package Measurement flow bar.

Shutdown

CAUTION When not using the water circulation pump, wait three minutes following
shutdown (i.e., three minutes after the yellow lamp located at the upper
section of SmartLab goes out), then halt the supply of cooling water. (Halting
the cooling water supply in less than three minutes may result in damage to
SmartLab.)

For more information on the shutdown procedure, refer to Section 2.6 of the “CBO
Maintenance Package Measurement” Help Topic of the online help section of the SmartLab
Guidance software.

While SmartLab is not used, it is recommended to turn off only the x-ray, and do not turn
off the vacuum unit. In this case, the controller remains powered; therefore SmartLab can be
started from SmartLab Guidance. If SmartLab is unused for a while (e.g. during the New
Year Holidays), press the “O” OFF button to turn the power of SmartLab off.

SmartLab: Automated Multipurpose X-ray Diffractometer 21

Turning On and Off SmartLab

Exiting SmartLab Guidance

After turning off the x-rays, exit SmartLab Guidance.

1 Click the Exit command under the File menu to exit SmartLab
Guidance.

Turning off SmartLab

If SmartLab is unused for a while (New Year Holidays, etc.), turn off SmartLab
according to the following procedure.

1 Check the SmartLab status (e.g., confirm that measurements have

been completed).

2 Press the “O” OFF button on the main panel.

main panel

3 Make sure the OPERATE lamp has turned off.

This procedure completely shuts down the SmartLab internal power supply.

22 SmartLab: Automated Multipurpose X-ray Diffractometer

Opening and Closing the Door
To prevent human exposure to x-ray radiation, the shutter and door are equipped
with an interlocking function. To ensure safety, when changing samples or optical
devices during x-ray generation, open and close the door by the following
procedure:

Opening the door

Under normal conditions, the door is locked and cannot be opened.

1 Press the DOOR LOCK button on the door.

2 The shutter will close and the door will be unlocked.

3 The DOOR LOCK button will flash, and you will hear beeping.

4 Open the door.

The shutter cannot be opened when the door is unlocked. The following message
also appears when the door is unlocked. SmartLab Guidance cannot be operated
until the door is locked again.

SmartLab: Automated Multipurpose X-ray Diffractometer 23

Opening and Closing the Door

Closing the door

1 Close the door of the radiation enclosure.

2 Press the DOOR LOCK button on the door.

3 When the door is properly locked, the DOOR LOCK button stops
flashing, and the beeping stops. The instrument is then ready for
operation.

Emergency stop switch (EMO)

Press this switch in the event of an emergency to cut off the power supply to the
main unit.
To cancel the emergency stop status, turn the button clockwise. After confirming
safety, press the “|” ON button on the main panel to restart SmartLab. (see
Turning on SmartLab, Starting SmartLab Guidance, Startup).

After restarting SmartLab, also restart SmartLab Guidance.

Emergency stop switch (EMO)

Turning on/off the internal lamp (LAMP)

Press once the LAMP button to turn on the internal lamp. Press again to turn it
off.

LAMP button

24 SmartLab: Automated Multipurpose X-ray Diffractometer

 Optics
This section introduces the names of parts and describes how they are installed. For
information on how to use the Kα1 unit, refer to the instruction manual of the Kα1
unit.

CBO unit (for Cu target)

The CBO unit is designed for characteristic x-rays (Kα x-rays) generated by the
standard Cu target. Changing selection slits allows switching between divergent
and parallel/convergent beams using a multilayer mirror. A parallel beam can
also be converted into a narrow beam for small-angle scattering measurements
or a small beam for micro area measurements.
Fine adjustments of the multilayer mirror can be performed from SmartLab
Guidance.

Table CBO unit

Unit name Abbreviation Illustration

CBO unit (for Cu target only)
Applicable to Cu wavelength, and
enables the switching between
divergent and parallel beams.
CBO（Cu）

CBO unit (for Cu and Co targets)

(optional: 9999)
Applicable to both Cu and Co
wavelengths, and enables the
switching between divergent and CBO(Cu/Co)
parallel beams.

CBO-E unit (for Cu target only)

(optional: 9999)
Applicable to Cu wavelength, and
enables the switching between
divergent and convergent beams. CBO-E

SmartLab: Automated Multipurpose X-ray Diffractometer 25

Optics

1 Attach the CBO unit to the shutter. Press the CBO unit against the
surface in the back and secure the unit in place with the Allen wrench
provided.

2 Insert the cable into the CBO connector of the incident connector box.

26 SmartLab: Automated Multipurpose X-ray Diffractometer

 CBO unit (for Cu target)

3 Insert a selection slit into the slit box of the CBO unit.

SmartLab: Automated Multipurpose X-ray Diffractometer 27

Optics

Table Selection slits

Corresponding
Name of optics Abbreviation Illustration
CBO

CBO(Cu)
For para-focusing CBO(Cu/Co) BB
CBO-E

For para-focusing（Co）
(included in the CBO (Cu/Co) CBO(Cu/Co) BB Co
unit)

For parallel beam

CBO(Cu)
(included in the CBO(Cu) and PB
CBO(Cu/Co)
CBO(Cu/Co) units)

For convergent beam

CBO-E CB
(included in the CBO-E unit)

For micro area measurements CBO(Cu)

PB03
(option: 2431C302) CBO(Cu/Co)

For small-angle scattering

CBO(Cu)
measurements SA
CBO(Cu/Co)
(option: 2680J111)

CBO(Cu)
For micro area measurements
CBO(Cu/Co) MA
(option: 2680G111)
CBO-E

For small-angle scattering CBO(Cu)

high-intensity measurements SA01
(option: 9999) CBO(Cu/Co)

The type of selection slit installed can be identified from SmartLab Guidance.

28 SmartLab: Automated Multipurpose X-ray Diffractometer

 CBO unit (for Cu target)

Table Selection slits for micro area measurements (option)

Name of optics Size Abbreviation Illustration

Parallel beam
φ0.3 mm PB03
(2431C302)

Parallel beam
φ0.1 mm PB01
(2431C301)

Point source x-rays*1

φ0.3 mm BB03
(2431C202)

Point source x-rays*1

φ0.1 mm BB01
(2431C201)

*1 : Switchable to the point source x-rays only using the sealed tube type
(2080B211/2080B212/2080B411).

The type of selection slit installed can be identified from SmartLab Guidance.
Above selection slits is used in combination with a collimator as a double pinhole
collimator.

SmartLab: Automated Multipurpose X-ray Diffractometer 29

Optics

Incident optics unit (standard incident optics unit)

Install an optical device to condition the incident x-ray beam.
Select an optical device from three types: parallel slit, 2-bounce monochromator,
and 4-bounce monochromator.

Incident parallel slit adaptor (IPS adaptor)

This adaptor is used to install a parallel slit.

Incident parallel slit adaptor

1 Install the incident parallel slit adaptor to the CBO unit by sliding it
down from the top section of the CBO unit. Secure it in place with the
Allen wrench provided.

30 SmartLab: Automated Multipurpose X-ray Diffractometer

 Incident optics unit (standard incident optics unit)

2 Connect the cable to the MONO/ADPT connector on the incident

connector box.

3 Install the parallel slit on the adaptor and secure it in place with the
Allen wrench provided

SmartLab: Automated Multipurpose X-ray Diffractometer 31

Optics

Table Incident parallel slits

Divergence
Type Abbreviation Illustration
limit angle

Open
None Soller_Slit_open
(option: 2680D115)

Soller slit 5º Soller_Slit_5.0 deg

Soller slit
2.5º Soller_Slit_2.5 deg
(option: 2680D114)

In-plane PSC
(Parallel Slit Collimator) 1.0º In-plane_PSC_1.0 deg
(option: 2680D113)

In-plane PSC
0.5º In-plane_PSC_0.5 deg
(option: 2680D112)

In-plane PSC
0.15º In-plane_PSC_0.15 deg
(option: 2680D111)

The type of installed incident parallel slit can be identified from SmartLab Guidance.

32 SmartLab: Automated Multipurpose X-ray Diffractometer

 Incident optics unit (standard incident optics unit)

2-bounce monochromator (option)

This optical device produces a monochromatized x-ray beam using a 2-bounce

channel cut crystal.
Fine alignment of the channel cut crystal are performed from SmartLab
Guidance.
A dedicated parallel slit can be installed after the channel cut crystal.

2-bounce monochromator

1 Attach the 2-bounce monochromator to the CBO unit by sliding it

down from the top section of the CBO unit. Secure it in place with the
Allen wrench provided.

SmartLab: Automated Multipurpose X-ray Diffractometer 33

Optics

2 Connect the cable to the MONO/ADPT connector on the incident

connector box.

3 Install a parallel slit on the 2-bounce monochromator. Secure it in

place with the Allen wrench provided.

34 SmartLab: Automated Multipurpose X-ray Diffractometer

 Incident optics unit (standard incident optics unit)

Table 2-bounce monochromators

Diffraction
Crystal Abbreviation Illustration
plane

Ge
220 Ge(220)x2
(option: 2680B111)

Ge
400 Ge(400)x2
(option: 2680B112)

The type of installed crystal can be identified from SmartLab Guidance.

Table Parallel slits for 2-bounce monochromator

Type Divergence Abbreviation Illustration

Open
None Soller_slit_open
(provided with the unit)

Soller slit
5.0º Soller_slit_5.0 deg
(option: 2680D213)

Soller slit
2.5º Soller_slit_2.5 deg
(option: 2680D212)

In-plane PSC
0.5º In-plane_PSC_0.5 deg
(option: 2680D211)

The type of parallel slit installed on the adaptor can be identified from SmartLab Guidance.

SmartLab: Automated Multipurpose X-ray Diffractometer 35

Optics

4-bounce monochromator (option)

This optical device produces a monochromatized x-ray beam using two

2-bounce channel cut crystals.
Fine alignment of the channel cut crystals can be performed from SmartLab
Guidance.

4-bounce monochromator

1 Attach the 4-bounce monochromator to the CBO unit by sliding it

down from the top section of the CBO unit. Secure it in place with the
Allen wrench provided.

36 SmartLab: Automated Multipurpose X-ray Diffractometer

 Incident optics unit (standard incident optics unit)

2 Connect the cable to the MONO/ADPT connector on the incident

connector box.

Table 4-bounce monochromators

Diffraction
Crystal Abbreviation Illustration
plane

Ge
220 Ge(220)x4
(option: 2680B211)

Ge
440 Ge(440)x4
(option: 2680B212)

The type of installed crystal can be identified from SmartLab Guidance

SmartLab: Automated Multipurpose X-ray Diffractometer 37

Optics

CBO-f unit (option: 2220C301)

Converges the parallel beam in the longitudinal direction onto the sample. The
optical device is used for the measurements of micro amount of a sample and of
micro area.
Fine alignment of the CBO-f unit is performed from SmartLab Guidance.

CBO-f unit

1 Install the CBO-f unit to the theta_s arm from the top, and secure it in
place with the Allen wrench provided.

38 SmartLab: Automated Multipurpose X-ray Diffractometer

 Incident optics unit (standard incident optics unit)

2 Connect the cable to the MONO/ADPT connector on the incident

connector box.

The type of installed crystal can be identified from SmartLab Guidance.

SmartLab: Automated Multipurpose X-ray Diffractometer 39

Optics

Incident slit box

This variable slit box is installed on the Zs axis on the theta_s arm.

Standard incident slit box

This slit box adjusts the slit width to control the beam divergence angle (for the
para-focusing method) or the beam width (for the parallel beam method). For
small-angle scattering measurements, this slit guards against parasitic scattering.
A length-limiting slit can also be inserted to limit the beam length along the
longitudinal axis.

Standard incident slit box

1 Attach the standard incident slit box to the Zs axis. Secure it in place
with the Allen wrench provided.

40 SmartLab: Automated Multipurpose X-ray Diffractometer

 Incident slit box

2 Connect the cable to the SLIT connector on the incident connector box.

3 Insert a length-limiting slit to control beam length along the

longitudinal axis.

SmartLab: Automated Multipurpose X-ray Diffractometer 41

Optics

Table Length-limiting slits

Length of limiting slit Abbreviation Illustration

15 mm 15

10 mm 10

5 mm 5

2 mm 2

0.5 mm
micro area optics 0.5
(option: 2680G111)

The type of inserted length-limiting slit can be identified from SmartLab Guidance.

Collimator holder (option)

Some types of pinhole collimators can be installed for micro area measurements.
Kβ filter for Cu can also be installed (optional).

Table Collimator holder

Name Usage Illustration

PB collimator holder Used in combination with

(2431D201) multilayer mirror or CBO-f unit.

BB collimator holder
Used in point focus optics.
(2431D101)

42 SmartLab: Automated Multipurpose X-ray Diffractometer

 Incident slit box

Table Incident filter (option)

Name Illustration

Absorber case
(2431H101)

Kβ filter for Cu
(2431H201)

Kβ filter for various wavelength can be supplied. Please contact the sales representative who
you purchased the instrument from.

SmartLab: Automated Multipurpose X-ray Diffractometer 43

Optics

1 Install the collimator holder to the Zs axis and secure it in place with
the Allen wrench provided.

2 Connect the cable to the SLIT connector on the incident connector box.

44 SmartLab: Automated Multipurpose X-ray Diffractometer

 Incident slit box

3 Insert the pinhole collimator into the collimator holder.

Table Pinhole collimators (option)

Pinhole diameter Abbreviation Illustration

φ 0.2 mm
0.2
(2431E103)

φ 0.1 mm
0.1
(2431E102)

φ 0.05 mm
0.05
(2431E101)

CAUTION Do not use the pinhole collimator (option) with the XY-4” phi attachment.
When using the pinhole collimator with the XY-4” phi attachment, the end of
the pinhole collimator collides with the sample and/or the sample plate from
the translation of X and Y axes, and thus the pinhole collimator, the sample,
and the sample stage may become damaged.

The type of inserted pinhole collimator can be identified from SmartLab Guidance.

SmartLab: Automated Multipurpose X-ray Diffractometer 45

Optics

Receiving slit box # 1

This slit box is installed on the sample side of the theta_d arm.

Standard receiving slit box # 1

For para-focusing optics, this slit box controls the anti-scatter slit width to
reduce the level of background scatter from the sample. For parallel beam optics,
it functions as the first slit in a double-slit receiving system.
The slit width can be controlled from SmartLab Guidance. A Kβ filter can be
inserted to remove Kβ x-rays from characteristic x-rays.

Standard receiving slit box # 1

1 Attach the standard receiving slit box # 1 to the rail of the theta_d arm.
Secure it in place with the Allen wrench provided.

46 SmartLab: Automated Multipurpose X-ray Diffractometer

 Receiving slit box # 1

2 Connect the cable to the SLIT1 connector on the receiving connector

box.

3 A Kβ filter may be inserted.

Check whether a Kβ filter is inserted from SmartLab Guidance.

Kβ filter (Ni foil)

The Kβ filter reduces the Kβ characteristic x-rays by approximately 90% while only
reducing the Ka characteristic x-rays by approximately 50%. Therefore almost all Kβ x-rays
can be removed. (Used for measurements based on the para-focusing method.)

SmartLab: Automated Multipurpose X-ray Diffractometer 47

Optics

4 The installation position can be read from the scale on the theta_d arm.

48 SmartLab: Automated Multipurpose X-ray Diffractometer

 Receiving optics unit # 1

Receiving optics unit # 1

This unit attaches after receiving slit box # 1. A parallel slit analyzer or 2-bounce
crystal analyzer can be installed on receiving optics unit # 1.

Receiving optical device adaptor (ROD adaptor)

This adaptor is used to install a parallel slit analyzer (PSA). A parallel slit
analyzer is installed so that the plates inside are mounted horizontally thereby
providing angular resolution for the theta_d axis.

Receiving optical device adaptor

1 Attach the receiving optical device adaptor to the rail of the theta_d
arm. Secure it in place with the Allen wrench provided.

SmartLab: Automated Multipurpose X-ray Diffractometer 49

Optics

2 Connect the cable to the ADPT1 connector on the receiving connector

box.

3 Attach a parallel slit analyzer to the adaptor. Secure it in place with the
Allen wrench provided.

50 SmartLab: Automated Multipurpose X-ray Diffractometer

 Receiving optics unit # 1

Table Parallel slit analyzers

Aperture angle Length Abbreviation Illustration

Open 45 mm PSA_open

1.0º
45 mm PSA_1.0 deg
(option: 2680F113)

0.5º 45 mm PSA_0.5 deg

0.114º
90 mm PSA_0.114 deg
(option: 2680F111)

Open 90 mm PSA_open

The standard configuration of SmartLab cannot incorporate either the PSA 0.114
deg. or PSA open (90 mm) in conjunction with a receiving parallel slit. In order to
do this, the configuration must be modified by, moving the receiving parallel slit
adaptor, standard slit box # 2, attenuator, and detector (counter) to the right.

The type of parallel slit analyzer installed on the adaptor can be identified from SmartLab
Guidance.

SmartLab: Automated Multipurpose X-ray Diffractometer 51

Optics

2-bounce analyzer (option)

The 2-bounce channel cut analyzer provides increased resolution on the 2-theta
axis by only allowing diffracted x-rays that satisfy the diffraction condition for
the analyzer crystal to enter the detector.
Fine alignment of the channel cut crystal can be performed from SmartLab
Guidance.

2-bounce analyzer

1 Attach the 2-bounce analyzer to the theta_d arm. Secure it in place

with the Allen wrench provided.

52 SmartLab: Automated Multipurpose X-ray Diffractometer

 Receiving optics unit # 1

2 Connect the cable to the ADPT1 connector on the receiving connector

box.

Table Crystal types

Crystal Diffraction plane Abbreviation Illustration

Ge
220 Ge(220)x2
(option: 2680C111)

Ge
400 Ge(400)x2
(option: 2680C112)

The type of crystal currently installed can be identified from SmartLab Guidance.

SmartLab: Automated Multipurpose X-ray Diffractometer 53

Optics

Receiving optics unit # 2

This unit attaches to before receiving slit box # 2. A parallel slit can be installed
in receiving optics unit # 2.

Receiving parallel slit adaptor (RPS adaptor)

This adaptor is used to install a parallel slit.

A parallel slit is installed so that the plates inside are mounted vertically
controlling axial divergence for the theta_d axis.

Receiving parallel slit adaptor

1 Attach the receiving parallel slit adaptor to the rail of the theta_d arm.
Secure it in place with the Allen wrench provided.

54 SmartLab: Automated Multipurpose X-ray Diffractometer

 Receiving optics unit # 2

2 Connect the cable to the ADPT2 connector on the receiving connector

box.

3 Attach a parallel slit to the adaptor. Secure it in place with the Allen
wrench provided.

SmartLab: Automated Multipurpose X-ray Diffractometer 55

Optics

Table Receiving parallel slits

Aperture
Type Abbreviation Illustration
angle

Soller slit 5.0º Soller_slit_5.0 deg

Soller slit
2.5º Soller_slit_2.5 deg
(option: 2680F114)

In-plane PSA
1.0º In-plane_PSA_1.0 deg
(option: 2680F113)

In-plane PSA
0.5º In-plane_PSA_0.5 deg
(use of PSA 0.5 deg.)

In-plane PSA
(use of PSA 0.114 deg.) 0.114º In-plane_PSA_0.114 deg
(option: 2680F111)

The type of parallel slit currently installed on the adaptor can be identified from SmartLab
Guidance.

56 SmartLab: Automated Multipurpose X-ray Diffractometer

 Receiving slit box # 2

Receiving slit box # 2

This slit box is installed in from of the detector on the theta_d arm.

Standard receiving slit box # 2

The standard receiving slit box # 2 contains the variable receiving slit and
controls measurement resolution in the para-focusing and double-slit receiving
configurations.
If a double-slit receiving system is used, it will function as the second slit.
Slit width and vertical position can be controlled from SmartLab Guidance.

Standard receiving slit box # 2

1 Attach the standard receiving slit box # 2 to the rail of the theta_d arm.
Secure it in place with the Allen wrench provided.

SmartLab: Automated Multipurpose X-ray Diffractometer 57

Optics

When using the para-focusing method, set the installation position to 300 mm.

2 Connect the cable to the SLIT2 connector on the receiving connector

box.

58 SmartLab: Automated Multipurpose X-ray Diffractometer

 Attenuator

Attenuator
The attenuator adjusts the intensity of the detected x-rays.

Standard attenuator

The system uses several types of attenuators on a rotating disc. Attenuators for
optics alignment are also built-in.
The type of attenuator can be switched from SmartLab Guidance. Attenuators
can be switched automatically for various measurements based on detected
intensity.

Standard attenuator

1 Attach the standard attenuator to the rail of the theta_d arm. Secure it
in place with the Allen wrench provided.

SmartLab: Automated Multipurpose X-ray Diffractometer 59

Optics

2 Connect the cable to the ATT connector on the receiving connector box.

The attenuator types used during actual measurements are as follows: Open, 1/70, 1/1000,
1/10000. The attenuator types used during alignments are as follows: 9 kWBB, 9 kWPB, 3
kWBB, 3 kWPB for alignment.

60 SmartLab: Automated Multipurpose X-ray Diffractometer

 Receiving optics unit CALSA (option: 2680K201)

Receiving optics unit CALSA (option: 2680K201)

CALSA is a multi-crystal analyzer, which is used by installing onto the theta_d
arm. It achieves the ultrahigh resolution of the X-ray diffraction beam from a
sample.
The positions of the analyzer crystals and detector can be aligned from
SmartLab Guidance.

CALSA

1 Remove all the units installed on the theta_d arm.

2 Attach CALSA on therail of the theta_d arm and set the installation
position to 200 mm. The position can be read from the scale on the
theta_d arm.

SmartLab: Automated Multipurpose X-ray Diffractometer 61

Optics

3 Secure it in place with the Allen wrench provided.

4 Connect the ADPT1, ADPT2, and SLIT2 cable to the ADPT1, ADPT2,
and SLIT2 connector on the receiving connector box.

62 SmartLab: Automated Multipurpose X-ray Diffractometer

 Receiving optics unit CALSA (option: 2680K201)

Receiving parallel slit

Install the parallel slit in a manner such that the stacking direction of the foils
should be the same as the direction of the theta_d axis scan (the direction of
axial divergence).

SmartLab: Automated Multipurpose X-ray Diffractometer 63

Optics

Table Receiving parallel slit

Type Aperture angle Abbreviation Illustration

Soller slit 5.0º Soller slit 5.0 deg

Soller slit 2.5º Soller slit 2.5 deg

(option)

In-plane PSA 1.0º In-plane PSA 1.0 deg

(option)

In-plane PSA 0.5º In-plane PSA 0.5 deg

(use of PSA 0.5 deg)

In-plane PSA 0.114º In-plane PSA 0.114 deg

(use of PSA 0.114 deg)

The type of the parallel slit installed on the adaptor can be identified from SmartLab
Guidance.

64 SmartLab: Automated Multipurpose X-ray Diffractometer

 Receiving optics unit CALSA (option: 2680K201)

CALSA beam conditioner

The slit, attenuator, and knife edge are prepared to be used with CALSA.
Insert the beam conditioner into CALSA to condition the X-ray beams.

Table Beam conditioner

Type Abbreviation Use Illustration

Knife edge KE Cuts off the
scattering X-rays
from the sample in
data measurements.

reference Receiving ARS Used for the 2-theta

slit axis alignment in
optics alignment.

Attenuator ATT 9 kW Used to attenuate the

or ATT 3 kW X-ray intensity in
optics alignment.

The type of the beam conditioner inserted into CALSA can be identified from SmartLab
Guidance.

SmartLab: Automated Multipurpose X-ray Diffractometer 65

Optics

Dtector (D/teX Ultra)

Detects X-rays diffracted from CALSA.

D/teX Ultra

1 Connect the power cable and LAN cable to D/teX Ultra.

2 Attach D/teX Ultra to the detector adaptor of CALSA. Secure it in

place with the Allen wrench provided.

66 SmartLab: Automated Multipurpose X-ray Diffractometer

 Detector

Detector adaptor
Used to attach the detector.

Detector adaptor

1 Attach the detector adaptor to the rail of the theta_d arm. Secure it in
place with the Allen wrench provided.

SmartLab: Automated Multipurpose X-ray Diffractometer 67

Detector

2 Connect the cable to the COUNTER connector on the receiving

connector box.

68 SmartLab: Automated Multipurpose X-ray Diffractometer

 Scintillation counter

Scintillation counter
The scintillation counter is attached to the detector adaptor. It detects x-rays
received by the receiving optics.

Check whether the scintillation counter is installed from SmartLab Guidance.

Scintillation counter

1 When detecting x-rays from the receiving optics directly (in absence of
the diffracted beam monochromator), install the scintillation counter
to the base with the Allen wrench provided.

SmartLab: Automated Multipurpose X-ray Diffractometer 69

Detector

2 Attach the base to the detector adaptor. Secure it in place with the
Allen wrench provided.

3 The installation position can be read from the scale on the theta_d arm.

70 SmartLab: Automated Multipurpose X-ray Diffractometer

 DBM unit for Cu (option: 2726H112)

DBM unit for Cu (option: 2726H112)

This unit is used to monochromatize the diffracted beam such that only Kα
x-rays are detected.
Change the curvature of the monochromating crystal from Bent (para-focusing
geometry) to Flat (parallel beam geometry) by rotating the dial on the top of the
monochromator housing.

Changeover dial

DBM (diffracted beam monochromator) unit for Cu

Diffracted beam monochromator unit using Cu for para-focusing optics only (Bent only) can
be supplied (2726H113).

1 Install the scintillation counter on the diffracted beam monochromator

unit. Secure it in place with the Allen wrench provided.

SmartLab: Automated Multipurpose X-ray Diffractometer 71

Detector

2 Install the unit on the detector adaptor. Secure it in place with the
Allen wrench provided.

3 The unit installation position can be read from the scale on the theta_d
arm.

When using the monochromator in Bent mode with para-focusing optics, the unit
must be installed at a specific position for a specific target given in the table below.
When using the monochromator in Flat mode, the exact position is not important.
Type of target Installation position
Cu 351.5 mm
Co 359.8 mm
Fe 364.7 mm
Cr 376.1 mm

72 SmartLab: Automated Multipurpose X-ray Diffractometer

 DBM unit for Cu (option: 2726H112)

4 Insert the monochromator slit (RSm) into the unit.

The presence/absence of the slit can be confirmed from SmartLab
Guidance.

Use the RSm only when using the monochromator in Bent mode for the
para-focusing method. The RSm is not used when using the monochromator in Flat
mode.

SmartLab: Automated Multipurpose X-ray Diffractometer 73

Detector

D/teX Ultra (option: 5741A300)

D/teX Ultra is a 1D detector in which small detecting devices are arranged.
Since D/teX Ultra detects x-ray intensity efficiently, the diffraction peaks of
minor components can be detected with a high speed scan.
D/teX Ultra should be installed to the detector adaptor. Check whether D/teX
Ultra is installed from SmartLab Guidance.

D/teX Ultra

1 When detecting x-rays from the receiving optics directly (in absence of
the diffracted beam monochromator), install D/teX Ultra to the base
with the Allen wrench provided.

2 Remove the receiving optical device adaptor (see Receiving optical

device adaptor (ROD adaptor)), move the receiving parallel slit
adaptor (see Receiving parallel slit adaptor (RPS adaptor)), standard
receiving slit box 2 (see Standard receiving slit box # 2), and standard
attenuator (see Standard attenuator) to the incident side, and then
install the detector adaptor.

74 SmartLab: Automated Multipurpose X-ray Diffractometer

 D/teX Ultra (option: 5741A300)

3 Install the base to the detector adaptor, and secure it in place with the
Allen wrench provided.

When the measurement is made in para-focusing optics, install the detector adaptor
at position 351 mm

Detector position

4 Connect the power cable and communication cable to the connector on

the back of D/teX Ultra. Before connecting the cables, press the “O”
OFF button to turn off the power of SmartLab.

SmartLab: Automated Multipurpose X-ray Diffractometer 75

Detector

DBM unit for Cu for D/teX Ultra (option: 2726P101)

This unit is used to monochromatize the diffracted beam such that only Kα
x-rays are detected.

DBM (diffracted beam monochromator) unit for Cu (for D/teX Ultra)

1 Install D/teX Ultra on the diffracted beam monochromator unit.

Secure it in place with the Allen wrench provided.

76 SmartLab: Automated Multipurpose X-ray Diffractometer

 DBM unit for Cu for D/teX Ultra (option: 2726P101)

2 Remove the receiving optical device adaptor (see Receiving optical

device adaptor (ROD adaptor)), receiving parallel slit adaptor (see
Receiving parallel slit adaptor (RPS adaptor)),standard receiving slit
box # 2 (see Standard receiving slit box # 2)), and standard attenuator
(see Standard attenuator).

3 Install the unit on the detector adaptor. Secure it in place with the
Allen wrench provided.

When the measurement is made in para-focusing optics, install the detector adaptor
at position 351 mm.

Detector position

SmartLab: Automated Multipurpose X-ray Diffractometer 77

Detector

PILATUS (option: 5742A101)

PILATUS is a low-noise high-sensitivity semi-conductor hybrid 2D detector.
Attach PILATUS to the PILATUS holder and install the PILATUS holder
(2431J101) to SmartLab, PILATUS can be placed either vertically or
horizontally.

Installation of PILATUS (left: horizontal, right: vertical)

78 SmartLab: Automated Multipurpose X-ray Diffractometer

 Sample Stage
To move the sample up and down, Z axis is installed on the SmartLab goniometer.
This mechanism enables the sample surface to be adjusted when using a sample
stage or an attachment.

Sample height alignment unit

Sample stages can be installed to the sample height alignment unit. To install a
sample stage, join the stage with the rail of the sample height alignment unit as
shown in the following figure, and slide it from top down. Make sure that the stage
is placed horizontally and secure it in place with the Allen wrench provided.

The direct beam stopper (option: provided with 5741A300) and knife edge (option:
2431G101) can also be installed to the sample height alignment unit. They will
reduce the background intensity in high-speed measurements using D/teX Ultra.

Direct beam stopper

SmartLab: Automated Multipurpose X-ray Diffractometer 79

Sample Stage

Standard sample stage

This can be used in combination with attachments.

Standard sample stage

β sample stage (option: 2430B101)

This can be used in combination with attachments.
The rotational axis (β) on the sample surface plane enables to perform
measurements by rotating the sample thereby reducing preferred orientation.

β sample stage

80 SmartLab: Automated Multipurpose X-ray Diffractometer

 ASC-6 (option: 2430H101)

ASC-6 (option: 2430H101)

Consecutive measurements can be performed by switching the six samples
mounted on the turntable.
The rotational axis (βs) on the sample surface plane enables to perform
measurements by rotating the sample thereby averaging the variation of particle
sizes.

Knife edge

Auto sample changer (ASC-6)

Table Standard accessories

Name Illustration
Al sample holder with base 0.5
for ASC
（2455E445）

Height alignment jig for ASC

General-purpose knife edge (optional : 2431G101) will be required to perform

measurements in the reflection geometry using a knife edge. If you own the
optional accessories for measurements in the vertical transmission geometry, the
general knife edge is not necessary.
General-purpose knife edge

SmartLab: Automated Multipurpose X-ray Diffractometer 81

Sample Stage

For vertical transmission geometry (option: 2455H105)

Measurements in the vertical transmission geometry can be performed when the

convergent beam optics using the CBO-E unit is available. The transmission film
sample holder (2455E463) is also necessary for this measurement.
Loosen the left lever and rotate the turntable 180 degrees clockwise for the
vertical transmission geometry.

Incident knife edge (INC. KE）

Center slit for ASC

Receiving knife edge (REC. KE)

Direct beam stopper (DBS)

Switch to the vertical transmission geometry

When measurements are performed in the reflection geometry using a knife edge,
install the reflection knife edge (REF. KE) to the extended base for ASC as shown
below.

Reflection knife edge (REF. KE)

82 SmartLab: Automated Multipurpose X-ray Diffractometer

 ASC-6 (option: 2430H101)

Table Accessories

Name Illustration

Transmission film sample holder

Center slit for ASC

Incident knife edge(INC. KE)

Extended base for ASC

Direct beam stopper (DBS)

Receiving knife edge (REC. KE)

Reflection knife edge (REF. KE)

Mylar foil －

SmartLab: Automated Multipurpose X-ray Diffractometer 83

Sample Stage

AntonPaar sample stage

Measurements can be performed using the AntonPaar sample stages equipped
with temperature adjustment mechanism. The stages are: HTK1200N, HTK16,
HTK2000, XRK900, TTK450, and CHC. For information of how to use the
sample stage and pipe arrangement, refer to the instruction manual of each stage.

AntonPaar sample stage adaptor

HTK16 CHC

Installation of the AntonPaar sample stages

84 SmartLab: Automated Multipurpose X-ray Diffractometer

 Attachments
You can switch between attachments with various adjust axes for different
measurement purposes.
Described below is the method for changing attachments.

1 Click Manual Control under the Control menu. Move the chi axis to 0°
and the phi axis to 0°.

2 Release the hook.

3 Open the clasps for the right and left sides. Remove the attachment.

Pin

Clasps

Hook

4 Make sure the right and left clasps are open.

5 Install the attachment by aligning the groove of the attachment with

the pin on the front.

6 Close the clasps and engage the front hook.

SmartLab: Automated Multipurpose X-ray Diffractometer 85

Attachments

Table Types of attachments

Name Description Description

This attachment has no moving
axis.
It is used for reflectivity
Standard attachment measurements and measurements
of powder and bulk samples.

This attachment has Rx and Ry

axes that permit tilt adjustments of
two axes intersecting at right
RxRy attachment angles.
(option: 2680A213)
It is used for RSM measurements
and various types of in-plane
measurements.
This attachment has +/– 10 mm X
and Y translation axes which are
perpendicular to each other.
XY-20 attachment It is used to position the sample
(option: 2680A211) for micro area measurements.
This attachment cannot be used
with 8-inch wafer sample plates.
This attachment has +/– 50 mm
provides X and Y translation axes
which are perpendicular to each
XY-4” phi attachment other. It is used for full-map
(option: 2680A212) measurement of 4-inch wafers.
This attachment can be used only
with the 4-inch XY mapping
sample plate.
This attachment is used to spin the
sample filled in a capillary during
measurements.
Capillary spin attachment
(option: 2430C101)

CAUTION Do not use the pinhole collimator (option) with the XY-4” phi attachment.
When using the pinhole collimator with the XY-4” phi attachment, the end of
the pinhole collimator collides with the sample and/or the sample plate from
the translation of X and Y axes, and thus the pinhole collimator, the sample,
and the sample stage may become damaged.

The type of attachment installed can be identified from SmartLab Guidance.

86 SmartLab: Automated Multipurpose X-ray Diffractometer

 Sample Plates
Select a sample plate based on the sample to be measured.

Height reference sample plate

Insert a glass sample holder or aluminum sample holder into the height reference
sample plate.
Place the height reference sample plate directly on the attachment.
To make adjustments, insert a center slit and Si powder reference sample.

Height reference sample plate

Transmission SAXS sample plate (option: 2680J111)

A transmission SAXS sample holder is inserted into the transmission SAXS
sample plate.
The transmission SAXS sample plate is placed directly on the attachment.

Transmission SAXS sample plate

・ Normally the height reference sample plate and transmission SAXS sample plate
should be used on top of the standard attachment. If using the height reference sample
plate or transmission SAXS sample plate with an attachment other than the standard
attachment, you must set each attachment axis to 0.

・ To install/remove each sample plate to/from an attachment, see Installing and removing
wafer sample plates.

SmartLab: Automated Multipurpose X-ray Diffractometer 87

Sample Plates

Capillary holder (option: 2430C101)

The capillary holder is used to mount the capillary sample onto the capillary spin
attachment. The capillary sample is spanned with the rotation (ωc) axis during
measurements. Attach the capillary sample to the capillary holder and mount the
holder to the capillary spin attachment. The prepared sizes of the holder are φ1.0
mm, φ0.7 mm, etc. Use the appropriate size for the capillary to be used.

Capillary spin attachment and capillary holder

Wafer sample plates and sample spacers

A wafer sample plate is used in measurements of wafer-shaped samples. A
sample spacer is placed on the attachment. The wafer sample plate is placed on
the sample spacer. A sample is placed on top of the wafer sample plate. Wafer
sample plates and sample spacers are available for 4-inch, 6-inch, and 8-inch
samples.

Wafer sample plate and sample spacer

CAUTION Placing a sample larger than the sample plate may damage the sample during
measurement.

88 SmartLab: Automated Multipurpose X-ray Diffractometer

 Wafer sample plates and sample spacers

Magnets supplied with the product are generally used to secure the sample in
place. For information on how to mount samples, see Wafer-shaped samples.

Magnets for securing sample in place

The sample holding magnets can be used for samples measuring up to approximately
3 mm in thickness.

The Z axis is used to align the sample surface with the center of the x-ray beam.
Since the thickness range for which the Z axis can be adjusted is 3 mm, you
must select the appropriate sample spacer based on the thickness of the sample
to be measured.

Table Sample spacers

Measurable sample thickness Abbreviation Illustration

0～3 mm
0-3 mm
(option: 2680A406)

3～6 mm
3-6 mm
(option: 2680A405)）

6～9 mm
6-9 mm
(option: 2680A404)

9～12 mm 9-12 mm
(option: 2680A403) 0-3 mm(blue stamped mark)

12～15 mm
12-15 mm
(option: 2640A402)
0-3 mm(blue stamped mark)
0～3 mm(*1)
15 mm～18 mm
15-18 mm
(option: 2680A401)
3-6 mm(blue stamped mark)
3～6 mm(*1)
*1: Sample thickness for using XY-4” φ attachment. Refer to the abbreviations in blue.

SmartLab: Automated Multipurpose X-ray Diffractometer 89

Sample Plates

Table Wafer sample plates

Name Illustration

4-inch wafer sample plate

(option: 2680A301)

6-inch wafer sample plate

(option: 2680A302)

8-inch wafer sample plate

(option: 2680A303)

4-inch wafer sample plate

(for 18-21 mm)
(option: 2680A301)
4-inch XY mapping sample plate
(provided with XY-4”φ attachment)
4-inch XY mapping sample plate
(for 6-9 mm)
(option)

Table List of possible combinations of attachment, sample spacer, and sample plate

Measurable
Attachment Sample spacer Sample plate
sample thickness
0-3 mm
3-6 mm 4-inch wafer sample plate 0-3 mm
6-9 mm 3-6 mm
6-inch wafer sample
9-12 mm 6-9 mm
plate(*1)
12-15 mm 9-12 mm
15-18 mm 8-inch wafer sample 12-15 mm
Standard attachment plate(*1)
RxRy attachment (black stamped 15-18 mm
XY-20 mm attachment mark)
4-inch wafer sample plate (for 18-21 mm) 18-21 mm
4-inch wafer sample plate
6-inch wafer sample plate(*1) 21-24 mm
8-inch wafer sample plate(*1)
0-3 mm
3-6 mm 4-inch area mapping sample 0-3 mm
(blue stamped plate 3-6 mm
XY-4"φ attachment mark)(*2)
4-inch XY mapping sample plate (for 6-9 mm) 6-9 mm
4-inch XY mapping sample plate 9-12 mm
*1: Both X and Y must be 0 mm when the sample is placed on the XY-20 mm attachment.
*2: When the XY-4” φ attachment is used, the thickness indicated by the blue stamp mark on the sample spacer is valid.

90 SmartLab: Automated Multipurpose X-ray Diffractometer

 Wafer sample plates and sample spacers

Installing and removing sample spacers

To mount a sample spacer to an attachment, align the sections indicated by the

arrows in the figure below, then turn the sample spacer clockwise to secure it in
place.

Installing the sample spacer on the attachment

To remove the sample spacer from the attachment, apply pressure to the bar
indicated by the arrow in the figure below, then turn the sample spacer
counterclockwise.

Removing the attachment

SmartLab: Automated Multipurpose X-ray Diffractometer 91

Sample Plates

Installing and removing wafer sample plates

To mount a wafer sample plate to a sample spacer, align the sections indicated
by the arrows in the figure below, then turn the sample plate clockwise to secure
it in place.
The wafer sample plate can be removed by turning it counterclockwise.

Installing/removing the wafer sample plate

See Installing and removing sample spacers for information on direct mounting (removing)
a wafer sample plate to (from) an attachment.

92 SmartLab: Automated Multipurpose X-ray Diffractometer

 Sample Holders
Use a sample holder when measuring samples that require preparation, such as
powder and bulk samples.

For information on preparing samples, refer to Section 2.8 of the “Quick theta/2-theta
measurement (BB)” or “Quick theta/2-theta measurement (PB/PSA)” Help Topic of the
online help section of the SmartLab Guidance software.

Glass sample holder

Use this sample holder to measure powder samples.

Glass sample holder

Aluminum sample holder

Use this sample holder to measure powder samples or small bulk samples.

Aluminum sample holder

Transmission SAXS sample holder (option: 2680J111)

Use this sample holder to measure fibrous or film samples by the transmission
method.

Transmission SAXS sample holder

SmartLab: Automated Multipurpose X-ray Diffractometer 93

 Column
Cross beam optics(CBO)
CBO is an optical system which easily switches between the divergent beam used in measurements in para-focusing
optics and the parallel beam conditioned by multilayer mirror, by replacing the selection slits. As shown in the
diagram, selection slit (BB) uses x-rays passing through optical path A, while selection slit (PB) uses x-rays passing
through optical path B. In SmartLab, the multilayer mirror is designed so that optical path A and optical path B
intersect at the center (goniometer center) of the sample at a distance of 300 mm from the x-ray focal point. There is
no need to remove the multilayer mirror when switching from parallel beam optics to para-focusing optics. Simply
change the selection slits and perform 2-theta axis adjustment one time.

Selection
選択スリット(BB)slit (BB)
X-ray
X 線源 source
（フィラメント）
Sample
試料

Optical
Opticalpath
path
光路AA(divergent
(divergentbeam)
A（発散ビーム） beam)

Selection slit (PB)

選択スリット(PB) Sample
X X-ray source
線源（フィラメント） 試料

Optical path
光路 B（平行ビーム）
B (parallel beam)

Switching between para-focusing optics and parallel beam optics by changing selection slits

CBO-E keeps the CBO feature which makes the optical paths A and B intersect on the sample. The only difference
is that the shape of the multilayer mirror used in the CBO-E unit is ellipsoidal while the mirror shape used for CBO
is parabolic.
The ellipsoidal multilayer mirror used in CBO-E has been designed so that one focus of the ellipsoid is placed at the
focus of the x-ray source and the other focus of the ellipsoid falls on the detector plane. When measuring capillary
samples or samples on the transmission SAXS sample plate in the transmission geometry, the measurement can be
performed very efficiently if a 1D detector like D/teX Ultra is used in combination. The CBO-E unit also switches
between measurements in the reflection geometry in para-focusing optics and those in the transmission geometry in
convergent optics. In both cases, D/teX Ultra enables very efficient measurements.

Detector position

X-ray source
Sample

Optical path B (convergent beam)

Selection slit (CB)

Diagram of the optics using CBO-E

 Accessories
Table Accessories

Name Illustration

Center slit

Si powder reference sample

Si wafer reference sample

Tool for installation of optical

devices (Allen wrench)

SmartLab: Automated Multipurpose X-ray Diffractometer 95

 Column
Incident monochromator crystal
The incident monochromator crystal system uses diffraction by Ge or Si crystals for x-ray monochromatization.
Ge(220)x2 crystals and Ge(440)x4 crystals are available as options for SmartLab. Select the appropriate crystal
based on the resolution required for measurements and the sample (d value). As an example, the Ge(220)x2 crystal
monochromatizes x-rays by diffracting them twice by Ge(220) lattice planes. Passing x-rays through this crystal
makes it possible to use only Kα1 x-rays with about 0.003 degree divergence. Shown below are the types and
resolutions of monochromator crystals and corresponding applications.

Table Types and resolutions of incident monochromator crystals

Type of Resolution
Applications
crystal (FWHM)
For applications requiring monochromatized Kα1
Ge(220)x2
0.008º< x-rays or for measurements of materials with
crystal
diffraction planes with d spacings of ca. 2 Å.
0.0022º For measurements of materials with diffraction
Ge(400)x2 planes with d spacings of ca. 1.4 Å.
crystal (when sample d
spacing is 1.41A)
Ge(220)x4 For applications requiring high resolution over a
0.0033º<
crystals broad 2-theta range.
Ge(440)x4 For applications requiring very high resolution over
0.0015º<
crystals a broad 2-theta range.

Slit collimation
スリットコリメーション Zoom
Ge(220)22結晶
Ge(220) crystal view
拡大
[任意単位] unit]

Ge(220)44結晶
Ge(220) crystal
強度[unspecified

Cu Kβ

W-Lα 69.00 69.10 69.20

Intensity

61.00 63.00 65.00 67.00 69.00

2θ/ω [deg]

2-theta/omega scan profile of Si(001) single crystal wafer measured with

different incident optics systems
Examples of Sample Mounting
Introduced below are some typical sample mounting methods.
For more information, refer to the SmartLab Guidance Reference Manuals, the
Package Measurements Help Topics of the online help section of the SmartLab
Guidance software.

Powder samples
Place powder samples in the indentation on the glass sample holder or aluminum
sample holder, then insert into the height reference sample plate.

Powder sample

Bulk samples
Use a 4-inchi wafer sample plate, 6-inch wafer sample plate, or 8-inch wafer
sample plate to measure bulk samples. Select the appropriate sample spacer and
sample plate based on sample thickness. For detailed information, refer to Wafer
sample plates and sample spacers.
Place the sample so that the sample surface to be measured is parallel to the
sample plate. A piece of clay may be used to secure the sample in place. If the
bulk sample is small enough to pass through the window on the provided
aluminum sample holder, you can secure the sample in the aluminum sample
holder and use the height reference sample plate.

Bulk sample on height reference sample plate

Sample for transmission SAXS measurements

For transmission SAXS measurements, clamp a fibrous or film sample to a
sample holder and secure it in place, then insert the holder into a sample plate.

SmartLab: Automated Multipurpose X-ray Diffractometer 97

Examples of Sample Mounting

Wafer-shaped samples
Use a 4-inch wafer sample plate, 6-inch wafer sample plate, or 8-inch wafer
sample plate to measure wafer-shaped samples.

Wafer-shaped sample

When placing or removing the sample, we recommend removing the sample plate and
sample spacer from the attachment. When removing the sample plate and sample spacer, we
recommend setting the chi axis to 0° and positioning the sample horizontally.

Place the sample at the center of the sample plate. Use the magnets provided to
hold the sample in place. The magnets can be used with samples that are up to 3
mm thick. For information on measuring samples thicker than 3 mm, see Bulk
samples.

CAUTION
Placing a sample larger than the sample plate may result in damage to the
sample during measurement.

Place an 8-inch wafer on the center of the 8-inch wafer sample plate; because the
space available for the magnets securing the sample in place is small. Be careful
while measuring of 8-inch wafers, because increasing the tilt axis (chi axis) can
cause the wafer to bend under its own weight.

98 SmartLab: Automated Multi Purpose X-Ray Diffractometer

 Measurements
This section introduces basic operating procedures for typical measurements. For
detailed information, refer to the SmartLab Guidance Reference Manuals, the Parts,
and Package Measurements Help Topics of the online help section of the SmartLab
Guidance software.

Preparing for measurements

1 Make sure that the OPERATE lamp on the main panel is lighting up in
green.

2 Launch SmartLab Guidance. Click Package Measurement under the

Task menu.

3 Click the Startup button to turn on the x-ray.

For information on the startup procedure, refer to Section 2.1 of the CBO Maintenance
Package Measurement Help Topic of the online help section of the Smartlab Guidance
software.

Setting the hardware configuration

1 Click Hardware Configuration in the Options menu to open the
Hardware Configuration dialog box.

SmartLab: Automated Multipurpose X-ray Diffractometer 99

Measurements

2 Click Goniometer to open the Goniometer dialog box.

Distance table

Limit table

3 Set the position of each optical device. To change the optical devices of
the receiving optics, inspect the installation positions of the standard
receiving slit box # 1, standard receiving slit box # 2, and detector
adaptor and enter the correct corresponding values.

Selecting a Package Measurement

1 Click Package Measurement under the Task menu.

2 Registered Package measurements are displayed in tree view. Select the

Package Measurement that matches the purpose of the measurement.

For information on the procedures of each Package Measurements, refer to the Package
Measurement Help Topic of the online help section of the SmartLab Guidance software.

100 SmartLab: Automated Multi Purpose X-Ray Diffractometer

Periodic Maintenance
Perform the following maintenance tasks at regular intervals to maintain the
performance of SmartLab.

Optics maintenance

You must perform re-adjustments following

Multilayer mirror
maintenance of the x-ray generator.
You must perform re-adjustments when changing the
Attenuator correction wavelength or following maintenance of the x-ray
generator.
You must perform re-adjustments when changing the
HV/PHA adjustment
wavelength to be measured.
You must perform dead-time correction
Dead-time correction
measurements after HV/PHA adjustments.

The characteristics of the detector will change over time. Replacement of the
detector is required when it reaches the end of its service life. However, you can
minimize performance degradation by making the appropriate adjustments.
We recommend performing HV/PHA adjustments and dead-time correction
measurement at periodic intervals.

・ HV/PHA adjustments
・ Dead-time correction measurement
To make these adjustments automatically, select Package Measurement from
the Task menu, then select Maintenance Package measurement under Utility.
For detailed information on measurement procedures, refer to the “CBO
Maintenance Package measurement” Help Topic of the online help section of the
SmartLab Guidance software.

Selecting Maintenance Package measurement

SmartLab: Automated Multipurpose X-ray Diffractometer 101

Periodic Maintenance

Cooling water
Check the amount of cooling water when using the water circulation pump. If
the water level is low, add water. Periodic replacement of cooling water is also
recommended.

Cooling water filter

This filter removes impurities from the cooling water. If the filter becomes
clogged with impurities, the water pressure may not rise appropriately. We
recommend changing the filter at periodic intervals.
Described below are the parts whose maintenance are required if using the
rotating anode type x-ray tube.

Target (2080A211/A411)
The target metal rotates at high speed to boost x-ray output. Pay close attention
and note any abnormal noise or vibrations, and if these occur please contact the
sales representative who you purchased the instrument from.
When contaminant (tungsten from the filament) from the electron gun (filament)
adheres to the target metal surface, you may observe characteristic x-rays from
the contamination, in addition to characteristic x-rays from the target metal. If
this happens, maintenance is required. Please contact the sales representative
who you purchased the instrument from.

Filament (2080A211/A411)
As electrons are discharged, the filament will become thinner, eventually
breaking the required circuit. Upon breaking, the filament will release a sudden
burst of electrons that can damage the target surface. To avoid this, we
recommend periodically changing the filament.

Ion gauge (vacuum gauge) (2080A211/A411)

Since the filament in the ion gauge may come loose after many hours of use, we
recommend changing the filament in the ion gauge at periodic intervals.

Rotary pump (2080A211/A411)

Check the oil level in the vacuum pump. If the oil level is low, add oil. We also
recommend periodic oil changes.

102 SmartLab: Automated Multi Purpose X-Ray Diffractometer

 Troubleshooting
Problem Remedy
1 The OPERATE lamp does not change The controller may be in the process of starting up.
color to green (remains red). Wait several minutes.
If the lamp fails to turn green after several minutes, the
controller may be malfunctioning. Press the OFF
button on the main panel to shut down SmartLab, then
press the ON button to restart SmartLab.
2 An error occurs during SmartLab There may be a problem in the connection between the
Guidance startup. SmartLab and the controller. Confirm that the
SmartLab startup procedure fails to OPERATE lamp on the main panel is lighting up in
complete properly. green. Confirm the connection status of the RS232C
connectors is OK.
After checking these items, shut down SmartLab
Guidance, then restart it. Restart SmartLab Guidance
after the SmartLab is restarted.
3 SmartLab stops abruptly during Make sure the OPERATE lamp on the main panel has
measurement or other operation. turned to red. SmartLab may have stopped due to
excessive force applied to the theta_s or theta_d arm.
Press the OFF button on the main panel to stop
SmartLab. Check the arms to see if any item obstructs
their operation, then restart SmartLab.
4 The x-ray generator stops during Click XG Control in the Control menu to open the
measurement or other operations. XG Control dialog box. Click Display in the Alarm
section to open the Alarm dialog box. Check for x-ray
generator alarms.
Refer to the XG status description box in the Alarm
dialog box that will indicate the details of the alarm,
which is brought when the pink alarm box in the
Alarm dialog box is clicked.

* If a problem other than those described above occurs or if the problem cannot be corrected by taking the countermeasure described,
please contact the sales representative who you purchased the instrument from.

SmartLab: Automated Multipurpose X-ray Diffractometer 103

Troubleshooting

Appendix Using the OPERATE Lamp

The OPERATE lamp indicates the status of the SmartLab controller. The lamp is usually green, but will
change to red and begin flashing at set intervals in the event of an abnormality. To reset the generated
alarm, you must restart SmartLab. After shutting down SmartLab Guidance, press the “O” OFF button,
then press the “|” ON button to restart SmartLab.
After SmartLab restarts, the OPERATE lamp will be flashing in green for 10 to 20 seconds. After that,
when the lamp lights up in green, SmartLab is ready to use. If the OPERATE lamp does not turn green,
flashing red instead after startup, or if the lamp turns green but changes to a flashing red immediately
during use, please contact the sales representative who you purchased the instrument from. Before
contacting, please refer to following tables to identify the alarm being generated.

Table Flashing pattern of the OPERATE lamp when SmartLab is starting up

Continuously
Condition Color Pattern
On / flashing

Immediately 250 ms
Green Flashing
after Power ON
250 ms

100 ms
10 seconds after
Green Flashing
Power ON
100 ms

Able to be
controlled from Continuously
Green
SmartLab On
Guidance

104 SmartLab: Automated Multi Purpose X-Ray Diffractometer

 90BRotary pump (2080A211/A411)

Table Patterns of the OPERATE lamp flashing and alarm sounds when an alarm generated

Continuously
Alarm point Color Pattern
On / flashing

400 ms 50 ms

XG alarm Green Flashing 2500 ms

50 ms
One long beep and two short beeps (repeats)
50 ms
Attachment
connecting Green Flashing 1000 ms
cover is open 50 ms
Two short beeps (repeats)
200 ms
Communication
Red Flashing
error 1000 ms

One beeps (repeats)

200 ms 200 ms

Encoder error Red Flashing 1000 ms

200 ms

Two beeps (repeats)

200 ms 200 ms

Servo alarm Red Flashing 1000 ms

200 ms 200 ms
Three beeps (repeats)

Table Causes of alarm

Cause Description
An error has occurred in the x-ray generator (XG). See # 4 in
XG alarm
Troubleshooting.
The cover of the attachment connection cable is open in the radiation
enclosure. Close the cover.

Attachment
connecting cover is
open

A communication error has occurred in the control board for the optical
Communication
devices in the incident and receiving optics. The cables for the incident and
error
receiving optics may be disconnected or broken.
An error has occurred in the encoder used to control the goniometer. The
Encoder error
encoder may not be adjusted correctly, or the detecting part may be stained.
The protection circuit is working as a result of motor electrical overload. See
Servo alarm
# 3 in Troubleshooting.

SmartLab: Automated Multipurpose X-ray Diffractometer 105

 Column
Kβ filter
The characteristic x-rays used for x-ray diffractometry generally contain Kα and Kβ x-rays. A substance that passes
Kα x-rays while absorbing most Kβ x-rays to monochromatize the beam is called a Kβ filter.
The mass absorption coefficient (hereinafter referred to as “absorption coefficient”) of an element becomes smaller
as wavelengths become shorter, and vice versa. However, when x-rays with energy greater than the binding energy
between the nucleus and electrons of an element, strike the element, the absorption coefficient suddenly increases
due to the photoelectric effect. This discontinuous point in the absorption coefficient is called an absorption edge.
LI absorption
edge
Mass absorption coefficient

LII absorption edge

LIII absorptin
edge

K absorption
edge

Wavelength (Å)

Change in mass absorption coefficient in accordance with wavelength (platinum)

For efficient absorption of Kβ x-rays only, select an element as a Kβ filter with its absorption edge wavelength
located between the Kα x-ray and Kβ x-ray wavelengths. Those elements will have an atomic number one or two
less than that of the target element. The following table shows the target elements commonly used for x-ray
diffractometry and their corresponding filters.

Table Kβ filters

Wavelength (Å) Metals used as a filter

Wavelength When I Kβ I Kα = 1 / 100

1 1

Target Substa of
Mass
Kα1 Kβ1 absorption
-nces Thickness per unit Kα1
edge
(mm) area transmissivity
(Å)
(g/cm2)
Cr 2.290 2.085 V 2.269 0.011 0.007 63
Fe 1.936 1.757 Mn 1.896 0.011 0.008 62
Co 1.789 1.621 Fe 1.743 0.012 0.009 61
Cu 1.541 1.392 Ni 1.488 0.015 0.013 55
Mo 0.7093 0.6323 Zr 0.689 0.081 0.053 43
Ag 0.5594 0.4970 Rh 0.534 0.062 0.077 41
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