Rigaku SmartLab User manual

Automated Multipurpose
X-ray Diffractomete
r
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.
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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.
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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
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Microsoft and Windows are trademarks or registered trademarks of Microsoft Corporation in the United
States and/or other countries.
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Other company names and product names are trademarks or registered trademarks of their respective
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Note that this manual omits the TM (™) and R (®) symbols.

SmartLab: Automated Multipurpose X-ray Diffractometer i
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

ii SmartLab: Automated Multipurpose X-ray Diffractometer
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
βsample stage (option: 2430B101)........................................................................80
ASC-6 (option: 2430H101) .....................................................................................81
For vertical transmission geometry (option: 2455H105)..................................82
AntonPaar sample stage ........................................................................................84

SmartLab: Automated Multipurpose X-ray Diffractometer iii
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 1
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.
SmartLab
system
Para-focusing
method
Parallel beam
SAXS
Micro area
4-bounce
monochromator
2-bounce
analyzer
2-bounce
analyzer
Ni filter
Diffracted beam
monochromator
PSA
PSA
Soller slit
Soller slit
Soller slit
Soller slit Soller slit
Soller slit
Soller slit
Soller slit
Soller slit
Soller slit
Soller slit
Soller slit
CBO-ｆSoller slit
Parallel beam
PSC
2-bounce
monochromator
+
PSC
PSA
PSA
2-bounce
monochromator
+
Soller slit
Phase ID
analysis/
Quantitative
analysis
Profile analysis
Preferred orientation
analysis
Rietveld analysis
Structure analysis
Film thickness analysis
Rocking curve
Reciprocal space mapping
Particle-/Pore-size
distribution analysis
Micro area
Preferred orientation
measurement
In-plane
measurement
CBO unit Incident optics Receiving optics
Soller slit
+
CALSA
D/teX Ultra
*In-plane arm (option) is required.
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

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
0
2000
4000
0 0.5 1 1.5 2
波長（Å）
強度
特性X線
連続X線
αβ
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. Kαx-rays contain Kα1x-rays
and Kα2x-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 Kα1x-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)
Element Atomic
number
Kα2Kα1Kβ
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
Intensity
Wavelength (Å)
Continuous
x-rays
Characteristic
x-rays

SmartLab: Automated Multipurpose X-ray Diffractometer 3
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

Product Features
4SmartLab: Automated Multipurpose X-ray Diffractometer
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.

Incident optics system
SmartLab: Automated Multipurpose X-ray Diffractometer 5
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 Kβx-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.

Product Features
6SmartLab: Automated Multipurpose X-ray Diffractometer
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.

Two-slit SAXS optics
SmartLab: Automated Multipurpose X-ray Diffractometer 7
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.

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 Kβfilter 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.
Optimum voltage
(equivalent load) (kV)
Target
Minimum
excitation
voltage
(kV) Intensity at
maximum
P/B ratio at
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

SmartLab: Automated Multipurpose X-ray Diffractometer 9
Names of Parts
General view of SmartLab
(Left: 2080A211/2080B211/2080A411/2080B411, Right: 2080B212)
1. Rotary pump Pump for maintaining the vacuum in the x-ray generator.
(2080A211/2080A411）
2. Control PC PC used to control SmartLab.
Main unit
Front view of SmartLab
(Left: 2080A211/2080B211/2080A411/2080B411, Right: 2080B212)
3.
1.
5.
4. 4.
3.
5.
2. 1. 2.
1.
2.

Names of Parts
10 SmartLab: Automated Multipurpose X-ray Diffractometer
1. Main panel Panel used to start and stop SmartLab.
2. Operating panel Panel used to turn the internal light on/off.
3. Door This door is opened to change samples and
optical devices.
4. X-ray warning lamp Lights when x-rays are generated.
5. Door-lock button Lock/Unlock the door.
Rear view of SmartLab
6. Power input connector External power supply connects here.
7. Connector for control PC The LAN cables used to control SmartLab
connect here.
8. Connectors for rotary pump
The power supply for the rotary pump
connects here.
(2080A211/2080A411)
9. Connectors for water
circulation pump
The water circulation pump (short-cut valve)
control connects here.
10. Pipes for cooling water The cooling water pipe of the x-ray generator
connects here.
11. Pipes for rotary pump The rotary pump pipe connect here.
(2080A211/2080A411)
12. Circuit breaker Circuit breaker for the power supply to the
main unit.
8. 9.
10.
6.
12.
7.
11.

Goniometer
SmartLab: Automated Multipurpose X-ray Diffractometer 11
Goniometer
Goniometer
1. Theta_s arm Arm for controlling x-ray beam incident angle.
2. X-ray tube X-ray generating device.
3. Incident optics Optical device for achieving desired incident
x-ray conditions.
4. Theta_d arm Arm for controlling the x-ray detector angle.
5. Receiving optics Optical device for achieving desired x-ray
receiving conditions.
6. Detector X-ray detector.
7. Sample stage Adjusts the position and orientation of the
sample to be measured.
8. In-plane arm Theta_d arm used for in-plane measurements.
(2080B212)
1.
2.
3.
4.
5.
6.
7.
8

Names of Parts
12 SmartLab: Automated Multipurpose X-ray Diffractometer
Theta_s arm
→CBO unit (for Cu target)
→Incident slit box
→Incident optics unit (standard incident optics unit)
Theta_d arm
→Receiving slit box # 1
→Receiving optics unit # 1
→Receiving optics unit # 2
→Detector
Sample attachment
→Sample Plates
→Attachments
→Sample Stage
•Kβfilter
PSA 0.114 deg, Ge(220)x2 etc.
• Receiving optical device adaptor/analyzer
• PSA
Soller slit 5.0 deg, In-plane PSA 0.5 deg etc.
• Receiving parallel slit adaptor
• Soller slit/in-plane PSA
• Scintillation counter, D/teX ultra
/diffracted beam monochromator for Cu
Height reference sample plate,
4-inch sample plate, etc.
• Sample plate
Standard
,
XY-4”
φ
,
etc.
• Attachment
Standard sample stage, βsample stage, etc.
• Sample stage
• Selection slit
PB, BB, SA, etc.
• Incident length-limiting slit
10
,
15
(
mm
),
etc.
Soller slit 5.0 deg、Ge(220)x2 CBO-f etc.
• Incident parallel slit
ada
p
tor/monochromato
r