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.
The contents of this manual are subject to change without prior notice.
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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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via hardcopy or electronically. If copies must be made, you must obtain our written approval
before doing so for each specific case.
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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.
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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
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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