Rigaku SmartLab User manual

Automated Multipurpose

X-ray Diffractomete

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.

Microsoft, Windows, Windows XP, Windows Vista, Windows 7, Microsoft Internet Explorer, Microsoft Excel, and

Microsoft Word Operating System are either registered trademarks or trademarks of Microsoft

Corporation in the United States and/or other countries. The ™ and ® marks have been omitted.

Adobe, the Adobe logo, and Reader are either registered trademarks or trademarks of Adobe Systems

Incorporated in the United States and/or other countries. The ™ and ® marks have been omitted.

The names of actual companies and products mentioned herein may be the registered trademarks or

trademarks of their respective owners.

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.

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

Soller slit

Soller slit Soller slit

Soller slit

CBO-ｆSoller slit

Parallel beam

PSC

2-bounce

monochromator

PSC

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

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

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