Me 11550

Cat. No. 2080A102/B101/M101/M102

SmartLab

Horizontal Sample Mount X-Ray Diffractometer

for Thin Film Analysis

Instruction Manual

Manual No. ME11550A02

Rigaku Corporation

Thank you for your purchase of Rigakus product. 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.

NOTICE

1. 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.

2. As a rule, one set of the instruction manual has to be purchased for each product. 3. If there are any missing or incorrectly collated pages in the delivered instruction manual, contact the nearest Rigaku branch office or sales office for instruction manual replacement. 4. In no event will Rigaku be responsible for the results of the use of this manual. 5. The contents of this manual are subject to change without prior notice.

Safety Precaution - 1

Safety Precautions in Handling X-ray Equipment 1. Introduction Thank you for purchasing Rigakus product. This instruction manual contains the basic safety precautions to observe when using the equipment. Be sure to read the precautions set forth in this manual before using the equipment and carefully observe them when you use the equipment. It is also essential that this manual be stored at such a place that the equipment operator can readily refer to it. For the detailed operating and handling procedures for each equipment unit, you should also read its instruction manual.

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2. Overall System Safety Precautions (1) All system components are designed so that the personnel will not be exposed to X-rays. If the

equipment is modified, however, the personnel may be exposed to X-rays. Equipment modifications must never be made without the written consent of Rigaku.

(2) If any warning label is separated from its specified location, immediately restore it to normal to maintain

a safe operating environment. (3) When generating X-rays, opening or closing the X-ray shutter, or operating the goniometer, verify that

there is no person around the equipment. If you do not complete such a verification step, any person around the equipment may be seriously endangered and items positioned near equipment with movable parts may be damaged.

In cases where you operate the equipment with a remote computer, provide means of confirming the conditions prevailing around the equipment as needed so that persons near the equipment will not be exposed to X-rays. Particularly before you open or close the X-ray shutter (for measurement or automatic setup program execution purposes), you have to make sure yourself that no other person is within the equipment and verify safety before initiating an operation.

Do not control the measurement process using a device other than the computer supplied as a part of the system, because safety hazards may be created by such a remote-controlled operation.

(4) When performing any operation with an assistant, observe the same precautions as stated above. (5) If the equipment is found abnormal, immediately stop it. Eliminate the causes of abnormalities and take

appropriate measures to prevent the recurrence of abnormalities. 2.1 Parts Removal Precautions

All component parts function not only to maintain the product performance characteristics but also to normally operate safety devices.

Parts removal, parts function alteration, or parts modification must never be attempted without the written consent of Rigaku. If parts removal, parts function alteration, or parts modification is performed, the safety devices may fail to function, thereby creating a safety hazard.

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3. Precautions to Be Observed to Avoid X-ray Exposure X-rays are harmful to the human body. Therefore, when handling X-ray apparatus, exercise due care to avoid being exposed to X-rays. To avoid radiation exposure, be sure to observe the following precautions. While the X-ray shutter is open, the X-ray direct beam is irradiated toward the sample position and the X-ray shutter main body open/close indicator lamp (red) comes on. While the indicator lamp is illuminated, never position your hands or any other parts of your body within or near the X-ray path. If your hands or other parts of your body are inadvertently placed within or near the X-ray path for sample replacement, attachment adjustment, or other purposes, they are exposed to X-rays and seriously endangered. If the X-ray shutter fails to open or close, the indicator lamp fails to go off, or any other abnormality is encountered in the X-ray shutter open/close sequence, immediately stop using the equipment and contact your Rigaku technical representative. 3.1 Notes on Radiation Enclosure and X-ray Shutter Safety Release Operation (1) Rigakus radiation enclosure is designed to eliminate the possibility of X-ray exposure outside the

radiation enclosure during normal use of the X-ray apparatus. When you use the radiation enclosure in conjunction with the safety mechanism during the operation of Rigakus standard X-ray diffractometer, you can use X-rays only when the radiation enclosure door is closed. Even if you carelessly open the door, the safety mechanism actuates to automatically stop X-ray generation.

(2) In the safety release state (in which the DOOR OPEN switch is depressed to blink the DOOR-OPEN or

OPEN SAFETY lamp), however, the safety mechanism is disabled so that X-ray generation does not stop when you open the door.

(3) The X-ray shutter safety mechanism works so that the X-ray shutter does not open while the radiation

enclosure door is open no matter whether the automatic or manual mode is chosen. However, if the X-ray shutter safety mechanism is placed in the release state when the radiation enclosure is in the safety release state, the shutter can be opened and closed while the radiation enclosure door is open so that any parts of your body inadvertently positioned in the X-ray path inside the radiation enclosure could be exposed to X-rays. Therefore, when the equipment is used with the radiation enclosure and X-ray shutter placed in the safety release state, the equipment must always be handled and operated under the direct guidance and control of certified X-ray apparatus handling personnel.

(4) The key for disabling the safety mechanism should always be handled under the control of a certified

X-ray apparatus supervisor. It should normally be removed from the safety release unit and placed under the control of a certified X-ray apparatus supervisor.

(5) If the safety mechanism is disabled, the controlled area enlarges beyond the outer surface of the X-ray

diffractometer enclosure. Therefore, when disabling the safety mechanism with the key, define the controlled area anew (by enclosing the area with a wall or the like, drawing a white line or striped line mark on the floor, encircling the area with a rope, setting up flags and joining them to mark the area, or marking the area in some other conspicuous manner) and provide an adequate safeguard (e.g., protective aprons, protective gloves, and shielding screens) to minimize the exposure of X-ray handling personnel to radiation.

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(6) If Rigakus radiation enclosure and safety mechanism are not purchased, the automatic X-ray shutoff

feature will not be exercised in accordance with radiation enclosure door opening/closing. If the X-ray shutter mounted coupling protector or an optical system part such as the slit box and direct beam stopper is removed from the standard assembly or modified, the personnel outside the equipment may also be exposed to X-rays. Never remove or modify such parts.

NOTICE :For the details of the radiation enclosure and X-ray shutter safety mechanism, refer to after mentioned text of this manual.

NOTICE :The safety mechanism reduces the possibility of radiation exposure. However, it does not

guarantee that you are absolutely safe from radiation exposure. 3.2 Notes on X-ray Shutter Safety Release Operation The X-ray shutter cannot be opened while the radiation enclosure door is open. However, when you insert the dedicated key into the shutter safety release switch and place the safety function in the release state, the X-ray shutter can be opened and closed even while the radiation enclosure is open. In such an instance, however, X-rays are emitted from the X-ray shutter section so that you may be exposed to X-rays. To avoid being exposed to X-rays, be sure to observe the following precautions.

(1) Operations must always be conducted under the direct guidance and control of a certified X-ray apparatus supervisor.

(2) The safety release key must be stored by a supervisor in order to

exercise thorough shutter open/close control.

(3) Be sure to close the X-ray shutter before starting an operation for the purpose of preventing your hands and other parts of your body from being positioned in the X-ray path or exposed to X-rays scattered around the X-ray path for prolonged periods of time during sample replacement, optical system adjustment, or other operation. If it is necessary to position your hands or face near the X-ray path while X-rays are generated with the X-ray shutter open, minimize the amount of exposure to X-rays as suggested below.

(a) Wear a film badge and other legally stipulated measurement

clothing to measure and record the radiation dose received.

(b) Wear a radiation-proof apron, safety goggles, and other necessary radiation-resistant clothing.

(c) Never place any part of your body in the X-ray path.

(d) Set the X-ray tube voltage and tube current at the minimum

levels required.

(e) Keep the maximum distance from the X-ray path during operations.

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3.3 Notes on X-ray Shutter Use

(1) If the X-ray shutter is removed, you will be exposed to

radiation hazard.

(2) The customer will never be allowed to remove or disassemble the X-ray shutter.

3.4 Notes on Radiation Enclosure Use

Rigakus radiation enclosure is designed to eliminate the possibility of X-ray exposure outside the radiation enclosure while it is normally installed. Therefore, do not remove or modify the door, side panel, direct beam stopper, or other component parts. If any such parts are removed inadvertently or otherwise, you may be exposed to X-rays.

DO NOT REMOVE SHUTTER RADIATION HAZARD

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4. Notes on Hazardous Substances

Metal beryllium is used as a material for the X-ray emission window, X-ray path of some sample atmosphere changer attachments, and X-ray counter window. If beryllium or its corrosion or compound comes into contact with or enters the human body, it troubles the human body. To avoid such troubles, observe the following precautions.

(1) Be sure that no part of your body comes into contact with metal

beryllium. (If you touch it with your bare hands or if skin is contacted, immediately flush with soap and water.)

(2) The metal beryllium must not be subjected to the following.

Wetting with water. (If the metal beryllium is wet with water,

absorb the water with paper or other material having a high water absorption power.)

Polishing. Scraping. Cutting. Breaking. Wiping with chemicals. Burning. Pulverizing or

vaporizing.

(3) If the metal beryllium is inadvertently broken, proceed as follows.

Do not touch with bare hands. Use care not to breathe in beryllium powder. Collect all broken chips of beryllium. Place them in a container

and hermetically seal it to prevent them from scattering. Have an expert agent dispose of the damaged beryllium parts.

If no appropriate expert agent is available, consult your nearest Rigaku office.

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5. Notes on High Voltage

While X-rays are being generated, a high voltage is supplied to the X-ray tube via the high-voltage cable. If the high-voltage cable is inadvertently disconnected from the equipment, you may receive a high-voltage electric shock. To avoid electrical shock hazard, be sure to observe the following precautions when connecting or disconnecting the high-voltage cable, cleaning the high-voltage cable head, changing the insulating grease, replacing the X-ray tube, or servicing the X-ray generator internal parts.

(1) Turn OFF both the X-ray generator power supply and

wall-mounted switch to make doubly sure that the power supply to the equipment is shut off.

(2) Since the high-voltage cable and transformer are electrically

charged with a high voltage, be sure to wait at least 30 minutes after power shutoff when initiating any servicing task.

(3) All servicing tasks must be carried out by the maintenance

personnel who has an adequate knowledge of electricity.

(4) When directly touching the high-voltage cable head for cleaning or other servicing purposes, short the head to the ground. Proceed to perform servicing tasks after the high-voltage electrical charge is completely removed.

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6. Notes on High and Low Temperatures

6.1 Attachment Handling Precautions

When you use an attachment that changes the sample atmosphere to a high temperature or low temperature, you may suffer a burn (including a low-temperature burn). To avoid suffering a burn, observe the following handling precautions.

(1) After the temperature is raised or lowered, do not perform the

sample replacement or other procedure until the furnace internal temperature is restored to the room temperature level.

(2) When using an attachment for spraying a high-temperature gas or

liquid or low-temperature gas or liquid on the sample, ensure that the gas or liquid does not come into direct contact with you body or clothing.

HOT KEEP AWAY FROM FURNACE

6.2 Replacement Precautions

If you attempt to replace the X-ray generator sealed-off X-ray tube or demountable (Rotor Flex) X-ray tube filament, cathode, or target immediately after the end of X-ray generation, you may suffer burns because the X-ray tube, filament, cathode, and target are heated to a high temperature. When replacing such X-ray generator parts, be sure to observe the following precautions.

(1) When replacing the sealed-off X-ray tube after X-ray use, wait at

least 30 minutes after X-ray system power OFF. Replace the X-ray tube after it is cooled down.

(2) When replacing the demountable (Rotor Flex) X-ray generator

X-ray tube parts after X-ray use, wait at least 1 hour after X-ray system power OFF, allowing the parts to cool down, and then provide a vacuum relief. After the temperature of the filament and cathode is restored to the room temperature level, initiate parts replacement.

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7. Precautions to Be Observed during the Use of a Vacuum or High-pressure Atmosphere

If an attachment designed for samples in a vacuum or high-pressure atmosphere is improperly used, container breakage or other accident may occur due to a pressure differential. It is essential that you thoroughly read the instruction manuals for the employed equipment, observe the operating precautions, and assure safety in compliance with all applicable laws. 8. Precautions to Be Observed during the Use of a Hazardous Gas Atmosphere When replacing the sample atmosphere with an explosive or flammable substance, corrosive substance, or other substance harmful to the human body, pay special attention to gastightness, exhaust, and chemical reactions and ensure safety in compliance with all applicable laws. 9. Equipment Transfer/Relocation While the equipment is transferred or relocated, it may be adversely affected by vibration or other impact. When transferring or relocating the equipment, consult your nearest Rigaku office.

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X-ray Apparatus Handling Precautions X-rays are harmful to the human body. Therefore, when handling X-ray apparatus, exercise due care to avoid being exposed to X-rays. Rigakus X-ray apparatus are carefully designed to eliminate the possibility of exposure to X-rays during normal use. However, if you handle the apparatus in a manner other than stated in their manuals, you may become exposed to X-rays. Further, when servicing the internal parts of the apparatus, you may run the risk of accidentally coming into contact with a high voltage. To avoid such accidents, be sure to observe the following precautions. (1) While X-ray generation operations or operations in a safety release state are performed, the X-ray

apparatus must always be handled under the control of a certified X-ray apparatus supervisor. Further, the SAFETY RELEASE key must be kept by the supervisor, and radiation enclosure door opening/closing must be placed under strict control.

(2) No component part must be removed or modified to change their functions without explicit written

instructions from the manufacturer. (3) Before accessing the X-ray path for sample replacement or other purposes, be sure to verify that no

X-rays are radiated and that the shutter is closed. You must observe this precaution to avoid placing your hands or other parts of your body in the X-ray path or exposing them to X-rays scattered around the X-ray path for prolonged periods of time. While the solenoid shutter lamp is illuminated, X-rays are emitted. While the lamp is lit, never position your hands or other parts of your body in the X-ray path because they will be exposed to radiation hazard.

When making optical system adjustments near the X-ray path, minimize the radiation dose as suggested below.

(i) The X-ray intensity setting should as low as possible. (ii) The operating position should be as far from the X-ray path as possible. (iii) The period of time during which you are near the X-ray path should be minimized (preferably not

longer than 5 seconds). (4) Rigakus radiation enclosure is designed to eliminate the possibility of X-ray exposure during normal use

of the X-ray apparatus. When you use the radiation enclosure in conjunction with the SAFETY RELEASE function during the use of Rigakus standard X-ray diffractometer, you can use X-rays only when the radiation enclosure door is closed. In the safety release state (in which the DOOR OPEN switch is depressed to blink the DOOR-OPEN lamp), however, the above automatic safety assurance function is disabled so that you can use X-rays with the door open.

(5) The high-voltage section of X-ray apparatus must be serviced by a person who has an adequate

knowledge of electricity, with the electrical power supply shut off and the high-voltage electric charge thoroughly removed.

NOTICE 1 :Rigaku cannot be responsible for accidents resulting from customers carelessness.

NOTICE 2 :The SAFETY RELEASE function is used to disable (turn OFF) the safety

feature temporality.

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Radiation Protection Mechanisms and Functions Component Mechanism Function

X-ray generator section Solenoid shutter Radiation enclosure SAFETY RELEASE unit

(1) The X-ray tube outer wall is made of heavy metal. (2) The solenoid shutter shield section consists of a

main shutter element (heavy metal, over3.5 mm) and an auxiliary shutter element (heavy metal, over3.5 mm). (Except the rotary shutter)

(3) When the solenoid shutter is open, it is indicated by the X-ray shutter red lamp.

(4) When the shutter open indicator lamp system is faulty due to lamp burnout, the solenoid shutter does not remain open (opens for a moment and then closes).

(5) The main shutter element is placed under the remote control of a computer.

(6) When the mechanical connection to the goniometer

or other external X-ray utilization section is lost, the auxiliary shutter element is closed by its internal spring. In this instance, the main shutter element also closes. (Except the rotary shutter)

(7) X-ray generation is indicated by the red warning lamp on the radiation enclosure.

(8) X-ray generation is unachievable when the X-ray generation indicator lamp is burned out.

(9) The goniometer and other mechanical operation sections are entirely covered by the radiation enclosure (box with a 3.2 mm thick iron lid).

(10) The radiation enclosure side wall positioned in the direct X-ray radiation direction is provided with a 2.5 mm thick, large lead plate.

(11) The X-ray shutter does not open if the radiation enclosure door is open.

(12) X-ray generation is unachievable when the warning lamp described in paragraph (7) above is burned out.

(13) Key input is needed to disable the safety feature. When the safety feature is disabled, the SAFETY RELEASE unit red LED blinks and the alarm buzzer intermittently beeps, indicating that you can manually open and close the X-ray shutter.

(14) When you press the DOOR OPEN button, its signal is processed by the computer, and the yellow lamp blinks at the operation panel to indicate that the door can be opened.

Complete shielding Same as above Warning Fail-safe operation Safety assurance and radiation exposure possibility minimizationSame as above Warning Fail-safe operation Shielding from scattered X-rays Shielding from possible direct X-rays Fail-safe operation Fail-safe operation Indication of the possibility of radiation exposure Shielding from X-rays in the event of inadvertent door opening

NOTICE :The safe mechanisms remarkably reduce the possibility of radiation exposure. However,

they do not guarantee that you are completely safe from radiation exposure in all sorts of operations.

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Before Using the Product Read this manual cover to cover before attempting to use SmartLab. Carefully read the safety precautions for handling of the x-ray generator 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 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

SmartLab Horizontal Sample Mount X-Ray Diffractometer for Thin Film Analysis i

Contents

1. Overview.................................................................................................................................................... 1

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

2.1 Horizontal sample mount high-accuracy theta-theta goniometer ..................................................... 3 2.2 Attachment base (open Eurlerian cradle) and attachments ............................................................... 3 2.3 X-ray generator ................................................................................................................................. 3 2.4 Cross beam optics (CBO) ................................................................................................................. 3 2.5 Crystal alignment mechanism (monochromators and analyzers) ..................................................... 4 2.6 Receiving analyzer system................................................................................................................ 4 2.7 Incident optics system....................................................................................................................... 4 2.8 Receiving optics system.................................................................................................................... 5 2.9 Optics switching system ................................................................................................................... 5 2.10 Optical device detection..................................................................................................................... 5 2.11 Control software ............................................................................................................................. 6 2.12 Two-slit SAXS optics ..................................................................................................................... 6 2.13 In-plane optics for detailed analysis of thin film structure ............................................................. 6

3. Names of Parts of the Instrument ........................................................................................................... 7

3.1 Main unit........................................................................................................................................... 7 3.2 Goniometer ....................................................................................................................................... 9 3.3 X-ray tube ....................................................................................................................................... 11 3.4 Theta_s arm .................................................................................................................................... 12 3.5 Theta_d arm .................................................................................................................................... 13 3.6 Detector mounting bracket.............................................................................................................. 14 3.7 Attachment base and attachments................................................................................................... 14

4. Software Configuration.......................................................................................................................... 15

4.1 Control software ............................................................................................................................. 15 4.2 Data processing software ................................................................................................................ 15 4.3 Data display software...................................................................................................................... 15 4.4 Analysis software (options) ............................................................................................................ 15

5. Turning on and off the instrument ....................................................................................................... 17

5.1 Turning on the instrument............................................................................................................... 17 5.2 Starting SmartLab Guidance (control software) ............................................................................. 17 5.3 Starting the x-ray generator ............................................................................................................ 18 5.4 Stopping the x-ray generator........................................................................................................... 19 5.5 Turning off the instrument .............................................................................................................. 20

Contents

ii SmartLab Horizontal Sample Mount X-Ray Diffractometer for Thin Film Analysis

6. Opening and Closing the Door .............................................................................................................. 21

6.1 Opening the door ............................................................................................................................ 21 6.2 Closing the door.............................................................................................................................. 22 6.3 Emergency stop switch (EMO)....................................................................................................... 22

7. Optics ....................................................................................................................................................... 23

7.1 CBO unit (for Cu target) ................................................................................................................. 23 7.2 Incident optics unit (standard incident optics unit)......................................................................... 26

7.2.1 Incident parallel slit adaptor (IPS adaptor) .......................................................................... 26 7.2.2 2-Bounce monochromator (option)...................................................................................... 29 7.2.3 4-bounce monochromator (option) ...................................................................................... 32

7.3 Incident slit box .............................................................................................................................. 34 7.3.1 Standard incident slit box..................................................................................................... 34

7.4 Receiving slit box # 1 ..................................................................................................................... 37 7.4.1 Standard receiving slit box # 1............................................................................................. 37

7.5 Receiving optics unit # 1 ................................................................................................................ 40 7.5.1 Receiving optical device adaptor (ROD adaptor) ................................................................ 40 7.5.2 2-bounce analyzer (option) .................................................................................................. 43

7.6 Receiving optics unit # 2 ................................................................................................................ 45 7.6.1 Receiving parallel slit adaptor (RPS adaptor) ...................................................................... 45

7.7 Receiving slit box # 2 ..................................................................................................................... 48 7.7.1 Standard receiving slit box # 2............................................................................................. 48

7.8 Attenuator ....................................................................................................................................... 50 7.8.1 Standard attenuator .............................................................................................................. 50

8. Detector ................................................................................................................................................... 53

8.1 Counter adaptor............................................................................................................................... 53 8.2 Scintillation counter........................................................................................................................ 55 8.3 Diffracted beam monochromator unit for Cu (DBM unit) ............................................................. 57

9. Attachments ............................................................................................................................................ 61

10. Sample plates ........................................................................................................................................ 63

10.1 Wafer sample plates and sample spacers ...................................................................................... 63 10.1.1 Installing and removing sample spacers............................................................................. 66 10.1.2 Installing and removing wafer sample plates ..................................................................... 67

10.2 Height reference sample plate....................................................................................................... 68 10.3 Transmission SAXS sample plate (option)................................................................................... 68

Contents

SmartLab Horizontal Sample Mount X-Ray Diffractometer for Thin Film Analysis iii

11. Sample holders...................................................................................................................................... 69

11.1 Glass sample holder ...................................................................................................................... 69 11.2 Aluminum sample holder.............................................................................................................. 69 11.3 Transmission method sample holder (option)............................................................................... 69

12. Accessories............................................................................................................................................. 71

13. Examples of sample mounting............................................................................................................. 73

13.1 Wafer-shaped samples .................................................................................................................. 73 13.2 Bulk samples................................................................................................................................. 74 13.3 Powder samples ............................................................................................................................ 74 13.4 Sample for SAXS measurement (transmission measurement) ..................................................... 74

14. Measurements ....................................................................................................................................... 75

14.1 Launching the software................................................................................................................. 75 14.2 Setting the hardware configuration............................................................................................... 75 14.3 Selecting a measurement package ................................................................................................ 76

15. Periodic Maintenance........................................................................................................................... 77

15.1 Optics maintenance....................................................................................................................... 77 15.2 Cooling water................................................................................................................................ 78 15.3 Cooling water filter ....................................................................................................................... 78 15.4 Target ............................................................................................................................................ 78 15.5 Filament ........................................................................................................................................ 78 15.6 Ion gauge (vacuum gauge)............................................................................................................ 78 15.7 Rotary pump ................................................................................................................................. 78

16. Troubleshooting.................................................................................................................................... 79

Appendix Using the OPERATE lamp ...................................................................................................... 80

First Edition: December 14, 2005 Japanese Second Edition: September 28, 2006

SmartLab Horizontal Sample Mount X-Ray Diffractometer for Thin Film Analysis 1

1. Overview This instrument is a thin film analysis 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 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.

Fig. 1.1 SmartLab structure and measurement examples

SmartLab 9-kW 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

Soller slit Soller slit

In-plane optics Parallel beam

PSC


+ PSC

PSA

PSA


+ Soller slit

Phase ID analysis/

quantitative analysis

Powder profile analysis Preferred orientation

measurement Thin-film/thick-film

measurement

Film thickness measurementReciprocal space mapping

Rocking curve

Particle size/pore diameter distribution

Micro region

Preferred orientation measurementIn-plane measurement

CBO unit Incident optics system Receiving optics system

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

X

X

Figure X-Ray spectrum of Cu target

The wavelengths of characteristic x-rays depend on the type of target used. Typical x-ray diffractometry uses K x-rays generated by several types of metal targets, as shown in the following table. K x-rays contain K1 x-rays and K2 x-rays whose wavelengths are quite close. Although this does not pose serious problems for ordinary measurement of powder samples for phase indentification (ID) analysis, optimal results can be achieved by using only K1 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 K1 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 ()

Element Atomic number

K2 K1 K

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

Inte

nsity

Wavelength ()

Continuous x-rays

Characteristic x-rays

2.1 Horizontal sample mount high-accuracy theta-theta goniometer


2. Product Features 2.1 Horizontal sample mount 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 0.0001.

2.2 Attachment base (open Eurlerian cradle) and attachments

The attachment base has a chi axis for tilt adjustment, a Z axis for adjustment of sample thickness, and a phi axis for adjustment of in-plane orientation. Additionally, the phi axis can be equipped with an 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.

2.3 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 2.1 Generator specifications

Max. load Max. voltage Max. current Target metal 9kW rotating anode 9 kW 45 kV 200 mA Cu 3kW sealed tube 3 kW 60 kV 50 mA Cu

2.4 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.

2. Product Features

4 SmartLab Horizontal Sample Mount X-Ray Diffractometer for Thin Film Analysis

2.5 Crystal 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. Crystal adjustment positions are preserved even after the unit is removed, enabling data measurements without readjustment, simply by installing the previously adjusted crystal.

2.6 Receiving analyzer system

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

1. Double-slit analyzer with two variable slits on receiving side Para-focusing,, small-angle scattering, and reflectivity measurement geometries, etc.

2. 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.

3. 2-bounce analyzer Reflectivity measurements requiring high resolution, RSM measurements, and rocking curve measurements, etc.

2.7 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.

1. CBO unit for incident beam selection

2. Standard incident optics unit to select Soller slit, 2-bounce monochromator (with Soller slit), or 4-bounce monochromator

3. Standard incident slit box equipped with variable slit and length-limiting slit

2.8 Receiving optics system


2.8 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.

1. Standard receiving slit box # 1 for installation of a K x-ray filter for measurements using para-focusing optics

2. Standard receiving optics unit # 1 for installation of various analyzers

3. Standard receiving optics unit # 2 for installation of parallel slit such as Soller slits

4. Standard receiving slit box # 2 with a slit position alignment mechanism

5. Standard attenuator for the adjustment of x-ray intensity

2.9 Optics switching system

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

2.10 Optical device detection

The control software 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 Width of receiving slit Type of analyzer Type of receiving Soller slit Presence/absence of diffracted beam monochromator, etc.

The control software checks whether the necessary optical devices are installed and displays a message for the optical configurations suitable for the users intended application. The measurement data file stores parameters for the optical devices during measurement to improve data reproducibility and traceability.

2. Product Features


2.11 Control software

The software used to control the instrument also guides the user through required measurement procedures and condition-setting processes, in addition to providing conventional instrument 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.

2.12 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. The control software 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.

2.13 In-plane optics for detailed analysis of thin film structure

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.


3. Names of Parts of the Instrument

Fig. 3.1 General view of the instrument

1. Rotary pump Pump for maintaining the vacuum in the x-ray generator.

2. Control PC PC used to control the instrument.

3.1 Main unit

Fig. 3.2 Front view of the instrument

1. Main panel Panel used to start and stop the instrument.

2. Operating panel Panel used to enable opening/closing of the door and turn the internal light on/off.

3. Door This door is opened to change samples and optical devices.

4. X-ray generator warning light Lights when x-rays are generated.

1

2

3 4

1

2



Fig. 3.3 Rear view of the instrument

5. Power input connector External power supply connects here.

6. Connector for control PC The cables used to control the instrument connect here. RCD: Connected to COM1 port of the PC XG: Connected to COM2 port of the PC

7. Connectors for rotary pump The power supply and the control cable for the rotary pump connect here.

8. Connectors for water circulation pump The water circulation pump (short-cut valve) control connects here.

9. Pipes for cooling water and rotary pump The cooling water pipe of the x-ray generator and the rotary pump pipe connect here.

10. Circuit breaker Circuit breaker for the power supply to the main unit.

5

6

7, 8

9

10

3.2 Goniometer


3.2 Goniometer

Fig. 3.4 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 attachment Adjusts the position and orientation of the sample to be

measured.

1

4

2

3

5

6

7



Selection slit

Incident parallel slit adaptor/monochromator

Incident length-limiting slit 10, 15 (mm), etc.

Incident slit box (see section 7.3)

PB, BB, SA, etc.

CBO unit (see section 7.1)

Soller slit 5.0 deg., in-plane PSC 0.5 deg., Ge(220)x2, etc.

Incident optics unit (see section 7.2)

Theta_s arm

Height reference sample plate, 4-inch sample plate, etc.

Sample plate (see section 10)

Standard, XY-4, etc. Attachment (see section 9)

0-3 mm, 3-6 mm, etc.

Sample plate (see section 10)

Sample plate

Sample spacer

Attachment

Sample attachment

Detector (see section 8)

Receiving slit box # 2 (see section 7.7)

PSA 0.114 deg., Ge(220)x2, etc.

Receiving optics unit 1 (see section 7.5)

Soller slit 5.0 deg., in-plane PSA 0.5 deg., etc.

Receiving optics unit 2 (see section 7.6)

K filter

Receiving optical device adaptor/analyzer PSA

Receiving parallel slit adaptor Soller slit/in-plane PSA

Scintillation counter/diffracted beam monochromator for Cu

Theta_d arm

3.3 X-ray tube


3.3 X-ray tube

Fig. 3.5 Rotating anode x-ray tube

1. Cooling water pipe Connect the x-ray generator cooling water 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) Evacuates the x-ray generator.

Fig. 3.6 Sealed x-ray tube

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.

1 2

3

5 1

2

4 3

6



3.4 Theta_s arm

Fig. 3.7 Theta_s arm

1. Incident connector box The control cable of the optical device connects here.

2. Cross beam optics (CBO) unit Optics unit for switching optics.

3. Incident optics unit Soller units, monochromators, etc. are installed here

4. Incident slit box Variable slit on the incident side.

1

2 3

4

3.5 Theta_d arm


3.5 Theta_d arm

Fig. 3.8 Theta_d arm

1. Receiving connector box The control cables for the optical devices connect here.

2. Receiving slit box # 1 Variable slit on receiving side.

3. Receiving optics unit # 1 Receiving optical devices (analyzer) are 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.

1

2

3 4

5 6



3.6 Detector mounting bracket

Fig. 3.9 Detector mounting bracket

1. Counter adaptor Used to attach the detector.

2. Base Used to secure the detector in place.

3.7 Attachment base and attachments

Fig. 3.10 Attachment base and example attachment

1. Attachment base Sample attachment unit.

2. Attachment Attachment to be mounted to the attachment base.

3. Sample spacer Used to adjust sample thickness.

4. Sample plate Plate on which sample holder or sample is placed.

1

2

1

23 4

4.1 Control software


4. Software Configuration 4.1 Control software

SmartLab Guidance Used to control SmartLab and perform measurements.

4.2 Data processing software

Standard data processing Performs basic data processing such as smoothing,

background removal, etc.

4.3 Data display software

Multiple recording Superimposes multiple measurement data for display.

3D Explore (option) Displays two-dimensional data such as RSM, pole figure,

etc. Performs simple data processing.

4.4 Analysis software (options)

JADE Performs basic data processing.

The additional functions are used to perform phase ID analysis, quantitative analysis, Rietveld analysis, etc.

GXRR Performs reflectivity analysis.

NANO-Solver Performs particle size/pore diameter distribution analysis.

Pore size analysis Performs analysis of particle size/pore diameter

distribution of thin film, accounting for diffuse scattering from surface and interface.

Rocking curve data processing

Performs simulation and analysis of rocking curve.

QA-Tex Performs quantitative analysis of the preferred

orientation of a sample.

Visual RIETAN Performs Rietveld analysis using RIETAN2000 and

MEM analysis using VENUS.

Tube voltage and tube current

The intensity of characteristic x-rays is proportional to the nth 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 K 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 K filter method, the P/B ratio (peak-to-background ratio) setting should be chosen.

Optimum voltage

(equivalent load) (kV) Target Minimum

excitation voltage

(kV) Intensity

at maximum

P/B ratio at maximum

Cu 8.86 40 to 55 25 to 35 Co 7.71 35 to 50 25 to 35 Fe 7.10 35 to 45 25 to 35 Cr 5.98 30 to 40 20 to 30

5.1 Turning on the instrument


5. Turning on and off the instrument Described below are the procedures for turning on and off the instrument.

5.1 Turning on the instrument

(1) Make sure the LINE lamp is on.

(2) Press the | ON button on the main panel.

Fig. 5.1 Main panel

(3) Make sure the | ON button lights.

(4) Make sure the OPERATE lamp changes from red to green.

Tip: The red lamp goes on when the instrument is starting up or when an error occurs. For detailed information, refer to section 16 in this manual.

5.2 Starting SmartLab Guidance (control software)

(1) Start SmartLab Guidance.

(2) Click the Start button. Select All Programs Rigaku SmartLab Guidance, then select SmartLab Guidance.

(3) At the login dialog, enter the registered user name and password in the fields for Login name and Password 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.)

(4) The control axes are initialized after the software is launched.

Tip: For detailed information on initialization, refer to section 14 in the SmartLab Guidance Reference Manual (ME13365A).

5. Turning on and off the instrument


5.3 Starting the x-ray generator

Select Package measurement from the Task menu and click Startup on the displayed Package measurement flow bar.

Fig. 5.2 Starting the x-ray generator

Tip: For more information on the startup procedure, refer to the SmartLab Guidance Package Measurement Manual (ME13405A).

CAUTION: 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 of water is 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.

5.4 Stopping the x-ray generator


5.4 Stopping the x-ray generator

Select Package measurement from the Task menu and click Shutdown in the displayed Package measurement flow bar.

Fig. 5.3 Shutting down the x-ray generator

Tip: For more information on the shutdown procedure, refer to the SmartLab Guidance Package Measurement Manual (ME13405A).

When not using the instrument, turn off the x-ray generation without shutting off the exhaust control. This continues to supply power to the controller so that the x-ray generator can be started (e.g., for aging) from the PC.

To completely shut down the power supply when not using the instrument for extended periods, power off the instrument.

Tip: We recommend keeping the vacuum equipment running. Shutting down the vacuum equipment may result in instrument damage.

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

5. Turning on and off the instrument


5.5 Turning off the instrument

When not using the instrument for an extended period, power the instrument down by the following procedure.

(1) Check the instrument status (e.g., confirm that measurements have been completed).

(2) Press the c OFF button on the main panel.

Fig. 5.4 Main panel

(3) Make sure the illuminated | ON button turns off.

Tip: This procedure completely shuts down the instrument internal power supply. Only the LINE lamp will remain lit. This lamp indicates that power is being supplied to the main unit.

6.1 Opening the door


6. 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:

6.1 Opening the door

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

(1) Press the DOOR LOCK button on the operating panel.

Fig. 6.1 Operating panel

(2) Close the shutter.

(3) The door will be unlocked.

(4) The DOOR LOCK button will flash, and you will hear beeping.

(5) Open the door.

CAUTION: 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.

6. Opening and Closing the Door


6.2 Closing the door

(1) Make sure the door is securely closed.

(2) Press the DOOR LOCK button on the operating panel.

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

6.3 Emergency stop switch (EMO)

Press this switch in the event of an emergency to trip the circuit breaker and cut off the power supply to the main unit.

To cancel the emergency stop status, turn the button clockwise. After confirming safety, turn on the circuit breaker to restart the instrument (see 5.1 through 5.3).

CAUTION: After restarting the instrument, also restart SmartLab Guidance.

Fig. 6.2 Emergency stop switch (EMO)

7.1 CBO unit (for Cu target)


7. Optics This section introduces the names of parts and describes how they are installed.


The CBO unit is designed for characteristic x-rays (K x-rays) generated by the standard Cu target. Changing selection slits allows switching between divergent and parallel 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 the PC.

Fig. 7.1 CBO unit

(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.

Fig. 7.2 Installing the CBO unit

7. Optics


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

Fig. 7.3 Cable connection

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

Fig. 7.4 Installing the selection slit



Table 7.1 Selection slits

Name of optics Abbreviation Illustration For para-focusing BB

For parallel beam PB

For small-angle

scattering measurements (option)

SA

For micro area

measurements (option)MA

For small-angle

scattering high-intensity

measurements (option)

SA01

Tip: The type of selection slit installed can be identified from the PC.

7. Optics


7.2 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. The type of installed optical device can be identified from the PC.

7.2.1 Incident parallel slit adaptor (IPS adaptor)

This adaptor is used to install a parallel slit.

Fig. 7.5 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.

Fig. 7.6 Installing the incident parallel slit adaptor



(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.

Fig. 7.8 Installing the parallel slit

7. Optics


Table 7.2 Incident parallel slits

Type Divergence limit angle

Abbreviation Illustration

Open (option)

None Soller Slit open

Soller slit 5 Soller Slit 5.0 deg

Soller slit (option)

2.5 Soller Slit 2.5 deg

In-plane PSC

(parallel slit collimator) (option)

1.0 In-plane PSC 1.0 deg

In-plane PSC

(option) 0.5 In-plane PSC 0.5

deg

In-plane PSC


deg

Tip: The type of installed incident parallel slit can be identified from the PC.



7.2.2 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 the PC.

A dedicated parallel slit can be installed after the channel cut crystal.

Fig. 7.9 2-Bounce monochromator

(1) Attach the 2-bounce monochromator to the CBO unit by sliding it down from the top


Fig. 7.10 Installing the 2-bounce monochromator

7. Optics




(3) Install a parallel slit on the 2-bounce monochromator. Secure it in place with the Allen

wrench provided.




Table 7.3 2-bounce monochromators

Crystal Diffraction

plane Abbreviation Illustration

Ge (option)

220 Ge (220) x 2

Ge

(option) 400 Ge (400) x 2

Tip: The type of installed crystal can be identified from the PC.

Table 7.4 Parallel slits for 2-bounce monochromator

Type Divergence Abbreviation Illustration Open

(provided with the unit)

None Soller slit open


5.0 Soller slit 5.0 deg



In-plane PSC


deg

Tip: The type of parallel slit installed on the adaptor can be identified from the PC.

7. Optics


7.2.3 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 the PC.

Fig. 7.13 4-bounce monochromator

(1) Attach the 4-bounce monochromator to the CBO unit by sliding it down from the top


Fig. 7.14 Installing the 4-bounce monochromator





Table 7.5 4-bounce monochromators

Crystal Diffraction


Ge (option)

220 Ge (220) x 4

Ge (option)

440 Ge (440) x 4

Tip: The type of installed crystal can be identified from the PC.

7. Optics


7.3 Incident slit box

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

7.3.1 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.

The slit width can be controlled from the PC. A length-limiting slit can also be inserted to limit the beam length along the longitudinal axis.

Fig. 7.16 Standard incident slit box

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

provided.

Fig. 7.17 Installing the standard incident slit box

7.3 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.

Fig. 7.19 Inserting the length-limiting slit

7. Optics


Table 7.6 Length-limiting slits

Length of limiting slit

Abbreviation Illustration

15 mm 15

10 mm 10

5 mm 5

2 mm 2

0.5 mm for micro area optics

(option)

0.5

Tip: The type of inserted length-limiting slit can be identified from the PC.

7.4 Receiving slit box # 1



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

7.4.1 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 the PC. A K filter can be inserted to remove K x-rays from characteristic x-rays.

Fig. 7.20 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.

Fig. 7.21 Installing the standard receiving slit box # 1

7. Optics


(2) Connect the cable to the SLIT1 connector on the receiving connector box.


(3) A K filter may be inserted.

Fig. 7.23 K filter insertion position

Tip: Determine whether a K filter is inserted from the PC.



Fig. 7.24 K filter (Ni foil)

Tip: The K filter reduces the K characteristic x-rays from by approximately 99% while only reducing the K characteristic x-rays by approximately 50%. Use of the K filter thereby eliminates In this way, the K filter virtually eliminates the unwanted K x-rays while only reducing the desired K x-rays by 50%. (Used for measurements based on the para-focusing method)

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

Fig. 7.25 Confirming the installation position

7. Optics


7.5 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. The type of analyzer installed can be identified from the PC.

7.5.1 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.

Fig. 7.26 Receiving optical device adaptor

(1) Attach the receiving optical device adaptor to the rail of the theta_d arm. Secure it in place


Fig. 7.27 Installing the receiving optical device adaptor



(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.

Fig. 7.29 Installing the parallel slit analyzer

7. Optics


Table 7.7 Parallel slit analyzers

Aperture angle Length Abbreviation Illustration Open 45 mm PSA open

1.0

(option) 45 mm PSA 1.0 deg

0.5 45 mm PSA 0.5 deg

0.114

(option) 90 mm PSA 0.114

deg

Open 90 mm PSA open

CAUTION: The standard configuration of the 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.

Tip: The type of parallel slit analyzer installed on the adaptor can be identified from

the PC.



7.5.2 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 the PC.

Fig. 7.30 2-bounce analyzer

(1) Attach the 2-bounce analyzer to the theta_d arm. Secure it in place with the Allen wrench provided.

Fig. 7.31 Installing the 2-bounce analyzer

7. Optics




Table 7.8 Crystal types

Crystal Diffraction


Ge (option)

220 Ge (220) x 2

Ge (option)

400 Ge (400) x 2

Tip: The type of crystal currently installed can be identified from the PC.




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

7.6.1 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.

Fig. 7.33 Receiving parallel slit adaptor

(1) Attach the receiving parallel slit adaptor to the rail of the theta_d arm. Secure it in place


Fig. 7.34 Installing the receiving parallel slit adaptor

7. Optics




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




Table 7.9 Receiving parallel slits

Type Aperture

angle Abbreviation Illustration

Soller slit 5.0 Soller slit 5.0 deg



In-plane PSA

(option) 1.0 In-plane PSA 1.0 deg

In-plane PSA

(use of PSA 0.5 deg.) 0.5 In-plane PSA 0.5 deg

In-plane PSA

(use of PSA 0.114 deg.)

0.114 In-plane PSA 0.114 deg

Tip: The type of parallel slit currently installed on the adaptor can be identified from the PC.

7. Optics



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

7.7.1 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 the PC.

Fig. 7.37 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


Fig. 7.38 Installing the standard receiving slit box # 2



(2) Connect the cable to the SLIT2 connector on the receiving connector box.


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

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

Fig. 7.40 Confirming the installation position

7. Optics


7.8 Attenuator

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

7.8.1 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 the PC. Attenuators can be switched automatically for various measurements based on detected intensity.

Fig. 7.41 Standard attenuator

(1) Attach the standard attenuator to the rail of the theta_d arm. Secure it in place with the

Allen wrench provided.

Fig. 7.42 Installing the standard attenuator

7.8 Attenuator


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


Tip: 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.

K filter

The characteristic x-rays used for x-ray diffractometry generally contain K and K x-rays. A substance that passes K x-rays while absorbing most K x-rays to monochromatize the beam is called a K filter. The mass absorption coefficient (hereafter 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.

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

For efficient absorption of K x-rays only, select an element with its absorption edge wavelength located between the K x-ray and K 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 K filters Wavelength () Filter

When 100/111 = KK II Target

K1 K1 Material Wavelength of absorption edge

() Thickness

(mm) Thickness (g/cm2)

K1 transmissivity

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

Mas

s ab

sorp

tion

coef

ficie

nt

LI absorption edge

LII absorption edge

Wavelength ()

K absorption edge

LIII absorption edge

8.1 Counter adaptor


8. Detector

8.1 Counter adaptor

This adaptor is used to install the detector (scintillation counter).

Fig. 8.1 Counter adaptor

(1) Attach the counter adaptor to the rail of the theta_d arm. Secure it in place with the Allen

wrench provided.

Fig. 8.2 Installing the counter adaptor

8. Detector


(2) Connect the cable to the COUNTER connector on the receiving connector box.


8.2 Scintillation counter


8.2 Scintillation counter

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

Determine whether the scintillation counter is installed from the PC.

Fig. 8.4 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.

Fig. 8.5 Installing the base

8. Detector


(2) Attach the base to the counter adaptor. Secure it in place with the All

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