Cat. No. 2080A102/B101/M101/M102 Smartlab Horizontal Sample Mount X-Ray Diffractometer For Thin Film Analysis Instruction Manual

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.
ME11507B
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.
ME11507B
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.
ME11507B
(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.
ME11507B
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.
DO NOT REMOVE
SHUTTER
RADIATION HAZARD
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.
ME11507B
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.
ME11507B
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.
ME11507B
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.
HOT
KEEP AWAY
FROM FURNACE
(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.
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.
ME11507B
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.
ME11507B
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.
ME11507B
Radiation Protection Mechanisms and Functions

Component
X-ray generator section
Solenoid shutter
Mechanism
(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.
Function
Complete shielding
Same as above
Warning
Fail-safe operation
(6) When the mechanical connection to the goniometer Safety assurance and
or other external X-ray utilization section is lost, the radiation exposure
auxiliary shutter element is closed by its internal
possibility minimization
spring. In this instance, the main shutter element Same as above
also closes. (Except the rotary shutter)
Radiation enclosure
(7) X-ray generation is indicated by the red warning
Warning
lamp on the radiation enclosure.
(8) X-ray generation is unachievable when the X-ray
Fail-safe operation
generation indicator lamp is burned out.
(9) The goniometer and other mechanical operation
Shielding from scattered
sections are entirely covered by the radiation
X-rays
enclosure (box with a 3.2 mm thick iron lid).
(10) The radiation enclosure side wall positioned in the Shielding from possible
direct X-ray radiation direction is provided with a direct X-rays
2.5 mm thick, large lead plate.
(11) The X-ray shutter does not open if the radiation
Fail-safe operation
enclosure door is open.
(12) X-ray generation is unachievable when the warning Fail-safe operation
lamp described in paragraph (7) above is burned
out.
SAFETY RELEASE unit (13) Key input is needed to disable the safety feature.
Indication of the
When the safety feature is disabled, the SAFETY possibility of radiation
RELEASE unit red LED blinks and the alarm
exposure
buzzer intermittently beeps, indicating that you can
manually open and close the X-ray shutter.
(14) When you press the DOOR OPEN button, its
Shielding from X-rays in
signal is processed by the computer, and the yellow the event of inadvertent
lamp blinks at the operation panel to indicate that door opening
the door can be opened.
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.
ME11507B
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
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
3.
4.
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
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
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
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
SmartLab Horizontal Sample Mount X-Ray Diffractometer for Thin Film Analysis
Contents
6.
7.
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
Optics ....................................................................................................................................................... 23
7.1
CBO unit (for Cu target)................................................................................................................. 23
7.2
Incident optics unit (standard incident optics unit)......................................................................... 26
7.3
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
Incident slit box .............................................................................................................................. 34

7.3.1
7.4
Receiving slit box # 1 ..................................................................................................................... 37

7.4.1
7.5
7.6
7.5.1
Receiving optical device adaptor (ROD adaptor) ................................................................ 40
7.5.2
2-bounce analyzer (option) .................................................................................................. 43
Receiving optics unit # 2 ................................................................................................................ 45
Standard receiving slit box # 2............................................................................................. 48
Attenuator ....................................................................................................................................... 50
7.8.1
8.
Receiving parallel slit adaptor (RPS adaptor) ...................................................................... 45
Receiving slit box # 2 ..................................................................................................................... 48

7.7.1
7.8
Standard receiving slit box # 1............................................................................................. 37
Receiving optics unit # 1 ................................................................................................................ 40
7.6.1
7.7
Standard incident slit box..................................................................................................... 34
Standard attenuator .............................................................................................................. 50
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
ii
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
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
14.
15.
16.
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
Measurements ....................................................................................................................................... 75
14.1
Launching the software................................................................................................................. 75
14.2
Setting the hardware configuration............................................................................................... 75
14.3
Selecting a measurement package ................................................................................................ 76
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
Troubleshooting.................................................................................................................................... 79
Appendix
Using the OPERATE lamp ...................................................................................................... 80
First Edition: December 14, 2005 Japanese

Second Edition: September 28, 2006
iii
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.
Soller slit
Para-focusin
g method
Soller slit
Soller slit
SmartLab
9-kW system
Parallel beam
Ni filter
2-bounce
monochromator
+
Soller slit
Soller slit
PSA
Soller slit
PSA
Soller slit
2-bounce analyzer
2-bounce analyzer
Micro area
In-plane
optics
Soller slit
Soller slit
Soller slit
PSC
PSA
Parallel beam
CBO unit
Fig. 1.1
Phase ID
analysis/
quantitative
analysis
Powder profile analysis

Preferred orientation
measurement
Thin-film/thick-film
measurement
Film thickness measurement

Reciprocal space mapping
Rocking curve
Soller slit
Soller slit
2-bounce
monochromator
+
PSC
Diffracted beam
monochromator
Soller slit
Soller slit
4-bounce
monochromator
SAXS
Soller slit
Particle size/pore diameter

distribution
Micro region
Preferred orientation measurement

In-plane measurement
PSA
Incident optics system Receiving optics system
SmartLab structure and measurement examples
Characteristic x-rays
X-Rays are generated by accelerating electrons to very high speeds in a vacuum and directing
them against the anode (target). The x-ray spectra generated by electrons colliding against the
target can be divided into two categories: a continuous spectrum indicating continuous x-rays
(white x-rays) and a discrete spectrum for characteristic x-rays.
4000
Intensity
Characteristic
x-rays
X
2000
Continuous
x-rays
0
0
0.5
Wavelength
1 ()
1.5
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
Target
Element
Atomic
number
Cr
24
Fe
26
Co
27
Cu
29
Mo
42
Ag
47
W
74
Wavelengths of characteristic x-rays

K2
Wavelength ()
K1
2.294
1.940
1.793
1.544
0.7135
0.5638
0.2138
2.290
1.936
1.789
1.541
0.7093
0.5594
0.2090
2.085
1.757
1.621
1.392
0.6323
0.4970
0.1844
2.1
2.
Horizontal sample mount high-accuracy theta-theta goniometer
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
2.4
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
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
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.
2.7
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.
Incident optics system

The following mechanisms enable switching between para-focusing optics, parallel beam optics, 2or 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
2.8
Receiving optics system
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.
2.9
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
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

1
Fig. 3.1
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.
Main unit
4
3
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.
3.
9
5
10
7, 8
6
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.
3.2
3.2
Goniometer
Goniometer
4
5
7
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.
3.
Theta_s arm
Selection slit
PB, BB, SA, etc.
CBO unit (see section 7.1)

Incident length-limiting slit
10, 15 (mm), etc.
Incident slit box (see section 7.3)
Incident parallel slit

adaptor/monochromator
Soller slit 5.0 deg., in-plane PSC 0.5 deg., Ge(220)x2, etc.
Incident optics unit (see section 7.2)
Theta_d arm
K filter
Receiving slit box # 2 (see section 7.7)
Receiving optical device adaptor/analyzer
PSA
PSA 0.114 deg., Ge(220)x2, etc.
Receiving optics unit 1 (see section 7.5)

Receiving parallel slit adaptor
Soller slit/in-plane PSA
Soller slit 5.0 deg., in-plane PSA 0.5 deg., etc.
Receiving optics unit 2 (see section 7.6)

Scintillation counter/diffracted beam
monochromator for Cu
Detector (see section 8)
Sample attachment
Sample plate
Height reference sample plate, 4-inch sample
plate, etc.
Sample plate (see section 10)

Sample spacer
0-3 mm, 3-6 mm, etc.
Sample plate (see section 10)

Attachment
Standard, XY-4, etc.
Attachment (see section 9)
10
3.3
3.3
X-ray tube
X-ray tube
4
6
2
1
5
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.
1
2
Fig. 3.6
Sealed x-ray tube
1. Cooling water pipe
Connect the x-ray generator cooling water pipe.
2.
X-ray generating source.
X-ray tube
3. Shutter
Controls x-ray emissions.
11
3.
3.4
Theta_s arm
2
1
Fig. 3.7
12
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.
3.5
3.5
Theta_d arm
Theta_d arm
3
6
Fig. 3.8
1
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.
13
3.
3.6
Detector mounting bracket
Fig. 3.9
3.7
Detector mounting bracket
1. Counter adaptor
Used to attach the detector.
2. Base
Used to secure the detector in place.
Attachment base and attachments
2
3
Fig. 3.10
14
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.
4.1
4.
Control software
Software Configuration
4.1
Control software
SmartLab Guidance
4.2
Used to control SmartLab and perform measurements.
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)

Performs basic data processing.
JADE
The additional functions are used to perform phase ID

analysis, quantitative analysis, Rietveld analysis, etc.
GXRR
Performs reflectivity analysis.

Performs particle size/pore diameter distribution
NANO-Solver
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
Performs simulation and analysis of rocking curve.
processing
QA-Tex
Performs quantitative analysis of the preferred

orientation of a sample.
Visual RIETAN
Performs Rietveld analysis using RIETAN2000 and

MEM analysis using VENUS.
15
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.
Target
Minimum
excitation
voltage
(kV)
Cu
8.86
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
Optimum voltage
(equivalent load) (kV)
Intensity
P/B ratio at
at
maximum
maximum
40 to 55
25 to 35
5.1
5.
Turning on the instrument
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).
17
5.
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
Tip:
Starting the x-ray generator
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.
18
5.4
5.4
Stopping the x-ray generator
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
Tip:
Shutting down the x-ray generator
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.)
19
5.
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.
20
6.1
6.
Opening the door
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.
21
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
22
Emergency stop switch (EMO)
7.1
7.
CBO unit (for Cu target)
Optics
This section introduces the names of parts and describes how they are installed.
7.1

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
23
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
24
Installing the selection slit
7.1
Table 7.1
Tip:
Selection slits
Name of optics
Abbreviation
For para-focusing
BB
For parallel beam
PB
For small-angle
scattering
measurements (option)
SA
For micro area

MA
For small-angle
scattering
high-intensity
SA01
Illustration
The type of selection slit installed can be identified from the PC.
25
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
(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
26
Incident parallel slit adaptor
Installing the incident parallel slit adaptor
7.2
(2)
Connect the cable to the MONO/ADPT connector on the incident connector box.
Fig. 7.7
(3)
Cable connection
Install the parallel slit on the adaptor and secure it in place with the Allen wrench provided.
Fig. 7.8
Installing the parallel slit
27
7.
Optics
Table 7.2
Type
Open
Incident parallel slits
Divergence
limit angle
Abbreviation
None
Soller Slit open
Soller slit
Soller Slit 5.0 deg
Soller slit
2.5
Soller Slit 2.5 deg
1.0
In-plane PSC 1.0
Illustration
(option)
(option)
In-plane PSC
(parallel slit collimator)
deg
(option)
In-plane PSC
0.5
(option)
In-plane PSC
(option)
Tip:
28
In-plane PSC 0.5

deg
0.15
In-plane PSC 0.15

deg
The type of installed incident parallel slit can be identified from the PC.
7.2
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
(1)
2-Bounce monochromator
Attach the 2-bounce monochromator to the CBO unit by sliding it down from the top
Fig. 7.10
Installing the 2-bounce monochromator
29
7.
Optics
(2)
Fig. 7.11
(3)
Install a parallel slit on the 2-bounce monochromator. Secure it in place with the Allen
wrench provided.
Fig. 7.12
30
Cable connection
7.2
Table 7.3
2-bounce monochromators
Diffraction
Crystal
plane
Ge
Abbreviation
220
Ge (220) x 2
400
Ge (400) x 2
Illustration
(option)
Ge
(option)
Tip:
The type of installed crystal can be identified from the PC.
Table 7.4
Parallel slits for 2-bounce monochromator
Type
Divergence
Abbreviation
Open
None
Soller slit open
5.0
Soller slit 5.0 deg
2.5
Soller slit 2.5 deg
0.5
In-plane PSC 0.5
Illustration
(provided with the

unit)
Soller slit
(option)
Soller slit
(option)
In-plane PSC
(option)
Tip:
deg
The type of parallel slit installed on the adaptor can be identified from the PC.
31
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
(1)
Attach the 4-bounce monochromator to the CBO unit by sliding it down from the top
Fig. 7.14
32
4-bounce monochromator
Installing the 4-bounce monochromator
7.2
(2)
Fig. 7.15
Table 7.5
Crystal
Ge
4-bounce monochromators
Diffraction
plane
Cable connection
Abbreviation
220
Ge (220) x 4
440
Ge (440) x 4
Illustration
(option)
Ge
(option)
Tip:
The type of installed crystal can be identified from the PC.
33
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
(1)
Attach the standard incident slit box to the Zs axis. Secure it in place with the Allen wrench
provided.
Fig. 7.17
34
Standard incident slit box
Installing the standard incident slit box
7.3
(2)
Connect the cable to the SLIT connector on the incident connector box.
Fig. 7.18
(3)
Incident slit box
Cable connection
Insert a length-limiting slit to control beam length along the longitudinal axis.
Fig. 7.19
Inserting the length-limiting slit
35
7.
Optics
Table 7.6
Tip:
36
Length-limiting slits
Length of limiting
slit
Abbreviation
15 mm
15
10 mm
10
5 mm
2 mm
0.5 mm for
micro area optics
(option)
0.5
Illustration
The type of inserted length-limiting slit can be identified from the PC.
7.4
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
(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
37
7.
Optics
(2)
Connect the cable to the SLIT1 connector on the receiving connector box.
Fig. 7.22
(3)
A K filter may be inserted.
Fig. 7.23
Tip:
38
Cable connection
K filter insertion position
Determine whether a K filter is inserted from the PC.
7.4
Fig. 7.24
Tip:
K filter (Ni foil)
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
39
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
(1)
Attach the receiving optical device adaptor to the rail of the theta_d arm. Secure it in place
Fig. 7.27
40
Receiving optical device adaptor
Installing the receiving optical device adaptor
7.5
(2)
Connect the cable to the ADPT1 connector on the receiving connector box.
Fig. 7.28
(3)
Cable connection
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
41
7.
Optics
Table 7.7
Parallel slit analyzers
Aperture angle
Length
Abbreviation
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
Open
90 mm
Illustration
deg
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.
42
7.5
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
(1)
2-bounce analyzer
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
43
7.
Optics
(2)
Fig. 7.32
Cable connection
Table 7.8
Crystal
Ge
Diffraction
plane
Crystal types
Abbreviation
220
Ge (220) x 2
400
Ge (400) x 2
Illustration
(option)
Ge
(option)
Tip: The type of crystal currently installed can be identified from the PC.
44
7.6
7.6

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
(1)
Receiving parallel slit adaptor
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
45
7.
Optics
(2)
Fig. 7.35
(3)
Attach a parallel slit to the adaptor. Secure it in place with the Allen wrench provided.
Fig. 7.36
46
Cable connection
7.6
Table 7.9
Receiving parallel slits
Type
Aperture
angle
Abbreviation
Soller slit
5.0
Soller slit 5.0 deg
Soller slit
(option)
2.5
Soller slit 2.5 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:
Illustration
The type of parallel slit currently installed on the adaptor can be identified from
the PC.
47
7.
Optics
7.7

This slit box is installed in from of the detector on the theta_d arm.
7.7.1

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
(1)
Attach the standard receiving slit box # 2 to the rail of the theta_d arm. Secure it in place
Fig. 7.38
48
Installing the standard receiving slit box # 2
7.7
(2)
Connect the cable to the SLIT2 connector on the receiving connector box.
Fig. 7.39
(3)
Cable connection
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
49
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
(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
50
Standard attenuator
Installing the standard attenuator
7.8
(2)
Attenuator
Connect the cable to the ATT connector on the receiving connector box.
Fig. 7.43
Tip:
Cable connection
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.
51
K filter
Mass absorption coefficient
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.
LI absorption
edge
LII absorption edge
LIII absorption
edge
K absorption
edge
Wavelength ()
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
Target
Wavelength ()
K1
K1
K filters
Filter
Material
Wavelength of
absorption edge
()
Thickness
(mm)
When I K I K = 1 / 100
Thickness
K1
transmissivity
(g/cm2)
1
Cr
2.290
2.085
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
8.1
8.
Counter adaptor
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
53
8.
Detector
(2) Connect the cable to the COUNTER connector on the receiving connector box.
Fig. 8.3
54
Cable connection
8.2
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
(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
55
8.
Detector
(2) Attach the base to the counter adaptor. Secure it in place with the Allen wrench provided.
Fig. 8.6
Installing the base to the counter adaptor
(3) The installation position can be read from the scale on the theta_d arm.
Fig. 8.7
56
8.3
8.3
Diffracted beam monochromator unit for Cu (DBM unit)

This unit is used to monochromatize the diffracted beam such that only K x-rays are detected.
Change the curvature of the monochromating crystal from Bent (para-focusing geometry) to Flat
(parallel beam geometry) by rotating the dial on the top of the monochromator housing.
Changeover dial
Fig. 8.8
Diffracted beam monochromator unit for Cu
(1) Install the scintillation counter on the diffracted beam monochromator unit. Secure it in place
Fig. 8.9
Installing the scintillation counter
57
8.
Detector
(2) Install the unit on the counter adaptor. Secure it in place with the tool provided.
Fig. 8.10
Installing the unit on the counter adaptor
(3) The unit installation position can be read from the scale on the theta_d arm.
Fig. 8.11
CAUTION: When using the monochromator in Bent mode with

para-focusing optics, the unit must be installed at a specific
for a specific target given in the table below. When using the
monochromator in Flat mode, the exact position is not
important.
Type of target
Cu
Co
Fe
Cr
58
Installation position
351.5 mm
359.8 mm
364.7 mm
376.1 mm
8.3
(4) Insert the monochromator slit (RSm) into the unit.

The presence/absence of the slit can be confirmed from the PC.
Fig. 8.12
Installing the monochromator slit (RSm)
CAUTION: Use the RSm only when using the monochromator in Bent
mode for the para-focusing method. The RSm is not used
when using the monochromator in Flat mode.
59
Incident monochromator crystal

The incident monochromator crystal system uses diffraction by Ge or Si crystals for x-ray
monochromatization. Ge(220)x2 crystals and Ge(440)x4 crystals are available as options for
SmartLab. Select the appropriate crystal based on the resolution required for measurements
and the sample (d value). As an example, the Ge(220)x2 crystal monochromatizes x-rays by
diffracting them twice by Ge(220) lattice planes. Passing x-rays through this crystal makes it
possible to use only K1 x-rays with about 0.003 degree divergence. Shown below are the
types and resolutions of monochromator crystals and corresponding applications.
Table
Types and resolutions of incident monochromator crystals
Type of
crystal
Resolution
(FWHM)
Resolutions and applications
Ge(220)x2
crystal
0.008<
For applications requiring monochromatized K1

x-rays.
Ge(400)x2
crystal
0.0022
(when sample d
spacing is
1.41A)
For high resolution high intensity measurements of

GaAs and other materials with diffraction planes with d
spacings of approximately 1.41.
Ge(220)x4
crystals
0.003<
For applications requiring high resolution over a broad

2-theta range.
Ge(440)x4
crystals
0.0015<
For applications requiring very high resolution over a

broad 2-theta range.
Intensity
[unspecified unit]
[]
Slit
collimation
Ge(220)2
Ge(220)2 crystal
Ge(220)4
Ge(220)4
crystal
Zoom
view
Cu K
W-L
61.00
63.00
69.00
65.00
69.10
69.20
67.00
69.00
2/ [deg]
Figure
2-theta/omega scan profile of Si(001) single crystal wafer measured with

different incident optics systems
9.
Attachments
You can switch between attachments with various adjust axes for different measurement purposes.
Described below is the method for changing attachments.

(1) Select Manual Control from the Control menu. Move the chi axis to 0 and the phi axis to 0.
(2) Disengage the latch on the front of the attachment.
(3) Open the clasps for the right and left sides. Remove the attachment.
Pin
Fig. 9.1
Removing the attachment
(4) Make sure the right and left clasps are open.
(5) Install the attachment by aligning the groove of the attachment with the pin on the front.
(6) Align the blades on both sides.
(7) Close the clasps and engage the front hook.
Fig. 9.2
Installing the attachment
61
9.
Attachments
Table 9.1
Name
Types of attachments
Description
Standard attachment
Illustration
This attachment has no moving

axis.
It is used for reflectivity
measurements and measurements
of powder and bulk samples.
RxRy attachment
This attachment has Rx and Ry
(option)
axes that permit tilt adjustments of

two axes intersecting at right
angles.
It is used for RSM measurements
and various types of in-plane
measurements.
XY-20 attachment
This attachment has +/- 10 mm X
(option)
and Y translation axes which are

perpendicular to each other.
It is used to position the sample
for micro area measurements.
This attachment cannot be used
with 8-inch wafer sample plates.
XY-4 phi attachment

(option)
This attachment has +/- 50 mm

provides X and Y translation axes
which are perpendicular to each
other.
It is used for full-map
measurement of 4-inch wafers.
This attachment can be used only
with the 4-inch XY mapping
sample plate.
Tip:
62
The type of attachment installed can be identified from the PC.
10.1
10.
Wafer sample plates and sample spacers
Sample plates
Select a sample plate based on the sample to be measured.
10.1

A wafer sample plate is used in measurements of wafer-shaped samples. A sample spacer is placed
on the attachment. The wafer sample plate is placed on the sample spacer. A sample is placed on top
of the wafer sample plate. Wafer sample plates and sample spacers are available for 4-inch, 6-inch,
and 8-inch samples.
Fig. 10.1
Wafer sample plate and sample spacer
CAUTION: Placing a sample larger than the sample plate may damage
the sample during measurement.
Magnets supplied with the product are generally used to secure the sample in place. Refer to 13.
Examples of sample mounting.
Fig. 10.2
Magnets for securing sample in place
Tip: The sample holding magnets can be used for samples measuring up to
approximately 3 mm in thickness.
63
10.
Sample plates
The Z axis is used to align the sample surface with the center of the x-ray beam. Since the thickness
range for which the Z axis can be adjusted is 3 mm, you must select the appropriate sample spacer
based on the thickness of the sample to be measured.
Table 10.1
Sample spacers
Sample thickness
Abbreviation
0-3 mm
0-3 mm
3-6 mm
3-6 mm
Illustration
(option)
6-9 mm
6-9 mm
(option)
9-12 mm
9-12 mm
(option)
0-3 mm (blue
0-3 mm (*1)
stamped mark)
12-15 mm
12-15 mm
(option)
3-6 mm (blue
3-6 mm (*1)
stamped mark)
15 mm-18 mm
15-18 mm
(option)
6-9 mm (blue
6-9 mm (*1)
stamped mark)
*1: Sample thickness for using XY-4 attachment. Refer to the abbreviations in blue.
64
10.1
Table 10.2
Wafer sample plates
Name
Illustration
4-inch wafer sample plate

(option)
(option)
(for 18-21 mm)
(option)
4-inch XY mapping sample
plate (option)
4-inch XY mapping sample
plate (for 18-21 mm)
(option)
Table 10.3
List of possible combinations of attachment, sample spacer, and sample plate
Attachment
Sample spacer
0-3 mm
3-6 mm
6-9 mm
Standard attachment
9-12 mm
RxRy attachment
12-15 mm
XY-20 mm
(black stamped mark)
attachment
Sample plate
Measurable
sample thickness
0-3 mm
6-inch wafer sample
3-6 mm
plate(*1)
6-9 mm
8-inch wafer sample
9-12 mm
plate(*1)
12-15 mm
4-inch wafer sample plate (for 18-21 mm)
18-21 mm

6-inch wafer sample plate(*1)
21-24 mm
8-inch wafer sample plate(*1)

0-3 mm
3-6 mm
6-9 mm
XY-4 attachment
(blue stamped
4-inch area mapping sample

plate
0-3 mm
3-6 mm
6-9 mm
mark)(*2)
4-inch area mapping sample plate (for 9-12 mm)
9-12 mm
4-inch area mapping sample plate
12-15 mm
*1: Both X and Y must be 0 mm when the sample is placed on the XY-20 mm attachment.
*2: When the XY-4 attachment is used, the thickness indicated by the blue stamp mark on the
sample spacer is valid.
65
10.
Sample plates
10.1.1
Installing and removing sample spacers

To mount a sample spacer to an attachment, align the sections indicated by the arrows in Fig.
10.3, then turn the sample spacer clockwise to secure it in place.
Fig. 10.3
Installing the sample spacer on the attachment
To remove the sample spacer from the attachment, apply pressure to the bar indicated by the
arrow in Fig. 10.4, then turn the sample spacer counterclockwise.
Fig. 10.4
66
Removing the attachment
10.1
10.1.2
Installing and removing wafer sample plates

To mount a wafer sample plate to a sample spacer, align the sections indicated by the arrows in
Fig. 10.5, then turn the sample plate clockwise to secure it in place.
The wafer sample plate can be removed by turning it counterclockwise.
Fig. 10.5
Installing/removing the wafer sample plate
Tip: Refer to 10.1.1 Installing and removing sample spacers for information on
direct mounting (removing) a wafer sample plate to (from) an attachment.
67
10.
Sample plates
10.2
Height reference sample plate

Insert a glass sample holder or aluminum sample holder into the height reference sample plate.
Place the height reference sample plate directly on the attachment.
To make adjustments, insert a center slit and Si powder reference sample.
Fig. 10.6
10.3
Height reference sample plate
Transmission SAXS sample plate (option)

A transmission SAXS sample holder is inserted into the transmission SAXS sample plate.
The transmission SAXS sample plate is placed directly on the attachment.
Fig. 10.7
Tip:
Transmission SAXS sample plate
Although the height reference sample plate and transmission SAXS sample plate
can be used on top of other attachments, it is recommended for maximum
precision that they be used attached to the standard attachment. If using the
height reference sample plate or transmission SAXS sample plate with an
attachment other than the standard attachment, you must set each attachment axis
to 0. Optics alignments, however, must be done with the height reference sample
plate attached to the standard attachment. Install/remove sample plates in the
same way as wafer sample plates.
68
11.1
11.
Glass sample holder
Sample holders
Use a sample holder when measuring samples that require preparation, such as powder and bulk
samples.
Tip:
For information on preparing samples, refer to section 2.8 in Quick theta/2-theta

measurement (BB) or Quick theta/2-theta measurement (PB/PSA) in the
SmartLab Guidance Package Measurement Manual (ME13405A).
11.1
Glass sample holder

Use this sample holder to measure powder samples.
Fig. 11.1
11.2
Glass sample holder
Aluminum sample holder

Use this sample holder to measure powder samples or small bulk samples.
Fig. 11.2
11.3
Aluminum sample holder
Transmission method sample holder (option)

Use this sample holder to measure fibrous or film samples by the transmission method.
Fig. 11.3
Transmission method sample holder
69
Penetration depth (effective thickness)

The following formula gives the ratio Gx between the intensity of diffracted x-rays from a
sample of infinite thickness and the intensity of diffracted x-rays from a sample with a specific
finite thickness of x cm.
dI D = 1 exp 2x
Gx = 0
sin
dI
0 D
Substitute the values for angle of the incident x-ray beam and x-ray absorption coefficient
(/cm) in the following formula to obtain x cm, the effective thickness.
x=
ln(1 G x ) sin K x sin

=
2
2
Diffracted x-ray utilization rate Gx

(%)
Kx
where,
K x = ln (1 G x )
50
75
90
95
99
99.5
0.69
1.39
2.30
3.00
4.61
6.91
The following table shows the results of calculations of the sample thicknesses x cm that give
a diffracted x-ray usage rate of 90% when Kx = 2.30 and = 90.
Substance
Al2O3
Si
SiO2
CaCO3
Powder
Fe2O3
ZnO
Ag2O
(tetragonal)
PbO I(
Al
Fe
Metal
SUS(18-8)
Cu
Pb
Polyethylene
Polymer
Vinyl chloride
Single crystal Si
substance
SiO2
Density
g/cm )
3.97/2
2.42/2
2.65/2
2.71/2
5.26/2
5.60/2
7.22/2
9.53/2
2.70
7.86
7.93
8.92
11.34
0.93
1.41
2.42
2.65
Mass/cm
absorption coefficient / /g)
(cm /g)
Thickness
for 90% utilization rate (mm)
90%mm)
MoK CuK CoK CrK MoK CuK CoK CrK
3.34
31.1
48.0
97.6
1.74
0.187
0.121
0.060
6.44
60.6
93.3
189
1.48
0.157
0.102
0.050
3.71
34.5
53.1
108
2.34
0.252
0.164
0.080
8.02
70.9
107
205
1.06
0.120
0.079
0.041
27.3
216
42.7
86.5
0.160
0.020
0.103
0.051
44.7
50.7
78.2
159
0.092
0.081
0.053
0.026
24.1
204
300
548
0.132
0.016
0.011 0.0058
112
216
311
540
0.022
0.011 0.0078 0.0089
5.16
48.6
74.8
152
0.826
0.088
0.057
0.028
38.5
308
52.8
108
0.038 0.0048
0.028
0.014
37.9
278
110
106
0.038 0.0052
0.013
0.014
50.9
52.9
81.6
166
0.025
0.024
0.016 0.0078
120
232
334
579 0.0085 0.0044 0.0030 0.0018
0.59
4.0
6.1
12.5
21.0
3.09
2.02
0.989
6.73
62.0
94.2
186.2
1.21
0.132
0.086
0.044
6.44
60.6
93.3
189
0.738
0.079
0.051
0.025
3.71
34.5
53.1
108
1.17
0.126
0.082
0.040
2
12.
Accessories
Table 12.1
Name
Accessories
Illustration
Center slit
Si powder reference sample
Si wafer reference sample
Optics removing tool
71
Cross beam optics

This system permits easy switching between a divergence beam used for measurements with
para-focusing optics and a parallel beam produced with a multilayer mirror. To switch, simply
replace the selection slits. As shown in the diagram, selection slit (BB) uses x-rays passing
through optical path A, while selection slit (PB) uses x-rays passing through optical path B. In
SmartLab, the multilayer mirror is designed so that optical path A and optical path B intersect
at the center (goniometer center) of the sample at a distance of 300 mm from the x-ray focal
point. There is no need to remove the multilayer mirror when switching from parallel beam
optics to para-focusing optics. Simply change the selection slits and perform 2-theta axis
adjustment one time.
(BB)
Selection
slit (BB)
X source
X-Ray
(filament)
Sample
Optical
pathA
A (divergence beam)
(PB)
Selection
slit (PB)
X
X-Ray
source
(filament)
Sample
Optical
path B (parallel beam)
B
Fig.
Switching between para-focusing optics and parallel beam optics by changing

selection slits
13.
Examples of sample mounting

Introduced below are some typical sample mounting methods.
For more information, refer to the manual provided with the control software.
13.1
Wafer-shaped samples
Use a 4-inch wafer sample plate, 6-inch wafer sample plate, or 8-inch wafer sample plate to measure
wafer-shaped samples.
Fig. 13.1
Tip:
Wafer-shaped sample
When placing or removing the sample, we recommend removing the sample

plate and sample spacer from the instrument. When removing the sample plate
and sample spacer, we recommend setting the chi axis to 0 and positioning the
sample horizontally.
Place the sample at the center of the sample plate. Use the magnets provided to hold the sample in
place. The magnets can be used with samples that are up to 3 mm thick. For information on
measuring samples thicker than 3 mm, refer to 13.2 Bulk samples.
CAUTION: Placing a sample larger than the sample plate may result in
damage to the sample during measurement.
CAUTION: Be careful when placing an 8-inch wafer on the 8-inch wafer

sample plate; the space available for the magnets securing
the sample in place is small. For measurements of 8-inch
wafers, increasing the tilt axis (chi axis) can cause the wafer
to bend under its own weight.
73
13.
Examples of sample mounting
13.2
Bulk samples
Use a 4-inchi wafer sample plate, 6-inch wafer sample plate, or 8-inch wafer sample plate to
measure bulk samples. Select the appropriate sample spacer and sample plate based on sample
thickness. For detailed information, refer to 10.1 Wafer sample plates and sample spacers.
Place the sample so that the sample surface to be measured is parallel to the sample plate. A piece of
clay may be used to secure the sample in place. If the bulk sample is small enough to pass through
the window on the provided aluminum sample holder, you can secure the sample in the aluminum
sample holder and use the height reference sample plate.
Fig. 13.2
13.3
Bulk sample on height reference sample plate
Powder samples
Place powder samples in the indentation on the glass sample holder or aluminum sample holder,
then insert into the height reference sample plate.
Fig. 13.3
13.4
Powder sample
Sample for SAXS measurement (transmission measurement)

For transmission SAXS measurements, clamp a fibrous or film sample to a sample holder and secure
it in place, then insert the holder into a sample plate.
74
14.1
14.
Launching the software
Measurements
This section introduces basic operating procedures for typical measurements. For detailed information,
refer to the SmartLab Guidance Reference Manuals, Parts Manuals, and Package Measurement
Manuals.
14.1
Launching the software

(1) Make sure the OPERATE lamp on the main panel is green.
(2) Launch SmartLab Guidance. Select Package Measurement from the Task menu.
(3) Click Startup to generate x-rays.
14.2
Setting the hardware configuration

(1) Click Hardware Configuration in the Options menu to open the Hardware Configuration
dialog box.
Fig. 14.1
Hardware Configuration dialog box
75
14.
Measurements
(2) Click Goniometer to open the Goniometer dialog box.
Fig. 14.2
Goniometer dialog box
(3) Set the position of each optical device. To change the optical devices of the receiving optics,
inspect the installation positions of the standard receiving slit box # 1, standard receiving slit
box # 2, and scintillation counter and enter the correct corresponding values.
14.3
Selecting a measurement package

(1) Select Package Measurement from the Task menu.
(2) Registered Package measurements are displayed in tree view. Select the Package Measurement
that matches the purpose of the measurement.
Fig. 14.3
Selecting the package
For information on measurement procedures for specific Package Measurements, refer to the
SmartLab Guidance Package Measurement Manual (ME13406A).
76
15.1
15.
Optics maintenance
Periodic Maintenance
Perform the following maintenance tasks at regular intervals to maintain the performance of the
instrument.
15.1
Optics maintenance
Multilayer mirror
You must perform re-adjustments following maintenance of the x-ray

generator.
Attenuator correction
You must perform re-adjustments when changing the wavelength or

following maintenance of the x-ray generator.
HV/PHA adjustment
You must perform re-adjustments when changing the wavelength to be

measured.
Dead-time correction
You must perform dead-time correction measurements after HV/PHA

adjustments.
The characteristics of the detector will change over time. Replacement of the detector is required
when it reaches the end of its service life. However, you can minimize performance degradation by
making the appropriate adjustments.
We recommend performing HV/PHA adjustments and dead-time correction measurement at periodic
intervals.
To make these adjustments automatically, select Package Measurement from the Task menu, then
select Maintenance Package measurement under Utility. For detailed information on measurement
procedures, refer to the Maintenance Package measurement section of the SmartLab Guidance
Maintenance Package Measurement Manual (ME13405A).
Fig. 15.1
Selecting Maintenance Package measurement
77
15.
Periodic Maintenance
15.2
Cooling water
Check the amount of cooling water when using the water circulation pump. If the water level is low,
add water. Periodic changes of cooling water are also recommended.
15.3
Cooling water filter

This filter removes impurities from the cooling water. If the filter becomes clogged with impurities,
the water pressure may not rise appropriately. We recommend changing the filter at periodic
intervals.
Sections 15.4 15.7 are maintenance required only for a 9 kW rotating anode x-ray generator.
15.4
Target
The target metal rotates at high speed to boost x-ray output. Pay close attention and note any
abnormal noise or vibrations.
When contaminant (tungsten from the filament) from the electron gun (filament) adheres to the
target metal surface, you may observe characteristic x-rays from the contamination, in addition to
characteristic x-rays from the target metal. If this happens, maintenance is required. Please contact
our service personnel.
15.5
Filament
As electrons are discharged, the filament will become thinner, eventually breaking the required
circuit. Upon breaking, the filament will release a sudden burst of electrons that can damage the
target surface. To avoid this, we recommend periodically changing the filament.
15.6
Ion gauge (vacuum gauge)

Since the filament in the ion gauge may come loose after many hours of use, we recommend
changing the filament in the ion gauge at periodic intervals.
15.7
Rotary pump
Check the oil level in the vacuum pump. If the oil level is low, add oil. We also recommend periodic
oil changes.
78
16.
Troubleshooting
Problem
The LINE lamp fails to go on.
Remedy
The instrument may not be receiving electric power. Check the main
circuit breaker located on the rear panel of the instrument. Also check
the connections for the power cable and circuit breaker on the supply
side.
The OPERATE lamp does not The controller may be in the process of starting up. Wait several
change color to green (remains minutes.
red).
If the lamp fails to turn green after several minutes, the controller may
be malfunctioning. Press the OFF button on the main panel to shut
down the instrument, then press the ON button to restart the
instrument.
An
error
occurs
during
SmartLab Guidance startup.
The
instrument
startup
procedure fails to complete
properly.
There may be a problem in the connection between the instrument and

the controller. Confirm that the OPERATE lamp on the main panel is
green. Confirm the connection status of the RS232C connectors.
After checking these items, shut down SmartLab Guidance, then
restart. Restart SmartLab Guidance after the instrument is restarted.
The instrument stops abruptly Make sure the OPERATE lamp on the main panel is red. The
during measurement or other instrument may have stopped due to excessive force applied to the
operation.
theta_s or theta_d arm. Press the OFF button on the main panel to stop
the instrument. Check the arms to see if any item obstructs their
operation, then restart the instrument.
The x-ray generator stops during Click XG Control in the Control menu to open the XG Control
measurement
or
other dialog box. Click Display in the Alarm section to open the Alarm
operations.
dialog box. Check for x-ray generator alarms.
A description of each alarm is displayed in the XG status description
section when the LED in the dialog box is clicked.
* If a problem other than those described above occurs or if the problem cannot be corrected by taking the
countermeasure described, please contact our service personnel.
79
Appendix
Using the OPERATE lamp
Appendix
Using the OPERATE lamp
The OPERATE lamp indicates the status of the SmartLab controller. The lamp is usually green, but
will change to red and begin flashing at set intervals in the event of an abnormality. To reset the
generated alarm, you must restart the instrument. After shutting down the control software (SmartLab
Guidance), turn off power to the instrument, then press the ON button to restart the instrument.
If an alarm is generated, stop, then restart the instrument. If the OPERATE lamp lights up in green in
10 to 20 seconds after the restart, the instrument may be used as usual. If the OPERATE lamp does not
turn green, flashing red instead after startup, or if the lamp turns green but changes to a flashing red
immediately during use, please contact our service personnel. Before contacting our service personnel,
please refer to Table 2 to identify the alarm being generated.
Table 1
Condition
Immediately
after Power
ON
Color
Continuously
On / flashing
Green
Flashing
250 ms
Green
Accessible
from PC
Green
100 ms
Flashing
100 ms
Continuously
On
Table 2
Controller
startup
failure
Controller
hung-up
Pattern
250 ms
10 seconds
after Power
ON
Cause of
alarm
Instrument startup
Color
Alarm generation
Continuously
On / flashing
Pattern
500 ms
Red
100 ms
Flashing
100 ms
500 ms
Red
500 ms
100 ms
Flashing
100 ms
500 ms
500 ms
Servo alarm
Red
Flashing
500 ms
Servo
overload
2000 ms
Red
Flashing
2000 ms
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Ver. 1.3
LINE OF BUSINESS
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Tokyo Branch
4-14-4, Sendagaya, Shibuya-ku, Tokyo 151-0051, Japan

Phone: 81-3-3479-0618 Fax: 81-3-3479-6112 e-mail: rinttyo@rigaku.co.jp
Rigaku Corporation
Rigaku Industrial Corporation
Rigaku Americas Corporation
Head Office
3-9-12, Matsubara-cho, Akishima-shi,
Tokyo 196-8666, Japan
Phone: 81-42-545-8189 Fax: 81-42-544-9223
14-8, Akaoji-cho, Takatsuki-shi,

Osaka 569-1146, Japan
Phone: 81-72-693-7990 Fax: 81-72-693-6746
9009 New Trails Drive

The Woodlands, TX 77381-5209, USA
Phone: 281-362-2300 Fax: 281-364-3628
e-mail:info@rigaku.com
http://www.rigaku.com/
06.02

Cat. No. 2080A102/B101/M101/M102 Smartlab Horizontal Sample Mount X-Ray Diffractometer For Thin Film Analysis Instruction Manual

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Manual No. ME11550A02

Thank you for your purchase of Rigakus product.

Safety Precautions in Handling X-ray Equipment

2. Overall System Safety Precautions

2.1 Parts Removal Precautions

All component parts function not only to maintain the product

3. Precautions to Be Observed to Avoid X-ray Exposure

3.2 Notes on X-ray Shutter Safety Release Operation

3.3 Notes on X-ray Shutter Use

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

3.4 Notes on Radiation Enclosure Use

Rigakus radiation enclosure is designed to eliminate the

4. Notes on Hazardous Substances

5. Notes on High Voltage

6. Notes on High and Low Temperatures

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

6.2 Replacement Precautions

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

8. Precautions to Be Observed during the Use of a Hazardous Gas Atmosphere

X-ray Apparatus Handling Precautions

Radiation Protection Mechanisms and Functions

Before Using the Product

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

Trademarks and registered trademarks

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

Horizontal sample mount high-accuracy theta-theta goniometer ..................................................... 3

Attachment base (open Eurlerian cradle) and attachments ............................................................... 3

X-ray generator ................................................................................................................................. 3

Cross beam optics (CBO) ................................................................................................................. 3

Crystal alignment mechanism (monochromators and analyzers) ..................................................... 4

Receiving analyzer system................................................................................................................ 4

Incident optics system....................................................................................................................... 4

Receiving optics system.................................................................................................................... 5

Optics switching system ................................................................................................................... 5

2.10 Optical device detection..................................................................................................................... 5

Control software ............................................................................................................................. 6

Two-slit SAXS optics ..................................................................................................................... 6

In-plane optics for detailed analysis of thin film structure ............................................................. 6

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

X-ray tube ....................................................................................................................................... 11

Theta_s arm .................................................................................................................................... 12

Theta_d arm .................................................................................................................................... 13

Detector mounting bracket.............................................................................................................. 14

Attachment base and attachments................................................................................................... 14

Control software ............................................................................................................................. 15

Data processing software ................................................................................................................ 15

Data display software...................................................................................................................... 15

Analysis software (options) ............................................................................................................ 15

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

Turning on the instrument............................................................................................................... 17

Starting SmartLab Guidance (control software) ............................................................................. 17

Starting the x-ray generator ............................................................................................................ 18

Stopping the x-ray generator........................................................................................................... 19

Turning off the instrument .............................................................................................................. 20

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

Opening the door ............................................................................................................................ 21

Closing the door.............................................................................................................................. 22

Emergency stop switch (EMO)....................................................................................................... 22

CBO unit (for Cu target)................................................................................................................. 23

Incident optics unit (standard incident optics unit)......................................................................... 26

Incident parallel slit adaptor (IPS adaptor) .......................................................................... 26

2-Bounce monochromator (option)...................................................................................... 29