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XRD-6000 Shimadzu X-ray Diffractometer Manual

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The XRD-6000, an X-ray diffractometer analyze crystalline states under normal atmospheric conditions. This method is non destructive. X-rays focused on a sample fixed on the axis of the spectrometer (goniometer) are diffracted by the sample. The changes in the diffracted X-ray intensities are measured, recorded and plotted against the rotation angles of the sample. The result is referred to as the X-ray diffraction pattern of the sample. Computer analysis of the peak positions and intensities associated with this pattern enables qualitative analysis, lattice constant determination and/or stress determination of the sample. Qualitative analysis may be conducted on the basis of peak height or peak area. The peak angles and profiles may be used to determine particle diameters and degree of crystallization, and are useful in conducting precise X-ray structural analysis.
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C141-E004E
X R D - 6 0 0 0
S h i m a d z u
X - r a y D i ff r a c t o m e t e r

A g e n e r a l p u r p o s e
X - r a y d i f f r a c t o m e t e r t o f u l f i l l y o u r v a r y i n g
a n a l y t i c a l n e e d s
X R D - 6 0 0 0

X R D - 6 0 0 0
S h i m a d z u X - r a y D i ff r a c t o m e t e r
E a s e o f u s e a n d a b u n d a n t f u n c t i o n s
h e r a l d a n e w e r a o f a n a l y s i s

The Windows XP-supported application software usher this compact, multi-functional,
general purpose X-ray Diffractometer into the networking era of analysis.
With its basic ease of use and abundant functions, the XRD-6000 boasts an integrated design
featuring a vertical goniometer and data processing software supporting the Windows XP user
interface.
The XRD-6000 offers solutions encompassing wide-ranging analysis requirements, from routine
qualitative and quantitative analysis to state change analysis, including stress analysis, residual
austenite quantitation, crystallite size / lattice strain, crystallinity calculation, materials analysis via
overlaid X-ray diffraction patterns, enhanced material evaluation and sample heating analysis.
And, of course, crystalline structural analysis is also supported, including precise lattice constant
determination and crystal system determination.
F e a t u r e s
H i g h - p r e c i s i o n b u i l t - i n v e r t i c a l g o n i o m e t e r
Routine performance maintenance for device is
This can measure various samples including hard-to-secure
easy
samples like powders and thin films as well as highly soluble
Adjustments to the optical system are performed by automatic
samples.
setting function. And as the XRD-6000 has a function to
automatically save the system's adjustment parameters,
Wi n d o w s X P e m p l o y e d a s s o f t w a r e p l a t f o r m
system status can be monitored and recorded. Consequently,
The main unit control and data processing software supports
routine performance maintenance can be easily controlled,
the widely used Windows XP user interface. For this reason,
D i s t i n g u i s h e d b o d y t h a t i s s a f e a n d c o m p a c t
data can export to marketed software, network support, and
multi-user accessibility is easily achieved.
The main body has been massively slimmed down (30%
reduction in installation surface area compared to previous
M u l t i - f u n c t i o n a l a u t o - s e a r c h / m a t c h s o f t w a r e
Shimadzu diffractometers), and as the rear is a sheer flat
( q u a l i t a t i v e a n a l y s i s ) e q u i p p e d a s s t a n d a r d
surface with no superfluous protrusions, the device can placed
The XRD-6000 is equipped with auto-search / match software
up against walls, which means it does not take up room when
as standard to aid qualitative analysis - the important analysis
installed on site or in the lab. The unit is also specifically
task of X-ray diffraction. The detailed search parameter
designed to promote ease of handling in sample loading and
settings, second search function, and the comparison display
positioning, and together with the door lock mechanism
of candidate substances on raw data profile make analysis
engaged during X-raying, provides a safe operating
easy to understand for even the beginner, and - what is more -
environment.
a greater success ratio in results can be achieved with the
system. In addition, an easy quantitative calculation function
and a function that incorporates element data from the X-ray
fluorescence spectrometer are also included in the system.
P 04 - XRD-6000 Features and Applications
P 14 - Options
P 23 - Main Specifications
Contents
P 06 - Principle and Construction
P 21 - Other Options
P 24 - Installation Requirements
Analysis and Standard Data
System Configuration
P 08 -
P 22 -
Processing Functions
and Accessories

X R D - 6 0 0 0 F e a t u r e s a n d A p p l i c a t i o n s
A general purpose X-ray diffractometer
P r i n c i p l e o f o p e r a t i o n
The XRD-6000, an X-ray diffractometer analyze crystalline states under normal atmospheric
Incident X-rays(λÅ)
Diffracted X-rays
conditions. This method is non destructive. X-rays focused on a sample fixed on the axis of the
spectrometer (goniometer) are diffracted by the sample. The changes in the diffracted X-ray
intensities are measured, recorded and plotted against the rotation angles of the sample. The
θ
θ
result is referred to as the X-ray diffraction pattern of the sample. Computer analysis of the
θ θ

peak positions and intensities associated with this pattern enables qualitative analysis, lattice
constant determination and/or stress determination of the sample. Qualitative analysis may be

conducted on the basis of peak height or peak area. The peak angles and profiles may be used
to determine particle diameters and degree of crystallization, and are useful in conducting
nλ = 2d • sinθ
precise X-ray structural analysis.
A p p l i c a t i o n s
Steels, non-ferrous metals, machinery, shipbuilding, welding, automobiles, ceramics, cement, glass, catalysts, electrical parts,
electronic materials, magnetic materials, superconductive materials, fibers, paper, pulp, food products, chemicals, agricultural
chemicals, dies, pigments, paints, pharmaceuticals, dental materials, biological matter, petroleum, coal, power generation, natural gas,
mining ore, soil, rocks, clay, minerals, construction, civil engineering, environment, and industrial waste
C o n s t r u c t i o n
C o m p a c t , X - r a y - p r o t e c t e d h o u s i n g
The compact construction (W900xD700xH1600mm) minimizes installation space requirements.
The front door is mounted on guide rollers to enable extremely light-touch and smooth door opening for facilitative
installation/exchange of samples and attachments. A magnet latch assures certain door closing, and to further en-
sure safety, a door interlock mechanism is automatically activated whenever X-rays are generated.
H i g h - p r e c i s i o n , v e r t i c a l g o n i o m e t e r
High-speed rate ( 1000 /min) and high-precision angle reproducibility (
0.001 ) provide fast measurement and
highly reliable data. The vertical goniometer unit allows analysis of samples in various states, substantially widen-
ing the application range. The drive mechanism features an independent dual axis
-2
linkage drive, and inde-
pendent 2
and
axis drives, freely selectable for efficient thin film and various other types of analysis.
Counter monochromator
(option)

Rotational sample stage
(option)

Vertical Goniometer
4

to fulfill your varying analytical needs
C o n s t r u c t i o n
High voltage transformer for high output X-ray tube
The high voltage transformer supports either the 2.2kW high output fine focus X-ray tube or 2.7kW high output broad focus X-ray tube.
X-ray tubes
The XRD-6000 will accept various types of X-ray tubes, including the normal focus (NF) 2kW type and broad focus (BF) 2.7kW type,
which are standard accessories, as well as the optional long fine focus (LFF) 2.2kW type. By attaching the optional counter
monochromator, all types of samples, including Fe samples can be analyzed using the standard Cu X-ray tube.
Highly stable X-ray generator
Shimadzu's long experience in producing high-performance X-ray generators has provided an X-ray generator of high stability, with
tube voltage and tube current both stable to within
0.01%. This stability is unaffected during fluctuation of source voltage or ambient
temperature, ensuring high reliability of data even during prolonged periods of data acquisition.
Detector
Goniometer
Monitor
A
B
B
A
B
Sample
X-ray tube
High voltage
Goniometer control
Standard data
transformer
Detector high
processing system
X-ray control
voltage PHA
XRD-6000 Relational Diagram
5

P r i n c i p l e a n d C o n s t r u c t i o n
Providing a Complete Analysis System
Analysis System
Standard Software
Options
X-ray generator control
X-ray ON/OFF, tube voltage/current setting
Qualitative analysis
Counter monochromator
Optical path adjustment
Goniometer adjustment
ICDD database PDF2, PDF4
Measurement
Single scan, multi-scan
PDF2 search software
File maintenance
ASCII data conversion
Quantitative analysis
ASCII data to XRD-6000 data conversion
Residual austenite quantitation software
XD-D1 data to XRD-6000 data conversion
Rotational sample stage
Basic data processing
Smoothing, background elimination,
Environmental quantitation analysis system
Kα1-Kα2 separation, peak search,
system error correction,
Peak processing
internal/external standard correction,
Overlapping peak separation
operations between data
Crystalline structural analysis
Graphic display
Vertical display, horizontal display
Precise lattice constant determination software
Overlay display (3D)
Rietveld method analysis software
Log display
Qualitative analysis
Auto search
State analysis
User database creation
Crystallite size/lattice strain calculation
Crystallinity calculation
Quantitative analysis
Calibration curve generation
Thin film measurement attachment
Quantitation
Fiber sample attachment
(with orientation evaluation software)
Stress measurement attachment
(with stress analysis software)
Sample heating attachment
Micro-measuring attachment
Auto search results and thin film sample overlay display
6

P r i n c i p l e a n d C o n s t r u c t i o n
Automatic Measurement, Easy Operation
[ Goniometer optical system adjustment and saving of adjustment data are both fully automated.]
M e a s u r e m e n t D i s p l a y
Wiht the XRD-6000, sample measurement condition can be set by easy operation.
The scheduling and the progress condition of the measurement can be confirmed at one view by the analysis spooler.
Multitasking for enhanced analysis efficiency
B a s i c D a t a P r o c e s s i n g
The multitasking capability provided with the Windows XP operating environment allows measurement and data processing to be
conducted simultaneously, enhancing the efficiency of analysis operations.
Basic Data Processing Screen
7

A n a l y s i s a n d S t a n d a r d D a t a P r o c e s s i n g F u n c t i o n s
Pleasant Data Processing Environment
G r a p h i c D i s p l a y
Data can be freely zoomed with a click of the mouse, so profile comparison of thin film data or heating measurement data etc. is easily
accamplished using combined 2-dimensional or 3-dimension-al display. The software also features a variety of other useful graphic
functions, such as intensity Log conversion display and hidden-line processing on the 3-dimensional display, among others. Each type
of data can be output to the color printer, so differences between samples can be recognized at a glance.
3-Dimensional Screen of Thin Film Sample
2-Dimensional Output of Thin Film Sample
A d d i n g / S u b t r a c t i o n o p e r a t i o n s
Data manipulation functions such as deletion of unnecessary peak profiles and addition of re-analyzed data to obtain a summed profile
are some of the invaluable tools available for conducting efficient data analysis. Spectral calculations are conducted in the window
displayed at right.
Spectral Calculation Window
8

F i l e M a i n t e n a n c e ~ D a t a F o r m a t C o n v e r s i o n ~
Conversion between profile data and text data, conversion from
Shimadzu X-ray Diffractometer
XD-D1(previous model) acquisition data to XRD-6000 format
data, and re-analysis are all possible. File format conversion is
conducted using the window displayed at right.
File Conversion Window
O p t i c a l A d j u s t m e n t s
The XRD-6000 system makes fully automatic optical adjustments to the goniometer from the computer screen, even for optional
attachments. In addition to completely automatically adjusting all settings, such as the zero angle for the
and 2
axes, the x-ray
detector high voltage settings, the PHA baseline and window width settings, it also automatically saves the settings information. This
feature can be utilized for routine maintenance.
The PHA (Pulse Height Analysis)
Adjustment Screen
HV (high voltage) adjustment screen
θ-Axis Adjustment Screen
9

A n a l y s i s a n d S t a n d a r d D a t a P r o c e s s i n g F u n c t i o n s
Enhanced Auto Search System
[ Auto Search, General Quantitation Software Provided as Standard ]
I d e n t i f i c a t i o n w o r k c a n b e p e r f o r m e d e f f i c i e n t l y o n s c r e e n .
D e t a i l e d s e a r c h p a r a m e t e r s c a n b e s e t .
To obtain correct results with automatic search/match, search para-
meters that conform to each sample must be set. The XRD-6000 en-
ables the setting of detailed search parameters such as selection of
files to be used in the search and three levels of element data input.
Furthermore, the XRD-6000 comes with a standard function for ele-
ment data, which takes up qualitative results (element analysis) from
X-ray fluorescence spectrometers as files via LAN.
R e p l e t e w i t h s e c o n d s e a r c h f u n c t i o n f o r a u t h o r i t a t i v e
i d e n t i f i c a t i o n o f s m a l l a m o u n t o f c o m p o n e n t s .
Identifying small amount of components with a primary search is diffi-
cult, a second search is needed after the maior components have
been identified. The XRD-6000 comes replete with a second search
function to provide an environment for easy identification of small
Search Parameter Setting Screen
amount of components.
V a r i o u s s e a r c h r e s u l t d a t a c a n b e d i s p l a y e d .
Search results can be stack-displayed with each standard data
display over raw data. Also, for easy comparison, standard substance
names, chemical equations, ore names, Miller indices, and ICDD
numbers can be displayed on each peak. Furthermore, an easy
quantitative calculation function using a corundum ratio for candidate
substances is included in the equipment.
If your system has a PDF2 or PDF4 database, PDF2 or PDF4
detailed data for candidate substances can be displayed on a
separate window.
Search Result Screen
D e d i c a t e d u s e r d a t a b a s e c a n b e c r e a t e d .
The user's very own database file - separate from the sub-file sup-
plied by ICDD (International Center for Diffraction Data) - can be cre-
ated. Selected ICDD standard data and substance data not regis-
tered with ICDD can be input into this file. And data obtained through
measurements by the XRD-6000 can be registered as they are in the
database file, which means that the user's basic samples can be reg-
istered, and comparisons made with those substances to provide an
extra dimension to quality control.
User Database Creation Screen
10

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