XRD 6000 Brochure Eng
XRD 6000 Brochure Eng
X-ray Diffractometer
XRD-6100
Ease of use and abundant functions herald a new era of analysis
X-Ray Diffractometer
XRD-6100
In addition to its basic ease of use and abundant functions, the XRD-6100 boasts an integrated design featuring a vertical goniometer and
data processing software supporting the Windows 7 user interface.
The XRD-6100 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. Of course, crystalline structural
analyis, including precise lattice constant determination, is also supported.
A g en er a l-p u r p o s e X -r a y d if f r a ct om et er
to ad d re s s y o u r v a r io u s a n a ly t ic al
n eed s X R D -6 1 0 0
Fea tu res
Hi g h -p rec i s i o n built -in v e r t ica l goniom e t e r
Enables measurements of a variety of samples including hard-to-secure samples like powders
and thin films as well as highly soluble samples.
Safe, c o mp ac t body
The main body has been massively slimmed and as the rear is a sheer flat surface with no
superfluous protrusions, the device can placed up against walls, which means it does not take
up room when installed on site or in the lab. The unit has also been specifically designed to
promote ease of handling in sample loading and positioning and, together with the door
lock mechanism engaged during X-raying, provides a safe operating environment.
Applications of X-ray Diffractometry
F e rro u s me ta ls
Steel
Qualitative analysis of steel sheet, measurement of
residual austenite and residual stress, analysis of friction and wear test samples,
measurement of iron oxide films and nitride layers, evaluation of plating and
texture.
Cast iron
Qualitative analysis of precipitates and additives in cast iron.
Surface-treated steel
Evaluation of characteristics of surface-treated areas, quality control, residual
stress measurement.
N o n - ferro u s me ta ls
Copper and zinc
Qualitative analysis of alloys, orientation measurements
of foil samples, evaluation of texture, qualitative analysis of plated areas.
Aluminum
Qualitative analysis of aluminum and aluminum alloys, oxides and nitrides,
evaluation of texture in rolled material.
Other metals
Qualitative analysis of metal alloys, oxides and nitrides, evaluation of
characteristics of surface-treated areas, residual stress measurement.
C e ra mics
Porcelain and ceramics
Qualitative analysis of raw materials, final product
evaluation, analysis of crystal structures during heating (crystal system, crystallite
size, lattice constant).
Cement and glass
Qualitative and quantitative analysis of clinker and cement (free lime, etc.),
qualitative analysis of raw materials. Qualitative analysis and orientation
measurements of thin film layers formed at the glass surface.
4
Pharmac eutic als and medic al tre at m en t
Pharmaceuticals
Qualitative analysis of raw materials, identification of
impurities. Crystal polymorphism analysis and degree of crystallinity
measurements, quality control during pharmaceutical manufacture using
crystallite size measurement. Final product quality check and crystal
polymorphism analysis related to patents.
Dental materials
Qualitative analysis of dental materials such as apatite.
XRD-6100
X-ray Diffractometer 5
Polycapillary optical system
This example shows measurements of the raw drug acetaminophen and its
16000.00
tablets during the process of manufacturing. Tablets can be directly analyzed
Intensity (CPS) C
ntsPerSecond
4000.00 Tablet 1
0.00
Ingredient
10.00 20.00 30.00 40.00
2 θ- θ
6
Qualitative and quantitative analysis of asbestos
and free silicic acids
The concentration of asbestos in construction materials is
measured using phase contrast dispersion staining microscopes
and X-ray diffractometers.
After pulverizing the sample acquired from the site in a pulverizer,
a phase contrast dispersion staining microscope and X-ray
diffractometer are used respectively to qualitatively analyze the
sample. If the sample is determined to contain asbestos at this
stage, then it is quantitatively analyzed using the X-ray
diffractometer. In actual practice, asbestos analysis (JIS A 1481)
requires sensitivity sufficient to determine 0.1 % content by
weight in 100 mg of acquired sample. To increase sensitivity so
that such trace asbestos levels can be detected, formic acid is used
to dissolve matrix components in the pulverized sample. Then the
residue after formic acid treatment is recovered in a fluorocarbon The major types of asbestos are serpentine asbestos (chrysotile) and amphibole
asbestos (amosite and crocidolite). The characteristic peaks of these types can
polymer binder filter using a suction filtration system for use in
be quantitatively analyzed by X-ray diffractometry.
quantitative analysis. In this case, the quantitative analysis is
performed using an X-ray diffractometer, where the absorption of
diffracted X-rays must be corrected to compensate for the
asbestos itself and the undissolved matrix components. This
correction process (base standard absorption correction method)
involves first measuring the metal plate (base plate) for a blank
filter, placing the filter with the formic acid-treated asbestos in the
diffractometer, and measuring the asbestos together with the
metal base plate to determine a correction factor from the
diffraction intensity ratio of the metal plate. Then that correction
factor is used to determine the corrected asbestos diffraction
intensity. Note that this method was originally developed for
measuring the free silicic acid content in mineral particulates
during work environment measurements.
Qualitative analysis results for asbestos
The XRD-6100 X-ray diffractometer environmental measurement
package includes a user database for environmental samples,
which is effective for increasing the accuracy of qualitative
analysis, a filter holder and rotational sample stage for use in the
base standard absorption correction method, and environmental
quantitation software for performing quantitative calculations that
correct for absorption. This environmental quantitation software
incorporates Shimadzu's proprietary measurement expertise
cultivated from many years in this field, which is especially
valuable when quantitating particularly trace levels of asbestos.
In addition, this XRD-6100 X-ray diffractometer environmental
measurement package is compliant with methods specified in the
Notification No. 0828001 by the Director of the Chemical Hazards
Control Division, Industrial Safety and Health Department, Labour
Standards Bureau, Ministry of Health, Labour and Welfare of
Screenshot of environmental quantitation software
Japan, such as for analyzing asbestos in natural minerals or
measuring the free silicic acid content in mineral particulates
during work environment measurements.
XRD-6100
X-ray Diffractometer 7
A general-purpose X-ray diffractometer to adress
your various analytical needs
P ri n c ip le o f o p era tio n Cons truc tion
The XRD-6100 analyzes crystalline states under normal
Compact, X-ray-protected housing
atmospheric conditions. This method is non-destructive. X-rays
The compact construction (W900xD700xH1600mm) minimizes
focused on a sample fixed on the axis of the spectrometer
installation space requirements.
(goniometer) are diffracted by the sample. The changes in the
The front door is mounted on guide rollers, enabling light and
diffracted X-ray intensities are measured, recorded and plotted
smooth opening of the door to facilitate easy
against the rotation angles of the sample. The result is referred
installation/exchange of samples and attachments. A magnet
to as the X-ray diffraction pattern of the sample. Computer
latch assures the door closers: and to further ensure safety, a
analysis of the peak positions and intensities associated with
door interlock mechanism is automatically activated whenever
this pattern enables qualitative analysis, lattice constant
X-rays are generated.
determination and/or stress determination. 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
High-precision, vertical goniometer
diameters and degree of crystallization, and are useful in
High-speed rate (1000°/min) and high-precision angle
conducting precise X-ray structural analysis.
reproducibility (±0.001°) provide fast measurement and highly
reliable data. The vertical goniometer unit allows analysis of
samples in various states, substantially widening the application
Incident X-rays(λÅ) Diffracted X-rays
range. The drive mechanism features an independent dual axis
θ -2θ linkage drive, and independent 2θ and θ axis drives,
freely selectable for efficient thin film and various other types
of analysis.
θ θ
θθ dÅ
dÅ
nλ = 2d · sinθ
Counter monochromator
(option)
8
X-ray tubes Highly stable X-ray generator
The XRD-6100 will accept various types of X-ray tubes, Shimadzu's long experience in producing high-performance
including the normal focus (NF) 2kW type and broad focus (BF) X-ray generators has enables the production of a highly stable
2.7kW type, which are standard accessories, as well as the X-ray generator, with tube voltage and tube current both
optional long fine focus (LFF) 2.2kW type. By attaching the stable to within ±0.01%. This stability is unaffected during
optional counter monochromator, all types of samples, fluctuation of source voltage or ambient temperature, ensuring
including Fe samples, can be analyzed using the standard Cu high reliability of data even during prolonged periods of data
X-ray tube. acquisition.
Detector
Goniometer Monitor
A
B
Angle of B
diffraction A
2θ B
θ
Sample
X-ray tube
XRD-6100
X-ray Diffractometer 9
Providing a Complete Analysis System
Analysis System
10
Automatic Measurement, Easy Operation
[ Goniometer optical system adjustment and saving of adjustment data are both fully automated.]
Measurement Display
Sample measurement conditions can be set by
easily.
The scheduling and the progress condition of the
measurement can be confirmed in one view by
the analysis spooler.
Measurement Screen
XRD-6100
X-ray Diffractometer 11
Pleasant Data Processing Environment
Graphic Display
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 accomplished using combined 2-dimensional or
3-dimensional 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.
Each type of data can be output to a color printer, so
differences between samples can be recognized at a glance.
Adding/Subtraction Operations
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 below.
12
File Maintenance ~Data Format Conversion~
Conversion between profile data and text data, conversion
from Shimadzu X-ray Diffractometer
XD-D1(previous model) acquisition data to XRD-6100 format
data, and re-analysis are all possible. File format conversion is
conducted using the window displayed at right.
Optical Adjustments
The XRD-6100 system makes fully automatic optical the θ and 2θ axes, the x-ray detector high voltage settings, the
adjustments to the goniometer from the computer screen, PHA baseline and window width settings, it also automatically
even for optional attachments. In addition to completely saves the settings information. This feature can be utilized for
automatically adjusting all settings, such as the zero angle for routine maintenance.
XRD-6100
X-ray Diffractometer 13
Enhanced Auto Search System
[ Auto Search, General Quantitation Software Provided as Standard ]
14
Polished Quantitation Software
Quantitative Analysis
The internal standard method and 2 intensity methods are
available to satisfy most of the application needs.
Further, up to 5 peaks may the specified for quantitation and up
to 10 sets of data may be calculated simultaneously.
Note: Residual austenite quantitation and environmental quantitation software packages are optional.
XRD-6100
X-ray Diffractometer 15
Accessories
In addition to the functions of PDF2, database PDF4 features data searching software (DDVIEW+), the display of 2D, 3D structural
charts, various lattice parameters, simulation wave form by the calculation, and the import of the measurement data.
There are two databases of PDF4+ (for general) and PDF4/Organics (for organics).
ICDD PDF4+ P/N for Educational Institutions P/N for Other Uses ICDD PDF4 / Organics P/N for Educational Institutions P/N for Other Uses
Single license Single license
(New, 1 year license) 239-50015-02 239-50015-01 (New, 1 year license) 239-50015-22 239-50015-21
16
Q u a l itativ e a n aly sis
Rotational Sample Stage RS-1001
The RS-1001 performs in-plane rotation of the sample in
combination with oscillation around the goniometer sample
axis (θ) to minimize the scatter in diffraction pattern intensities
attributable to the sample crystalline orientation, and thereby
enhance the precision in most types of quantitative analysis.
Main specifications
Rotation ß axis (sample in-plane)
Rotation speed 1 to 60rpm
Minimum step width 0.1 degree
Operation modes Constant speed rotation,oscillation sample
in-plane rotation scan (continuous, step)
Measuring angle range 2θ 5° to 163°
Main specifications
Measuring angle range 2θ 5° to 163°
XRD-6100
X-ray Diffractometer 17
Accessories
Main specifications
Sample position 5
Sample size Powder:25mm ø
Filter: 25mm ø (option)
Rotation speed 1 to 60rpm
Measuring angle range 2θ5° to 163°
Main specifications
Rotation ß axis (sample in-plane)
Rotation speed 1 to 60rpm
Minimum incidence angle 0.1degree
Sample suction pump AC100V, 10W (1 pump)
Operation modes Constant speed rotation, oscillation, sample
in-plane rotation scan, (continuous, step)
18
Fiber Sample Attachment
Used in combination with the Rotational Sample Stage
(RS-1001), this system measures the degree of orientation for Fiber sample
fibers. The acquired data is then processed using the provided attachment
fiber sample attachment software to calculate the degree of
orientation. Rotational
sample stage
Part Description P/N
Fiber sample attachment (with S/W) 215-22624
Mode:
The emission slit is adjusted so that all sample surfaces are
irradiated with the X-ray of the same width. The detector
slits (SS and RS) are also adjusted in accordance with the
irradiation width.
Fixed Irradiation Width Mode: Degree of Orientation Evaluation Screen
The DS, SS and RS slit widths are fixed at the set values.
XRD-6100
X-ray Diffractometer 19
Accessories
Key Specifications
Pinhole Emitter Slit 0.1, 0.2, 0.3, 0.5, 1, or 2 mm diameters
XYZ Movement ±7.5 mm
Sample Surface Observation CCD camera image viewed on computer
Method screen
Main specifications
Inclined axis α axis
Inclined angle range 0 to 50 degrees
Operation modes Oscillating, fixed
20
PCL-1001 Polycapillary Unit
The polycapillary unit is a new optical X-ray element that splits
a single X-ray beam emitted from a point’s light source into
multiple X-ray beams using three-dimensionally arranged
capillary optics. This creates a powerful parallel beam output
that covers a large area.
1) Compared to conventional methods, this unit uses the X-ray
more effectively and increases the intensity of the diffracted
X-ray, allowing more sensitive analysis.
2) With conventional methods, variations in sample surface
height are directly translated into variations in X-ray diffraction
angles. This polycapillary unit uses parallel beams, so it is not
affected by variations in sample surfaces.
Main Specifications
Thermocouple Pt-Pt/Rh
Measurement temperature 1500°C max. in vacuum, air
1200°C max. using inert gas (N2)
Control functions PID value setting, fixed temperature control
(temperature increase, decrease, hold, stop)
Power supply Single phase 200/220V±10% 10A
HA-1001
Part Description P/N for Other Uses
Sample heating attachment
(for XRD-6100 with temperature controller) 215-23000
XRD-6100
X-ray Diffractometer 21
Accessories
Main Specifications
TTK-450
Thermocouple PT100 resister
Power supply RT to 300°C (in the air,or an inert gas)
Temperature RT to 450°C (in vacuum) TTK-450
22
Q u a l ita tiv e a n aly sis
Residual Austenite Quantitation
(P/ N 2 15 - 00430- 92)
A common method to quantify residual austenite is to apply
the method for samples consisting of 2 components such as
tempered copper α-iron and γ- iron. Special software allows the
determination without the need of standard sample.
The software directly uses the intensity ratio of the measured
X-ray peaks of the α-iron and γ- iron components to
theoretically perform the calculation. The five-peak average
method is used to make the determination, so scattering due
to the matrix effect is reduced, enhancing the reliability of the
results. Using the rotational sample stage (P/N 215-21766) for
measurement further helps to overcome data scattering.
P e a k P ro ce ssin g
Overlapping Peak Separation Software
(P/ N 2 15 - 00423- 92)
Using the Gauss and Lorentz models, overlapping peaks are
separated one by one, with information including position,
intensity, width at half height and integrated intensity
calculated for each diffraction peak.
These are then utilized to conduct quantitative analysis and
crystalline structure analysis.
XRD-6100
X-ray Diffractometer 23
Optional Software
S ta te A n aly sis
Crystallite Size & Lattice Strain Software
(P / N 21 5- 00426- 92)
Samples normally consist of crystallites ranging in size from
several μm to tens of μm. However, in the case of catalyst
crystallites, which may measure several hundred Å, X-ray
diffraction is insufficient, resulting in diffraction peak
spreading. This software quantitatively determines that spread,
and applies the Scherrer's equation to calculate the crystallite
size. When there is involvement of lattice strain, the diffraction
spread is determined for a number of diffraction peaks, and
from the resultant line slope and intercepts, the size of each of
the crystallites and the lattice strain are calculated. (Hall's
Method)
Hall's Equation Calculation Result Screen
24
Other Accessories
Sample Holders
The following sample holders, inclusinf the alminum sample
holder, which is supplied as standard with the diffractometer,
are available for different applications.
With its built-in cooler, the Cooling Water Circulator cools the
X-ray tube and X-ray generator by circulating cooled, pure or
clean water. The unit is recommended when no tap water is
available or the available water is of poor quality.
Main specifications
Power supply Three phase 200V ±10% 10A (RKE1500B-V-G2-SP)
Ambient temperature 5 to 40°C
Cooling capacity 5.3kw/h (50/60Hz) (RKE1500B-V-G2-SP) RKE1500B-V-G2-SP
XRD-6100
X-ray Diffractometer 25
Accessories
Brickmaking, ceramics
Construction, engineering
Environment (Asbestos)
Analysis Objective Par t De scrip tio n Part Number
Environmental quantitative
*Environmental Quantitative Analysis Stage RS-2001 Note1 P/N 215-21767-01
6 (Filter holders Zn, with S/W)
analysis system
Filter holder Al (ø 25mm) P/N 215-23765-92
8 Precise lattice constant determination Precise lattice constant determination S/W P/N 215-00424-92
10 Crystallite size / lattice stress Crystallite Size / Lattice Stress S/W P/N 215-00426-92
17 Micro Measurement with CCD camera Micro-Measuring Attachment MDA-1201 P/N 215-23180-94
19 Strong pallarel beam X-ray source poly-capirally unit PCL-1002 P/N 215-24375-91
1) Can be used together with general purpose rotational sample stage
Note1: Please arrange optional additional ASSY(P/N215-23705) with optional driver ASSY(P/N215-21764) at the same time when you arrange the accessories of the asterisk.
Moreover, even when two or more accessories are arranged, the option driver ASSY and optional additional ASSY can use it combinedly with one unit.
Note2: When I arrange an auto 5 position sample changer, please arrange two optional additional ASSY.
26
Specifications
XR D - 61 0 0
XRD-6100
Item 2kW Type 3kW Type High-resolution type
Type Cu, NF type Cu, BF type Cu, LFF type
X-ray tube Focus 1.0 x 10mm 2.0 x 12mm 0.4 x 12mm
Max. output 2kW 2.7kW 2.2kW
Max. output 3kW
Output stability ±0.01% (for 10% power fluctuations)
Max. tube voltage 60kV
Max. tube current 80mA
X-ray generator Voltage step width 1kV
Current step width 1mA
Overload limit setting Setting changeable with tube type
X-ray tube protection Against undervoltage, overload, overvoltage, overcurrent and/or failure of water supply
Safety mechanisms Door interlock mechanism (X-ray can be generated only after the door is closed) Emergency stop
Type Vertical type
Scanning radius 185mm
Min. step angle 0.002° (2θ) 0.001° (θ)
Angle reproducibility ±0.001° (2θ)
Scanning angle range -6° to 163° (2θ), -180° to 180°(θ)
Scanning system θ/2θ linkage mode, θ, 2θ independent mode
Goniometer Operation mode
Continuous scan measurement, step scan measurement, calibration, positioning,
θ axis oscillation (when using 2θ continuous scan or step scan)
Max. speed 1000°/minute (2θ)
Scanning speed 0.1° to 50°/min (2θ), 0.05° to 25°/min (θ)
Divergence slit (DS) 0.5°, 1°, 2°, 0.05mm
Scattering (SS) 0.5°, 1°, 2°
Receiving slit (RS) 0.15mm, 0.3mm
Dimensions W900 x D700 x H1600
Casing Leakage X-rays Less than 2.5μSv/h (at maxium output)
X- ra y Tu b e s an d X -ray Filters
Focus Type Type NF Type BF Type LFF
Focus Size 1 x 10mm 2 x 12mm 0.4 x 12mm
X-Ray Filter
Tube voltage, current 60kV, 50mA 60kV, 60mA 60kV, 55mA
Target X-ray Tube Maximum Load & P/N
Cu 2.0kW (239-24014-01)*2 2.7kW (210-24016-21) 2.2kW (210-24100-11) Part Description P/N
Co 1.8kW (062-40003-04) 2.7kW (210-24016-24) 1.8kW (210-24100-14) Ni filter (for Cu) (215-22500-02)
Fe 1.5kW (062-40003-05) 2.2kW (210-24016-25) 1.0kW (210-24100-15) Fe filter (for Co) (215-22500-03)
Cr 2.0kW (062-40003-06) 2.7kW (210-24016-26) 1.9kW (210-24100-16) V filter (for Cr) (215-22500-05)
*2 When using it as a point focus, combine a X-ray tube and a point focus head of following P/N.
1) X-ray tube (Cu target, 2.0kW, NF) P/N 210-24016-11
2) Point focus head P/N 239-16047
*When using the polycapillary system, use LFF type.
D e te cto rs
OneSight Wide-Range High-Speed Detector Scintillation Detector
(FD-1001 1D High-Speed Detector P/N 215-24320-91) SC-1003 P/N 215-24385-92
0-159˚ : Radius of Goniometer 275 mm Scintillator Na I
Scan range 0-150˚ : Radius of Goniometer 200 mm Scaler Preset time: 0.1 to 1000s; digits: 7
0-148˚ : Radius of Goniometer 185 mm 500 to 1200 V high-voltage power supply,
Operation mode Step-scan mode, One-shot mode HV/PHA
baseline and window auto-controlled
Sensor Reverse biased pn-junction array
Detection principle Single photon counting
Weight 280 g
Active area 64 × 8 mm
Number of channels 1280
Width of one channel 50 μm
D a ta Pro ce ssin g U n it
C o mp u ter IBM PC/AT compatible
OS Windows 7
C o n tro lled elements Goniometer, X-ray generation, tube voltage, tube current, detector high voltage, PHA, scaler
B asic d ata proc es s ing Smoothing, BG elimination, Kα1-Kα2 separation, peak searching, peak width at half height, integrated intensity,
systematic error correction, internal/external standard correction, operations between data, graphic display
Qu alita tive analys is Database (library) creation, automatic library search (ICDD PDF2/PDF4 options) calibration curve generation, quantitation calculation
Qu an tit ative analys is Calibration curve generation, quantitative analysis
*Windows and Windows 7 are registered trademarks of Microsoft Corporation (USA) in the United States and other countries.
*Additionally noted company names and product names are the trademarks or registered trademarks of the respective companies.
*The notationsTM and ® are not used in this document.
XRD-6100
X-ray Diffractometer 27
XRD-6100
Installation Requirements
3500
200 to
600
3000
900 650
Unit: mm
Entrance width at least 800
Company names, product/service names and logos used in this publication are trademarks and trade names of Shimadzu Corporation or its
affiliates, whether or not they are used with trademark symbol “TM” or “®”.
Third-party trademarks and trade names may be used in this publication to refer to either the entities or their products/services. Shimadzu
disclaims any proprietary interest in trademarks and trade names other than its own.