Difray-401k
Desktop X-ray diffractometer
- Bragg-Brentano and Debye-Scherrer focusing geometries
- High-speed position-sensitive detector
- Autonomous water cooling
- Compact design
- Freed from radiation control
- Highly reliable X-ray tube and detector with extended lifetime characteristics
- Analytical software with integrated database
TECHNICAL DESCRIPTION
Difray-401k is a desktop X-ray powder diffractometer designed to solve a wide range of analytical, technological and scientific research problems of materials science. The main purpose of the instrument is qualitative and quantitative determination of phase composition of powder samples, wires, plates, single crystals and other objects.
The use of a position-sensitive gas-filled detector in Difray-401k makes it possible to get a high-quality diffraction pattern in a few minutes. A broad range of the spectrum (43 degrees) is detected simultaneously, so certain analytical tasks can be carried out without changing the positions of the X-ray tube and the detector.
To get a complete diffraction pattern (from 0 to 154 degrees), measurements are made in several angle intervals with subsequent software stitching of the acquired spectra.
Movement of the detector and the X-ray source can be performed manually, with a step of 2.5 degrees (basic package), and also in the automatic scanning mode, with a step of 0.01 degrees (extended package).
All components of the Difray-401k X-ray diffractometer are highly reliable and do not require replacement during the entire lifetime of the instrument. This significantly reduces the cost of maintaining the diffractometer and saves the budget.
The instrument can be equipped with:
- multipurpose sample unit
- automatic sample stage for 6 samples (autosampler)
- single crystal analysis sample unit
- texture sample unit
The Difray-401k diffractometer with the multipurpose sample unit |
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The multipurpose sample unit is intended for the analysis of powders, micro-objects and wires. This unit makes it possible to automatically move the sample in vertical and horizontal planes, so one can select a point for analysis on a conductor or micro-sample, or to sequentially analyze two powder samples placed in cuvettes. The minimum size of an analyzed sample in each direction is 0.1 mm. The maximum size of an analyzed sample in each direction is 20 mm. Sample rotation during the measurements is possible. Cuvettes used for the analysis of powders have the following sizes (depth/diameter, mm): 0.5×10, 1×10, 2×10, 0.5×5, 1×5. Collet holders for conductors, wires and micro-objects have the following sizes (diameter, mm): 0.5, 1.6, 2.5, 3,5. |
The Difray-401k diffractometer with the autosampler |
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The automatic sample stage (autosampler) makes it possible to install up to 6 cuvettes or sample holders for analysis in automatic mode. Sample rotation during the measurements is possible. The autosampler is convenient for the analysis of similar materials, which are analyzed according to corresponding dedicated programs. Cuvettes used for the analysis of powders have the following sizes (depth/diameter, mm): 0.5×10, 1×10, 2×10, 0.5×5, 1×5. Sample holders are intended for installation of solid samples with a flat surface with the diameter of up to 20 mm and thickness of up to 5 mm. |
The Difray-401k diffractometer with the single crystal analysis sample unit |
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This sample unit makes it possible to determine the direction and magnitude of single crystal misorientation, as well as to monitor whether the orientation of the base slice corresponds to the crystallographic direction. The measurements are performed automatically. In addition to analysis of single crystals, the sample unit also provides the ability to analyze powder samples and plates. The range of azimuthal rotations in the plane of the sample (the ϕ angle) is 0...360° (step 0.005°). The movement of the X-ray source is carried out automatically in the range of angles from 0° to 90° (step 0.001°). |
The Difray-401k diffractometer with the texture sample unit |
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This sample unit makes it possible to make automatic measurements (scanning along the θ, ϕ and χ angles) of any objects (plates, powders, massive objects, etc.). The range of azimuthal rotations in the plane of the sample (the ϕ angle) is 0…360° (step 0.001°). The slope of the sample in its plane (the χ angle) can vary in the range from -60° to 90° (step 0.001°). The movement of the X-ray source is carried out automatically in the range of angles from 0° to 90° (step 0.001°). |
Depending on the problem being solved, various methods of X-ray radiation collimation are used.
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Monocapillary glass collimator |
Adjustable slit collimator |
Slit holder with a set of replaceable slits (0.2, 0.4, 0.6, 0.8 mm) |
TECHNICAL CHARACTERISTICS
| X-ray focusing geometries | Bragg-Brentano, Debye-Scherrer |
| Goniometer radius | 114 mm |
| Full range of diffraction angle measurements, 2θ | 0÷154° |
| Simultaneous spectrum detection range | 43° |
| Detector type | Bent gas-filled position-sensitive detector |
| X-ray tube type | BSV-33 |
| X-ray tube anode material | Cr (Fe, Co, Cu) |
| X-ray tube adjustment range | 10 — 30 kV; 1 — 6 mA |
| Power consumption | < 500 W |
| Power supply | 220 V / 50 Hz |
| Dimensions (W×H×D) | 600×615×430 mm |
| Weight | 53 kg |
| Installation area | 1,5 m2 |
| PC interface | USB, RS-232 |
| Cooling | Autonomous cooling system |
OPERATING CONDITIONS
| Ambient temperature | From 10 to 35°С |
| Relative humidity | Up to 80% at the temperature of 25°C |
| Atmospheric pressure | 84 — 106.7 kPa (630 — 800 mm Hg) |
| Power supply | Voltage 220±22 V, frequency 50±1 Hz |
SOFTWARE
The instrument software includes four modules: Difract_Measurements, Difract_Processing, Difract_Base и Difract_Analysis.
Difract_ Measurements: instrument control and data acquisition
- turning on the instrument
- control of the X-ray tube high voltage power supply
- monitoring the state of the instruments components
- setting parameters for X-ray diffraction measurements
- making measurements, including ones that correspond to different measurement scenarios
- output of reports on measurement results
Difract_Processing: data processing and analysis
- preliminary data processing (smoothing, addition and subtraction of diffractograms, determination of the background line, peak approximation)
- detector calibration by diffraction angles using calibration samples
- "stitching" of spectra for two or more adjacent measurement ranges
- automatic scaling of diffractograms
- search and determination of diffraction maxima positions in automatic and manual modes
- simultaneous display of several diffractograms
- saving the measured diffractograms in various formats
Difract_Base: phase analysis
- qualitative phase analysis
- semi-quantitative analysis using the corundum numbers method, the calibration curve method and the ratio of 100% lines method
- refinement of unit cell parameters using the least squares method
- search within the integrated diffraction database containing 120 thousand compounds
- creation of custom libraries of diffractograms
- determination of the degree of crystallinity
- determination of sizes of coherent scattering regions
- output of reports on analysis results
Difract_Analysis: quantitative analysis
- quantitative phase analysis using the method of calibrations
- display and processing of several diffractograms
- creation of calibration tables
- various methods of spectra processing (approximation of diffraction peaks by various functions, finding the background line, deconvolution, etc.)
- creation of diffractogram processing scenarios for the Difract_ Measurements module