Simultaneous Position-Resolved Determination of Phase and Stress Distributions by means of an X-ray Diffractometer with a Two-Dimensional Position-Sensitive Detector

1995 ◽  
Vol 28 (5) ◽  
pp. 561-567 ◽  
Author(s):  
D. Stephan ◽  
G. Grosse ◽  
K. Wetzig

With an X-ray area detector and a suitable Soller-plate collimator in the scattered radiation field, it is possible to realize a versatile X-ray diffractometer. The local diffraction information of a sample can be registered simultaneously and visualized with a spatial resolution better than 0.5 mm, maintaining reasonable measuring times of a few minutes. Results of measurements applied to local phase analysis (distribution of retained austenite and carbon on a cross section of case-hardened steel), to the determination of lateral stress distributions (laser-hardened track on C45 steel) and to the analysis of crystallite orientation (coarse-grained YBa2Cu3O δ ) are presented.

1980 ◽  
Vol 24 ◽  
pp. 123-138 ◽  
Author(s):  
Herbert E. Göbel

AbstractBy collecting the diffracted X-rays in a focussing powder diffractometer with a linear position-sensitive detector (PSD), the data accumulation time can be widely reduced. Due to the focussing properties of the geometrical arrangement good resolution can be simultaneously achieved over a few degrees of the diffraction angle 2 Theta. The full pattern is collected by scanning the PSD along the entire 2 Theta arc. Scanning speeds of several hundred degrees per minute are possible and still yield well plotted diagrams.This work demonstrates the performance of the system in different tasks of X-ray powder diffraction such as identification of unknown materials, quantitative analysis, determination of lattice constants and microcrystalline properties. The results, evaluated by parts of the program system DIFFRAC 11, show that the accuracy and resolution of the continuously scanning PSD technique match these tasks without difficulty and reach the precision limits of powder diffractometry itself. It is demonstrated that the data collection velocity, which matches well the data evaluation times, is not the only advantage compared to conventional diffractometets.


Author(s):  
D. Prella ◽  
F. Cámara

AbstractIn order to check for the accuracy of X-ray diffracted data collected with an area-detector diffractometer (FAST-Nonius), we have carried out several data collections on a good-quality pyrope crystal (space group


2020 ◽  
Vol 86 (6) ◽  
pp. 29-35
Author(s):  
V. P. Sirotinkin ◽  
O. V. Baranov ◽  
A. Yu. Fedotov ◽  
S. M. Barinov

The results of studying the phase composition of advanced calcium phosphates Ca10(PO4)6(OH)2, β-Ca3(PO4)2, α-Ca3(PO4)2, CaHPO4 · 2H2O, Ca8(HPO4)2(PO4)4 · 5H2O using an x-ray diffractometer with a curved position-sensitive detector are presented. Optimal experimental conditions (angular positions of the x-ray tube and detector, size of the slits, exposure time) were determined with allowance for possible formation of the impurity phases during synthesis. The construction features of diffractometers with a position-sensitive detector affecting the profile characteristics of x-ray diffraction peaks are considered. The composition for calibration of the diffractometer (a mixture of sodium acetate and yttrium oxide) was determined. Theoretical x-ray diffraction patterns for corresponding calcium phosphates are constructed on the basis of the literature data. These x-ray diffraction patterns were used to determine the phase composition of the advanced calcium phosphates. The features of advanced calcium phosphates, which should be taken into account during the phase analysis, are indicated. The powder of high-temperature form of tricalcium phosphate strongly adsorbs water from the environment. A strong texture is observed on the x-ray diffraction spectra of dicalcium phosphate dihydrate. A rather specific x-ray diffraction pattern of octacalcium phosphate pentahydrate revealed the only one strong peak at small angles. In all cases, significant deviations are observed for the recorded angular positions and relative intensity of the diffraction peaks. The results of the study of experimentally obtained mixtures of calcium phosphate are presented. It is shown that the graphic comparison of experimental x-ray diffraction spectra and pre-recorded spectra of the reference calcium phosphates and possible impurity phases is the most effective method. In this case, there is no need for calibration. When using this method, the total time for analysis of one sample is no more than 10 min.


2021 ◽  
Vol 28 (3) ◽  
Author(s):  
Daisuke Ishikawa ◽  
Alfred Q. R. Baron

The detailed fabrication and performance of the temperature-gradient analyzers that were simulated by Ishikawa & Baron [(2010). J. Synchrotron Rad. 17, 12–24] are described and extended to include both quadratic and 2D gradients. The application of a temperature gradient compensates for geometric contributions to the energy resolution while allowing collection of a large solid angle, ∼50 mrad × 50 mrad, of scattered radiation. In particular, when operating relatively close to backscattering, π/2 − θB = 1.58 mrad, the application of a gradient of 1.32 K per 80 mm improves the measured total resolution from 60 to 25 meV at the full width at half-maximum, while when operating further from backscattering, π/2 − θB = 6.56 mrad, improvement from 330 to 32 meV is observed using a combination of a gradient of 6.2 K per 80 mm and dispersion compensation with a position-sensitive detector. In both cases, the operating energy was 15.8 keV and the incident bandwidth was 22 meV. Notably, the use of a temperature gradient allows a relatively large clearance at the sample, permitting installation of more complicated sample environments.


Optik ◽  
2019 ◽  
Vol 186 ◽  
pp. 469-478
Author(s):  
Anmin Yin ◽  
Yufan Wang ◽  
Cheng Tao ◽  
Xuedao Shu ◽  
Zhenge Zhu ◽  
...  

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