On the use of one-dimensional position sensitive detector for x-ray diffraction reciprocal space mapping: Data quality and limitations

2005 ◽  
Vol 76 (6) ◽  
pp. 063912 ◽  
Author(s):  
Olivier Masson ◽  
Alexandre Boulle ◽  
René Guinebretière ◽  
André Lecomte ◽  
Alain Dauger
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.


1994 ◽  
Vol 38 ◽  
pp. 201-213 ◽  
Author(s):  
S. R. Lee ◽  
B. L. Doyle ◽  
T. J. Drummond ◽  
J. W. Medernach ◽  
P. Schneider

Abstract Reciprocal space mapping can be efficiently carried out using a position-sensitive x-ray detector (PSD) coupled to a traditional double-axis diffractometer. The PSD offers parallel measurement of the total scattering angle of all diffracted x-rays during a single rocking-curve scan. As a result, a two-dimensional reciprocal space map can be made in a very short time similar to that of a one-dimensional rocking-curve scan. Fast, efficient reciprocal space mapping offers numerous routine advantages to the x-ray diffraction analyst. Some of these advantages arc the explicit differentiation of lattice strain from crystal orientation effects in strain-relaxed heteroepitaxial layers; the nondestructive characterization of the size, shape and orientation of nanocrystalline domains in ordered-alloy epilayers; and the ability to measure the average size and shape of voids in porous epilayers. Here, the PSD-based diffractometer is described, and specific examples clearly illustrating the advantages of complete reciprocal space analysis are presented.


1979 ◽  
Author(s):  
T.P. Russell ◽  
R.S. Stein ◽  
M.K. Kopp ◽  
R.E. Zedler ◽  
R.W. Hendricks ◽  
...  

1985 ◽  
Vol 18 (6) ◽  
pp. 487-492 ◽  
Author(s):  
A. Burian ◽  
P. Lecante ◽  
A. Mosset ◽  
J. Galy ◽  
J. Van Dun ◽  
...  

Expressions for the absorption correction function are obtained in the form of integral equations for the case of a flat-plate sample and a position-sensitive detector. It is shown that the absorption correction used for both transmission and reflection geometries with a conventional diffractometer may be applied to a diffractometer equipped with a linear position-sensitive detector. The application of a Savitzky–Golay-type digital filter considerably facilitates the analysis of the data without losing pertinent information.


1987 ◽  
Vol 31 ◽  
pp. 325-330
Author(s):  
B. A. Foster ◽  
E. R. Wolfel

The method for quantitative X-ray diffraction analysis of multiphase mixtures presented here is based on transmission measurements of thin samples. The integral of all reflections of interest are measured with a position sensitive detector at one time while the transmission factor of the sample is measured simultaneously with a scintillation counter. The method has the advantages that only a few (1-5) mg of substance are required, absorption effects due to sample matrix are measured directly and the method is automated. The measurements are made with the STOE/ Nicolet Automatic Focusing X-ray Diffraction system in conjunction with the STOE/Nicolet Curved Position Sensitive Detector.


1990 ◽  
Vol 23 (6) ◽  
pp. 476-484 ◽  
Author(s):  
J. C. Osborn ◽  
T. R. Welberry

The use of a one-dimensional position-sensitive detector for diffuse X-ray scattering measurements is described. Calibration procedures for scattering angle and intensity measurements are discussed. Some nonuniformities have been found in the counting efficiency as a function of distance along the detector. A procedure is described for measuring the diffuse scattering in a section of reciprocal space.


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