A Guinier Diffractometer with a Scanning Position Sensitive Detector

1981 ◽  
Vol 25 ◽  
pp. 315-324 ◽  
Author(s):  
Herbert E. Göbel

AbstractA strictly focussing Guinier diffractometer using a linear position-sensitive proportional counter (PSPC) to detect the diffracted x-rays is described. The data collection time for a complete pattern can so be reduced to minutes Instead of hours as it used to be in conventional film- or counter-Guinier systems. The PSPC collects all diffracted x-rays over several degrees of 2 Theta in parallel and composes the full pattern by a continuous scan over the whole 2 Theta range. This principle was described in Adv. In X-Ray Anal. Vol. 22, 255 ff and 24, 123 ff. for Bragg-Brentano diffractometers.

1978 ◽  
Vol 11 (3) ◽  
pp. 173-178 ◽  
Author(s):  
E. Prince ◽  
A. Wlodawer ◽  
A. Santoro

The recent development of linear position-sensitive detectors for neutrons and X-rays leads to the possibility of large improvements in the efficiency of data collection in single-crystal diffractometers. In order to take advantage of the properties of a linear position-sensitive detector it is desirable to use a diffraction geometry which causes the diffracted beams from many different reflecting planes to lie in a common plane. A design for a diffractometer utilizing the flat-cone geometry is described, and the relevant mathematical formulas are summarized. An instrument using this design has been constructed as a modification to an existing four-circle diffractometer and is now operating. Practical details of its construction, of the collection and handling of data, and of data rates are discussed.


1992 ◽  
Vol 36 ◽  
pp. 617-622
Author(s):  
J. L. Radtke ◽  
D. W. Beard

AbstractPosition sensitive detectors provide efficient X-ray detection over large solid angles; this capability has revolutionized X-ray diffractometry by reducing data collection time. This paper describes testing of a new single-axis position sensitive detector designed to locate 0.6-2 Angstrom X-rays. Dead time, quantum efficiency, energy resolution, and spatial resolution were measured. Standard powder diffraction patterns were observed with the detector, and data sets are presented. The impact of detector performance parameters on diffraction experiments is discussed.


1980 ◽  
Vol 24 ◽  
pp. 177-180 ◽  
Author(s):  
K. Taniguchi ◽  
K. Oka ◽  
N. Yamaki ◽  
S. Ikeda

An active recording x-ray crystal spectrometer for extended x-ray absorption fine structure (EXAFS) has been built using a position sensitive detector of the self scanning photodiode array (SSPA) type. The SSPA detector has energy and position sensitivity for x-rays. The spectrometer was applied to the measurement for EXAFS of the several compounds in foil, powder and liquid states. The spectra can be obtained rapidly, and compare very well with other methods. We found that the SSPA detector is very useful for the measurement of EXAFS.


1982 ◽  
Vol 26 ◽  
pp. 269-274 ◽  
Author(s):  
B. Sleaford ◽  
V. Perez-Mendez ◽  
C.N.J. Wagner

AbstractA curved, one-dimensional position-sensitive detector has been designed and constructed for the measurement of the scattering patterns from non-crystalline materials. The chamber is a one-dimensional, pressurized, gas-filled detector with delay line readout for position encoding. It covers an angular range of 45° in 2θ, and its quantum efficiency is 80% and 50% for 17.5 and 60 KeV x-rays, respectively, when using a Xe-20%CO2 gas mixture at 7 atm.


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


1987 ◽  
Vol 112 ◽  
Author(s):  
J. Caurel ◽  
D. Beaufort ◽  
E. Y. Vernaz

AbstractThis study was undertaken to clarify the alteration process of French LWR synthetic glass leached by distilled water at 250 and 300°C for 28 days. The present experiments emphasize “in situ” identification of the alteration products in small areas (20 × 10−4 mm2 ) along the alteration profile by a specific X-ray diffraction technique.Experimental assembly: The sample is irradiated by an incident X-ray beam (Co k α, 40 mA, 40 Kv) focused to a 150 μ m diameter. The sample oscillates around a θ central selected position and the diffracted X-rays are detected simultaneously in a 14.5 (2 θ ) solid angle, then recorded by the linear position sensitive detector and stored in a multichannel analyzer.


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.


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