Defect structure analysis of polycrystalline materials by computer-controlled double-crystal diffractometer with position-sensitive detector

1983 ◽  
Vol 16 (1) ◽  
pp. 89-95 ◽  
Author(s):  
R. Yazici ◽  
W. Mayo ◽  
T. Takemoto ◽  
S. Weissmann

The method represents an extension of a previously developed X-ray double-crystal diffractometer method when a film was used to record the crystallite reflections, each reflecting crystallite being regarded as the second crystal of a double-crystal diffractometer. By utilizing a position-sensitive detector (PSD) with interactive computer controls, the tedious and limiting task of data acquisition and analysis is greatly simplified. The specimen is irradiated with crystal-monochromated radiation and the numerous microscopic spots emanating from the reflecting crystallites are recorded separately by the position-sensitive detector and its associated multichannel analyzer at each increment of specimen rotation. An on-line minicomputer simultaneously collects these data and applies the necessary corrections. This process is then automatically repeated through the full rocking-curve range. The computer carries out the rocking-curve analysis of the individual crystallite reflections as well as that of the entire reflecting crystallite population. The instrument is provided with a specimen translation device which permits analysis of large sections of solid specimens. Thus, sites of local lattice defects induced either mechanically, chemically or by radiation can rapidly be established and quantitatively determined in terms of rocking-curve parameters as well as imaged by X-ray topography, by inserting a film in front of the PSD. The versatility and usefulness of the method is demonstrated by examples given from studies of fracture, fatigue and stress-corrosion cracking of commercial alloys.

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.


1986 ◽  
Vol 82 ◽  
Author(s):  
T. S. Ananthanarayanan ◽  
R. G. Rosemeier ◽  
W. E. Mayo ◽  
J. H. Dinan

SUMMARYThere is a considerable body of work available illustrating the significance of X-ray rocking curve measurements in micro-electronic applications. For the first time a high resolution (100-150µm) 2-dimensional technique called DARC (Digital Autcmated Rocking Curve) topography has been implemented. This method is an enhancement of the conventional double crystal diffractometer using a real time 2-dimensional X-ray detector.Several materials have been successfully examined using DARC topography. Same of these include: Si, GaAs, AlGaAs, InGaAs, HgMnTe, Al, Inconel, steels, etc. By choosing the appropriate Bragg reflection multi-layered micro-electronic structures have been analyzed nondestructively. Several epitaxial films, including HgCdTe and ZnCdTe, grown by molecular beam epitaxy, have also been characterized using iARC topography. The rocking curve half width maps can be translated to dislocation density maps with relative ease. This technique also allows the deconvolution of the micro-plastic lattice strain ccaponent from the total strain tensor.


2006 ◽  
Vol 524-525 ◽  
pp. 859-864
Author(s):  
Neila Hfaiedh ◽  
Manuel François ◽  
Khemais Saanouni

Internal stresses are an important factor in understanding the work hardening behaviour of polycrystalline materials. The goal of the present paper is to study the development of second order stresses in textured copper sheets at large plastic strains, up to fracture by X-ray diffraction. Second order stresses manifest themselves as peak displacements and width changes as azimuth and tilt angles are varied. As the acquisition is performed with a position sensitive detector, a specific correction of intensities is required in order to take into account texture influence on peak shape and consequently on peak position and width.


1990 ◽  
Vol 205 ◽  
Author(s):  
Axel NØrlund Christensen

AbstractTime resolved X-ray powder diffraction was used to follow the crystallization processes in the systems MgO-MgCl2-H2O and MgO-H2O. A Stoe X-ray powder diffractometer with a position sensitive detector was used. The crystalline reaction products are [Mg2(OH)3(H2O)2]C1.H2O and Mg(OH)2 dependent upon the MgC12 concentrations in the heterogeneous systems. Mg(OH)2 was the product in a 1.50 M MgCl2 solution and [Mg2(OH)3(H2O)3]Cl.H2O was formed in 3.00 and 5.17 M MgCl2 solutions at 20°C.


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