X-Ray Diffraction Intensity of Oxide Solid Solutions: Application to Qualitative and Quantitative Phase Analysis

1982 ◽  
pp. 119-128
Author(s):  
Ronald C. Gehringer ◽  
Gregory J. McCarthy ◽  
R. G. Garvey ◽  
Deane K. Smith
1982 ◽  
Vol 26 ◽  
pp. 119-128 ◽  
Author(s):  
Ronald C. Gehringer ◽  
Gregory J. McCarthy ◽  
R.G. Garvey ◽  
Deane K. Smith

Solid solutions are pervasive in minerals and in industrial inorganic materials. The analyst is often called upon to provide qualitative and quantitative X-ray phase analysis for specimens containing solid solutions when all that is available are Powder Diffraction File (PDF) data or commercial standards for the end members. In an earlier paper (1) we presented several examples of substantial errors in accuracy of quantitative analysis that can arise when the crystallinity and composition of the analyte standard do not match those of the analyte in the sample of interest. We recommended that to obtain more accurate quantitative analyses, one should determine the analyte composition (e.g., from XRF on grains seen in a SEM or from comparison of cell parameters with those of the end members) and synthesize an analyte standard with this composition and with a crystallinity approximating that of the analyte (e.g., as determined from peak breadth or α1/ α2 splitting).


1966 ◽  
Vol 38 (12) ◽  
pp. 1741-1745 ◽  
Author(s):  
R. F. Karlak ◽  
D. S. Burnett

1957 ◽  
Vol 1 ◽  
pp. 39-58
Author(s):  
Ralph H. Hiltz ◽  
Stanley L. Lopata

AbstractIn view of present difficulties encountered in met alio graphic methods of phase analysis of titanium and its alloys, the possibility of utilizing integrated X-ray intensities for phase analysis was investigated. Power Formula variables were calculated for titanium, and relative areas of three alpha and one beta peak were determined. Recorded X-ray intensities were obtained from a large number of titanium specimens. The recorded intensities were analyzed and the results compared with those from metallographic analysis. The errors in the method arising from the nature of titanium, texture and peak overlapping, were studied and where possible, compensated for by adjusting the method of measurement and calculation.


2007 ◽  
Vol 57 (12) ◽  
pp. 1145-1148 ◽  
Author(s):  
LaReine A. Yeoh ◽  
Klaus-Dieter Liss ◽  
Arno Bartels ◽  
Harald Chladil ◽  
Maxim Avdeev ◽  
...  

2005 ◽  
Vol 20 (3) ◽  
pp. 218-223 ◽  
Author(s):  
Chang-An Wang ◽  
Aiguo Zhou ◽  
Liang Qi ◽  
Yong Huang

Materials in the Ti–Al–C ternary system commonly contain three coexisting phases, Ti3AlC2, Ti2AlC, and TiC. Quantitative phase analysis in this ternary system was investigated using X-ray diffraction. First, nonoverlap diffraction peaks were selected: the (002) peak at 2θ=9.5° for Ti3AlC2 (I∕I0=26.5), the (002) peak at 2θ=13.0° for Ti2AlC (I∕I0=39), and the (111) peak at 2θ=35.9° for TiC (I∕I0=78), respectively. Then, based on the mixing-sample method without internal standards, a set of equations was derived for determining the amounts of Ti3AlC2, Ti2AlC, and TiC in a sample using the intensities of the selected diffraction peaks. Finally, the applicability and error sources for this method were investigated. The method is simple and straightforward, and is applicable to the entire Ti–Al–C ternary system, since the derivation of this equation group is self-checking.


Crystals ◽  
2020 ◽  
Vol 10 (1) ◽  
pp. 27 ◽  
Author(s):  
Stanko Popović

X-ray powder diffraction is an ideal technique for the quantitative analysis of a multiphase sample. The intensities of diffraction lines of a phase in a multiphase sample are proportional to the phase fraction and the quantitative analysis can be obtained if the correction for the absorption of X-rays in the sample is performed. Simple procedures of quantitative X-ray diffraction phase analysis of a multiphase sample are presented. The matrix-flushing method, with the application of reference intensities, yields the relationship between the intensity and phase fraction free from the absorption effect, thus, shunting calibration curves or internal standard procedures. Special attention is paid to the doping methods: (i) simultaneous determination of the fractions of several phases using a single doping and (ii) determination of the fraction of the dominant phase. The conditions to minimize systematic errors are discussed. The problem of overlapping of diffraction lines can be overcome by combining the doping method (i) and the individual profile fitting method, thus performing the quantitative phase analysis without the reference to structural models of particular phases. Recent suggestions in quantitative phase analysis are quoted, e.g., in study of the decomposition of supersaturated solid solutions—intermetallic alloys. Round Robin on Quantitative Phase Analysis, organized by the IUCr Commission on Powder Diffraction, is discussed shortly. The doping methods have been applied in various studies, e.g., phase transitions in titanium dioxide, biomineralization processes, and phases in intermetallic oxide systems and intermetallic alloys.


1979 ◽  
Vol 23 ◽  
pp. 375-379
Author(s):  
Z. Mencik ◽  
M. A. Short ◽  
C. R. Peters

Synthetically prepared silicon nitride is one of the more promising ceramic materials for structural components of gas turbines. Typical material may contain a-silicon nitride, Si3N4 (which is believed to always contain oxygen and therefore, according to Grievson, Jack and Wild, is more properly written as Si11.5N15O0.5), β-silicon nitride, Si3N4, silicon oxynitride, Si2ON2, silicon metal, Si, and α-cristobalite, SiO2. Because the physical properties of the ceramic parts are dependent on their phase composition, it is essential that a technique be available for performing a phase analysis. An X-ray diffraction procedure has been, developed for the quantitative phase analysis of synthetically prepared silicon nitride. This procedure converts experimentally measured intensities of selected X-ray diffraction peaks to weight fractions of components using empirically determined intensity coefficients.


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