TY - JOUR

T1 - Procedure of the Quantitative Powder X-Ray Diffraction Analysis of Low-Temperature Alumina Forms

AU - Petrov, I. yu.

AU - Pakharukova, V. p.

AU - Tsybulya, S. v.

N1 - The work was supported by the Ministry of Science and Higher Education of the Russian Federation (project FWUR-2024-0032).

PY - 2025/3/28

Y1 - 2025/3/28

N2 - A procedure is proposed for the quantitative powder X-ray diffraction (XRD) analysis of powder mixtures of nanocrystalline low-temperature alumina forms. It is based on the presentation of the XRD pattern of the mixture being analyzed by a linear combination of the XRD profiles of reference oxides. The purpose of the quantitative analysis is the least-squares refinement of weight coefficients of the profiles until agreement is achieved between the experimental and generated XRD patterns. The pre-normalization procedure of the experimental XRD profiles with conversion to electronic units enables the analysis of data obtained on instruments with different measurement geometries and instrumental parameters. The procedure is verified using γ-Al2O3 and χ-Al2O3 mixtures of set compositions, and the accuracy of this procedure is compared with that of the calibration plot method. The absolute error of the χ-Al2O3 weight fraction determined by the procedure proposed is two times lower than that of the calibration plot method: 5 wt.% against 10 wt.%. By simulating the noise in the model XRD profiles it is shown that the random error contribution is about 1 wt.%.

AB - A procedure is proposed for the quantitative powder X-ray diffraction (XRD) analysis of powder mixtures of nanocrystalline low-temperature alumina forms. It is based on the presentation of the XRD pattern of the mixture being analyzed by a linear combination of the XRD profiles of reference oxides. The purpose of the quantitative analysis is the least-squares refinement of weight coefficients of the profiles until agreement is achieved between the experimental and generated XRD patterns. The pre-normalization procedure of the experimental XRD profiles with conversion to electronic units enables the analysis of data obtained on instruments with different measurement geometries and instrumental parameters. The procedure is verified using γ-Al2O3 and χ-Al2O3 mixtures of set compositions, and the accuracy of this procedure is compared with that of the calibration plot method. The absolute error of the χ-Al2O3 weight fraction determined by the procedure proposed is two times lower than that of the calibration plot method: 5 wt.% against 10 wt.%. By simulating the noise in the model XRD profiles it is shown that the random error contribution is about 1 wt.%.

KW - alumina

KW - quantitative powder X-ray diffraction analysis

UR - https://www.scopus.com/record/display.uri?eid=2-s2.0-105001262742&origin=inward&txGid=1fa70dd341f957ae144ab5d9d3c26950

U2 - 10.1134/S0022476625030096

DO - 10.1134/S0022476625030096

M3 - Article

VL - 66

SP - 516

EP - 529

JO - Journal of Structural Chemistry

JF - Journal of Structural Chemistry

SN - 0022-4766

IS - 3

ER -