X-ray powder diffraction (XRD): Basic principles & practical applications (2025)

Evaluation via multivariate techniques of scale factor variability in the rietveld method applied to quantitative phase analysis with X ray powder diffraction

Materials Research-ibero-american Journal of Materials, 2006

The present work uses multivariate statistical analysis as a form of establishing the main sources of error in the Quantitative Phase Analysis (QPA) using the Rietveld method. The quantitative determination of crystalline phases using x ray powder diffraction is a complex measurement process whose results are influenced by several factors. Ternary mixtures of Al 2 O 3 , MgO and NiO were prepared under controlled conditions and the diffractions were obtained using the Bragg-Brentano geometric arrangement. It was possible to establish four sources of critical variations: the experimental absorption and the scale factor of NiO, which is the phase with the greatest linear absorption coefficient of the ternary mixture; the instrumental characteristics represented by mechanical errors of the goniometer and sample displacement; the other two phases (Al 2 O 3 and MgO); and the temperature and relative humidity of the air in the laboratory. The error sources excessively impair the QPA with the Rietveld method. Therefore it becomes necessary to control them during the measurement procedure.

Robustness of the quantitative phase analysis of X-ray diffraction data by the Rietveld method

arXiv: Materials Science, 2020

The quality of X-ray powder diffraction data and the number and type of refinable parameters has been examined with respect to their effect on quantitative phase analysis (QPA) by the Rietveld method using data collected from two samples from the QPA round robin [Madsen et al. J. Appl. Cryst. (2001), 34, 409--26]. For specimens where the diffracted intensity is split between all phases approximately equally accurate results could be obtained with a maximum observed intensity in the range of 1000--200000 counts. The best refinement model was one that did not refine atomic displacement parameters, but did allow other parameters to refine. For specimens where there existed minor or trace phases, this intensity range changed to 5000--1000000 counts. The refinement model with the most accurate results was one that refined a minimum of parameters, especially for the minor/trace phases. Given that all phases were quite crystalline, step sizes for both types of specimen could range between ...

The effect of data quality and model parameters on the quantitative phase analysis of X-ray diffraction data by the Rietveld method

Journal of Applied Crystallography, 2021

The quality of X-ray powder diffraction data and the number and type of refinable parameters have been examined with respect to their effect on quantitative phase analysis (QPA) by the Rietveld method using data collected from two samples from the QPA round robin [Madsen, Scarlett, Cranswick & Lwin (2001). J. Appl. Cryst. 34, 409–426]. From the analyses of these best-case-scenario specimens, a series of recommendations for minimum standards of data collection and analysis are proposed. It is hoped that these will aid new QPA-by-Rietveld users in their analyses.

Outcomes of the International Union of Crystallography Commission on Powder Diffraction Round Robin on Quantitative Phase Analysis: samples 1 a to 1 h

Journal of Applied Crystallography, 2001

The International Union of Crystallography (IUCr) Commission on Powder Diffraction (CPD) has sponsored a round robin on the determination of quantitative phase abundance from diffraction data. Specifically, the aims of the round robin were (i) to document the methods and strategies commonly employed in quantitative phase analysis (QPA), especially those involving powder diffraction, (ii) to assess levels of accuracy, precision and lower limits of detection, (iii) to identify specific problem areas and develop practical solutions, (iv) to formulate recommended procedures for QPA using diffraction data, and (v) to create a standard set of samples for future reference. Some of the analytical issues which have been addressed include (a) the type of analysis (integrated intensities or full-profile, Rietveld or full-profile, database of observed patterns) and (b) the type of instrument used, including geometry and radiation (X-ray, neutron or synchrotron). While the samples used in the ro...

Fitting Full X-Ray Diffraction Patterns for Quantitative Analysis: A Method for Readily Quantifying Crystalline and Disordered Phases

Advances in Materials Physics and Chemistry, 2013

Fitting of full X-ray diffraction patterns is an effective method for quantifying abundances during X-ray diffraction (XRD) analyses. The method is based on the principal that the observed diffraction pattern is the sum of the individual phases that compose the sample. By adding an internal standard (usually corundum) to both the observed patterns and to those for individual pure phases (standards), all patterns can all be normalized to an equivalent intensity based on the internal standard intensity. Using least-squares refinement, the individual phase proportions are varied until an optimal match is reached. As the fitting of full patterns uses the entire pattern, including background, disordered and amorphous phases are explicitly considered as individual phases, with their individual intensity profiles or "amorphous humps" included in the refinement. The method can be applied not only to samples that contain well-ordered materials, but it is particularly well suited for samples containing amorphous and/or disordered materials. In cases with extremely disordered materials where no crystal structure is available for Rietveld refinement or there is no unique intensity area that can be measured for a traditional RIR analysis, full-pattern fitting may be the best or only way to readily obtain quantitative results. This approach is also applicable in cases where there are several coexisting highly disordered phases. As all phases are considered as discrete individual components, abundances are not constrained to sum to 100%.

Outcomes of the International Union of Crystallography Commission on powder diffraction round robin on quantitative phase analysis: samples

2014

Diffraction (CPD) has sponsored a round robin on the determination of quantitative phase abundance from diffraction data. Speci®cally, the aims of the round robin were (i) to document the methods and strategies commonly employed in quantitative phase analysis (QPA), especially those involving powder diffraction, (ii) to assess levels of accuracy, precision and lower limits of detection, (iii) to identify speci®c problem areas and develop practical solutions, (iv) to formulate recommended procedures for QPA using diffraction data, and (v) to create a standard set of samples for future reference. Some of the analytical issues which have been addressed include (a) the type of analysis (integrated intensities or full-pro®le, Rietveld or full-pro®le, database of observed patterns) and (b) the type of instrument used, including geometry and radiation (X-ray, neutron or synchrotron). While the samples used in the round robin covered a wide range of analytical complexity, this paper reports...

X-ray powder diffraction

Quantitative Phase Analysis Using the Rietveld Method

Quantitative phase analysis of multicomponent mixtures using X-ray powder diffraction data has been approached with a modified version of the Rietveld computer program of Wiles & Young [ J. Appl. Cryst. (1981), 14, 149-151]. This new method does not require measurement of calibration data nor the use of an internal standard; however, the approximate crystal structure of each phase of interest in a mixture is necessary. The use of an internal standard will allow the determination of total amorphous phase content in a mixture. Analysis of synthetic mixtures yielded high-precision results, with errors generally less than 1.0% absolute. Since this technique fits the complete diffraction pattern, it is less susceptible to primary extinction effects and minor amounts of preferred orientation. Additional benefits of this technique over traditional quantitative analysis methods include the determination of precise cell parameters and approximate chemical compositions, and the potential for the correction of preferred orientation and microabsorption effects.

14+ MILLION TOP 1% MOST CITED SCIENTIST 12.2% AUTHORS AND EDITORS FROM TOP 500 UNIVERSITIES The Quantification of Crystalline Phases in Materials: Applications of Rietveld Method

2020

An estimation of the correctness of XRD results obtained from the analysis of materials with bimodal crystallite size distribution

An estimation of the correctness of XRD results obtained from the analysis of materials with bimodal crystallite size distribution † Vladimir Uvarov * and Inna Popov 36 powder artificial mixtures and 2 usual samples with a bimodal crystallite size distribution have been prepared and examined by an X-ray diffraction method. We estimated the capability of the Rietveld refinement at a "double-phase model" mode and the correctness of the results. The homogeneity and the crystallite sizes of pure phases used in the preparation of the mixtures were checked by TEM. In most cases, Rietveld refinement at a "double-phase model" mode provided reliable information about both the crystallite size and percentage of constituents. Reliability of XRD results was higher for the powder mixtures with a larger difference in crystallite sizes. It was found that the shape of the crystallites can have a significant impact on the analysis results, and for columnar crystals, the employed method did not always provide correct results. When size distribution of the material deviates from a bimodal one, the correctness of the result decreases. Such an investigation was performed for the first time.