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Combining XRD and XRF analysis in one Rietveld-like fitting

Published online by Cambridge University Press:  18 April 2017

M. Bortolotti ,
L. Lutterotti  and
G. Pepponi
M. Bortolotti*
Affiliation:
Dipartimento di Ingegneria Industriale, Università degli Studi di Trento, Italy
L. Lutterotti
Affiliation:
Dipartimento di Ingegneria Industriale, Università degli Studi di Trento, Italy
G. Pepponi
Affiliation:
Center for Materials and Microsystems, Fondazione Bruno Kessler, Trento, Italy
*
a)Author to whom correspondence should be addressed. Electronic mail: [email protected]
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Abstract

X-ray diffraction (XRD) and X-ray fluorescence (XRF) are widely used analytical techniques for materials characterization; the information they provide can be considered complementary, as the former is mostly used to obtain crystallographic information and analyze phase content, whereas the latter is sensitive to elemental composition. Many researchers and technologists working in a variety of application fields already use them together in some sort of a “combined” approach, by separately performing XRD and XRF data collection and analysis on the same sample and then comparing the analytical results obtained to integrate and complement the respective analytical information. In this work, we propose a true combined approach to merge both XRD and XRF data acquisition and analysis. Custom analytical X-ray instrumentation has been developed to perform the simultaneous data acquisition, by using a single X-ray source and dedicated detectors to collect the diffracted and fluorescent X-ray photons from the same sample volume. Additionally, a combined XRD/XRF data analysis methodology has been implemented by extending Rietveld based code to incorporate the full pattern fitting of XRF spectra starting from the phases instead of a simple matrix elemental composition. We report two analytical examples from different application fields to better illustrate the capabilities of the proposed approach.

Keywords

X-ray diffractionX-ray fluorescencecombined analysisquantitative phase analysisRietveld method
Type
Technical Articles
Information
Powder Diffraction , Volume 32 , Supplement S1 , September 2017 , pp. S225 - S230
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Copyright
Copyright © International Centre for Diffraction Data 2017 

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References

De Voorde, L. V., Vekemans, B., Verhaeven, E., Tack, P., De Wolf, R., Garrevoet, J., Vandenabeele, P., and Vincze, L. (2015). “Analytical characterization of a new mobile X-ray fluorescence and X-ray diffraction instrument combined with a pigment identification case study,” Spectrochim. Acta B 110, 14–19.Google Scholar
Ebel, H. (1999). “X-ray Tube Spectra,” X-ray Spectrom. 28, 255–266.Google Scholar
Ingerle, D., Pepponi, G., Meirer, F., Wobrauschek, P., and Streli, C. (2016). “JGIXA – a software package for the calculation and fitting of grazing incidence X-ray fluorescence and X-ray reflectivity data for the characterization of nanometer-layers and ultra-shallow-implants,” Spectrochim. Acta B 118, 20–28.Google Scholar
Kerner, J. A., Franco, E. D., and Marshall, J. (1995). “Combined XRD and XRF analysis for portable and remote applications,” Adv. X-Ray Anal. 38, 319–324.Google Scholar
Kogure, T. and Inoue, A. (2005). “Determination of defect structures in kaolin minerals by high-resolution transmission electron microscopy (HRTEM),” Am. Mineral. 90, 85–89.Google Scholar
Lutterotti, L. (2010). “Total pattern fitting for the combined size–strain–stress–texture determination in thin film diffraction”, Nucl. Instrum. Methods Phys. Res. B 268, 334–340.Google Scholar
Lutterotti, L., Bortolotti, M., Ischia, G., Lonardelli, I., and Wenk, H.-R. (2007). “Rietveld texture analysis from diffraction images,” Z. Kristallogr. 26, 125–130.Google Scholar
Lutterotti, L., Voltolini, M., Wenk, H.-R., Bandyopadhyay, K., and Vanorio, T. (2009). “Texture analysis of a turbostratically disordered Ca-montmorillonite,” Am. Mineral. 95, 98–103.CrossRefGoogle Scholar
Pantos, E., Kockelmann, W., Chapon, L. C., Lutterotti, L., Bennet, S. L., Tobin, M. J., Mosselmans, J. F. W., Pradell, T., Salvado, N., Butí, S., Garner, R., and Prag, A. J. N. W. (2005). “Neutron and X-ray characterisation of the metallurgical properties of a 7th century BC Corinthian-type bronze helmet,” Nucl. Instrum. Methods Phys. Res. B 239, 16–26.Google Scholar
Rietveld, H. M. (1967). “Line profiles of neutron powder-diffraction peaks for structure refinement,” Acta Crystallogr. 22, 151–152.Google Scholar
Rietveld, H. M. (1969). “A profile refinement method for nuclear and magnetic structures,” J. Appl. Crystallogr. 2, 65–71.Google Scholar
Schönenberger, J., Momose, T., Wagner, B., Leong, W. H., and Tarnawski, V. R. (2012). “Canadian field soils I. Mineral composition by XRD/XRF measurements,” Int. J. Thermophys. 33, 342–362.Google Scholar
Ufer, K., Roth, G., Kleeberg, R., Stanjek, H., Dohrmann, R., and Bergmann, J. (2004). “Description of X-ray powder pattern of turbostratically disordered layer structures with a Rietveld compatible approach,” Z. Kristallogr. 219, 519–527.Google Scholar
Vaniman, D. T., Bish, D., Guthrie, G., Chipera, S., Blake, D. E., Collins, S. A., Elliott, S. T., and Sarrazin, P. (1999). “Process monitoring and control with CHEMIN, a miniaturized CCD-based instrument for simultaneous XRD/XRF analysis,” Proc. SPIE Int. Soc. Opt. Eng. 3769, 243–251.Google Scholar