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Comparison of two standards for powder X-ray diffraction

Marek A. Kojdecki Witold Z. Mielcarek 1Krystyna Prociów 1Joanna B. Warycha 1

1. Electrotechnical Institute, Division of Electrotechnology and Materials Science (IEL), M. Skłodowskiej-Curie 55/61, Wrocław, Poland

Abstract

Instrumental line-profiles measured as parts of X-ray diffraction patterns may be interpreted as convolutions of instrumental line-profiles and pure line-profiles, containing information on crystalline microstructure of investigated materials. Instrumental line profiles are important for precision of powder X-ray diffraction analyses. They can be measured from a standard material of same composition as a studied material that consists of sufficiently big and unstrained crystallites to ensure negligible contribution to line-profiles from crystalline microstructure in comparison to contribution from all instrumental factors. Frequently such standard can be hardly obtained and some standard reference material should be used instead. This substitution makes necessary further numerical procedure for determining instrumental line-profiles corresponding to Bragg angles for a material under study. In this work two standard materials, lanthanum hexaboride and zinc oxide, are compared and possible source of little discrepancy between X-ray diffraction patterns from them is revealed. Lanthanum hexaboride (NIST SRM 660a) was supported by NIST (with certificate No MD20899, mean crystallite size of 8.8 µm and cubic unit cell parameter of 0.41569162 nm ± 0,00000097 nm). Zinc oxide powder was produced by crystallisation from vapour. The measurements were performed by using a powder diffractometer (DRON) in the Bragg-Brentano configuration with radius of 180 mm, equipped with a cobalt X-ray tube (BWS-29), emission slits of 2 mm, receiving slit of 0.5 mm and Soller slit of 2°30'. X-ray diffraction pattern were recorded in range 20°-164° 2θ in scanning mode with step of Δ2θ=0.01° and counting time 3sec/step. The line profiles from lanthanum hexaboride were described by using fundamental parameter approach [1] and from them the line profiles corresponding to Bragg angles from zinc oxide were computed and compared with those from zinc oxide. The crystalline structure of SRM 660a was accounted [2]. The conclusions will be presented.

[1] R.W. Cheary, A. Coelho: A fundamental parameter approach to X-ray line-profile fitting, J. Appl. Cryst. 25 (1992), 109-121.
[2] C.T. Chantler, N.A. Rae, C.Q. Tran: Accurate determination and correction of the lattice parameter of LaB6 (standard reference material 660) relative to that of Si (640b), J. Appl. Cryst. 40 (2007), 232-240.

 

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Presentation: Poster at 11th European Powder Diffraction Conference, Poster session, by Marek A. Kojdecki
See On-line Journal of 11th European Powder Diffraction Conference

Submitted: 2008-05-05 02:42
Revised:   2009-06-07 00:48