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The optimum standard specimen for X-ray diffraction line-profile analysis

Published online by Cambridge University Press:  10 January 2013

J. G. M. van Berkum ,
G. J. M. Sprong ,
Th. H. de Keijser ,
R. Delhez  and
E. J. Sonneveld
J. G. M. van Berkum
Affiliation:
Delft University of Technology, Laboratory of Materials Science, Rotterdamseweg 137, 2628 AL Delft, The Netherlands
G. J. M. Sprong
Affiliation:
Delft University of Technology, Laboratory of Materials Science, Rotterdamseweg 137, 2628 AL Delft, The Netherlands
Th. H. de Keijser
Affiliation:
Delft University of Technology, Laboratory of Materials Science, Rotterdamseweg 137, 2628 AL Delft, The Netherlands
R. Delhez
Affiliation:
Delft University of Technology, Laboratory of Materials Science, Rotterdamseweg 137, 2628 AL Delft, The Netherlands
E. J. Sonneveld
Affiliation:
TNO Plastics and Rubber Research Institute, P.O. Box 6031, 2600 JA Delft, The Netherlands
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Abstract

A perfect general purpose standard specimen for high accuracy line-profile analysis is shown to be an illusion. Balancing the partly contradictory requirements, an optimum standard specimen for a parafocusing diffractometer is developed. To obtain the optimum standard specimen, a 5–10 μm particle size fraction is taken from the NIST certified Si powder SRM640a, about 1.5 mg/cm2 of this powder is uniformly deposited on a (510) oriented Si single-crystal wafer and the assembly is heat treated for 2 h at 1273 K to remove lattice imperfections. All procedures necessary are precisely given, easily applicable, and reproducing. For the present standard specimens, the random errors due to crystal statistics are quantified and shown to be acceptable for spinning specimens; the systematic errors due to residual size and transparency broadening are determined semi-empirically and can be eliminated, if desired. Thus the proposed optimum standard specimen allows the determination of instrumental line profiles free from systematic errors and with random errors in the line width of the order of 0.001 °2θ, allowing a full use of the capacities of modern diffractometers and data evaluation procedures.

Keywords

powder diffractioninstrumental broadeningstandard specimenline-profile accuracycrystal statistics

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Type
Research Article
Information
Powder Diffraction , Volume 10 , Issue 2 , June 1995 , pp. 129 - 139
Copyright
Copyright © Cambridge University Press 1995

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