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Accurate fully automated powder diffraction data using zero-background sample holders

Published online by Cambridge University Press:  10 January 2013

S. T. Misture ,
L. R. Chatfield  and
R. L. Snyder
S. T. Misture
Affiliation:
Institute for Ceramic Superconductivity, New York State College of Ceramics atAlfred University, Alfred, New York 14802
L. R. Chatfield
Affiliation:
Institute for Ceramic Superconductivity, New York State College of Ceramics atAlfred University, Alfred, New York 14802
R. L. Snyder
Affiliation:
Institute for Ceramic Superconductivity, New York State College of Ceramics atAlfred University, Alfred, New York 14802
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Abstract

An increasingly frequent used sample holder, the zero-background holder (ZBH), is evaluated for use in external standard calibration of powder patterns. The effectiveness of the ZBH calibration method is determined by comparison to the conventional internal- and external-standard calibration techniques. The three calibration methods are compared using the results of lattice parameter refinements of test powders, using Si as the standard. Several test materials were used in the evaluation which cover a wide range of absorption coefficients so sample transparency effects can be distinguished from sample displacement effects. Results of the calibrations clearly indicate that the ZBH method gives precision and accuracy comparable to the internal-standard method, and significantly better than the external-standard technique. In addition, the ZBH method yields substantially better results than the internal-standard method for materials with low absorption coefficients. Low-angle calibrations are also made on a ZBH using a proposed standard, silver behenate, which has peaks from 1.5° to 20° 2θ. These calibrations have shown that if care is not taken to establish a monolayer of powder on the ZBH crystal, significant errors in refined lattice parameters will result.

Type
Research Article
Information
Powder Diffraction , Volume 9 , Issue 3 , September 1994 , pp. 172 - 179
Copyright
Copyright © Cambridge University Press 1994

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