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A beryllium dome specimen holder for XRD analysis of air sensitive materials

Published online by Cambridge University Press:  29 February 2012

Mark A. Rodriguez ,
Timothy J. Boyle ,
Pin Yang  and
Damon L. Harris
Mark A. Rodriguez*
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185-1411
Timothy J. Boyle
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185-1411
Pin Yang
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185-1411
Damon L. Harris
Affiliation:
Brush Wellman Electrofusion Products, Fremont, California 94538-6346
*
a)Author to whom correspondence should be addressed. Electronic mail: marodri@sandia.gov
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Abstract

A specially designed specimen holder employing a beryllium dome has been fabricated for collection of X-ray diffraction (XRD) data from highly reactive materials. The specimen holder has a robust O-ring type seal (<10−9Torr) and no observed intensity artifacts in the 1° to 150° 2θ range. The design also minimizes specimen displacement errors and allows for analysis of both powders and bulk specimens (i.e., pellets). The simple design makes for straightforward assembly of the holder within the confines of a glove box. XRD analysis of hygroscopic LaBr3 powders collected with this holder are suitable for Rietveld structure refinement, yielding unit cell lattice parameters of a=7.9703(6) Å and c=4.5122(6) Å; cell volume=248.44(6) Å3; Rp=7.70%.

Keywords

berylliumreactiveair-sensitiveBeDXRD
Type
X-Ray Diffraction
Information
Powder Diffraction , Volume 23 , Issue 2 , June 2008 , pp. 121 - 124
Copyright
Copyright © Cambridge University Press 2008

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