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Miniaturization of mechanical milling for powder X-ray diffraction

Published online by Cambridge University Press:  17 August 2012

Andrew J. Locock ,
David Chesterman ,
Diane Caird  and
M. John M. Duke
Andrew J. Locock*
Affiliation:
Department of Earth and Atmospheric Sciences, University of Alberta, Edmonton, Alberta T6G 2E3, Canada
David Chesterman
Affiliation:
Department of Earth and Atmospheric Sciences, University of Alberta, Edmonton, Alberta T6G 2E3, Canada
Diane Caird
Affiliation:
Department of Earth and Atmospheric Sciences, University of Alberta, Edmonton, Alberta T6G 2E3, Canada
M. John M. Duke
Affiliation:
SLOWPOKE Nuclear Reactor Facility, University of Alberta, Edmonton, Alberta T6G 2N8, Canada
*
a)Author to whom correspondence should be addressed. Electronic mail: alocock@ualberta.ca
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Abstract

To enable mechanical milling of small (0.1–1.0 g) samples, a cylindrical grinding vessel machined from polypropylene and furnished with tungsten carbide rods has been designed and produced for use inside the conventional jar of a McCrone Micronizing Mill. The vessel is about one-seventh the volume of the conventional jar supplied by the manufacturer. The conditions of milling for both the conventional and the miniaturized-grinding assemblies were tested using quartz sand as a limiting case. The median grain sizes of the resultant powders were measured by an X-ray gravitational-sedimentation method, with contamination from the grinding media measured by Rietveld refinement and by instrumental neutron activation analysis. The use of tungsten carbide grinding elements permits rapid wet milling of a small sample to the same median grain size in about one-third of the time required by a regular sample ground in corundum. The relative contamination (by tungsten carbide on a weight basis) using the miniaturized-grinding assembly is about 6(1)% of the proportion of corundum contamination yielded by the conventional grinding assembly.

Keywords

grain sizeminiaturizationmicronizingmillingtungsten carbide
Type
Technical Articles
Information
Powder Diffraction , Volume 27 , Issue 3 , September 2012 , pp. 189 - 193
Copyright
Copyright © International Centre for Diffraction Data 2012

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