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Diffraction studies of order–disorder at high pressures and temperatures

Published online by Cambridge University Press:  01 March 2012

John B. Parise,
Sytle M. Antao,
Charles D. Martin and
Wilson Crichton
John B. Parise*
Affiliation:
Department of Geosciences and Mineral Physics Institute and Department Chemistry, State University of New York, Stony Brook, New York 11794-2100
Sytle M. Antao
Affiliation:
Department of Geosciences and Mineral Physics Institute, State University of New York, Stony Brook, New York 11794-2100
Charles D. Martin
Affiliation:
Department of Geosciences and Mineral Physics Institute, State University of New York, Stony Brook, New York 11794-2100
Wilson Crichton
Affiliation:
European Synchrotron Radiation Facility, B.P. 220, F-38043 Grenoble, France
*
a)Author to whom correspondence should be addressed. Electronic mail: john.parise@sunysb.edu
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Abstract

Recent developments at synchrotron X-ray beamlines now allow collection of data suitable for structure determination and Rietveld structure refinement at high pressures and temperatures on challenging materials. These include materials, such as dolomite(CaMg(CO3)2) that tends to calcine at high temperatures, and Fe-containing materials, such as the spinel MgFe2O4, which tend to undergo changes in oxidation state. Careful consideration of encapsulation along with the use of radial collimation produced powder diffraction patterns virtually free of parasitic scattering from the cell in the case of large volume high-pressure experiments. These features have been used to study a number of phase transitions, especially those where superior signal-to-noise discrimination is required to distinguish weak ordering reflections. The structures adopted by dolomite, and CaSO4, anhydrite, were determined from 298 to 1466 K at high pressures. Using laser-heated diamond-anvil cells to achieve simultaneous high pressure and temperature conditions, we have observed CaSO4 undergo phase transitions to the monazite type and at highest pressure and temperature to crystallize in the barite-type structure. On cooling, the barite structure distorts, from an orthorhombic to a monoclinic lattice, to produce the AgMnO4-type structure.

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Read Hot X-Rays
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Powder Diffraction , Volume 20 , Issue 2 , June 2005, pp. 80 - 86
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Copyright © Cambridge University Press 2005

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