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Title: Diffraction studies of order-disorder at high pressures and temperatures

Journal Article · · Powder Diffraction
DOI:https://doi.org/10.1154/1.1913715· OSTI ID:1008686

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(CO{sub 3}){sub 2}) that tends to calcine at high temperatures, and Fe-containing materials, such as the spinel MgFe{sub 2}O{sub 4}, 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 CaSO{sub 4} 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 AgMnO{sub 4}-type structure.

Research Organization:
Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
Sponsoring Organization:
USDOE
OSTI ID:
1008686
Journal Information:
Powder Diffraction, Vol. 20, Issue (2) ; 06, 2005; ISSN 0885-7156
Country of Publication:
United States
Language:
ENGLISH