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Title: Closed, heated reaction chamber design for dynamic high-temperature x-ray-diffraction analyses of gas/solid displacement reactions

Journal Article · · Review of Scientific Instruments
DOI:https://doi.org/10.1063/1.2136076· OSTI ID:20778494
; ; ;  [1]
  1. School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, Georgia 30350 (United States)

A closed, x-ray transparent chamber for containing a hot reactive gas (generated from an internal condensed source) has been designed and evaluated for use in dynamic x-ray-diffraction analysis of a gas/solid displacement reaction. The chamber consisted of a square-bottom base and lid machined from dense pyrolytic graphite. The base contained a flat pedestal, upon which SiO{sub 2} microshells (the reactant oxide) were placed, raised above adjacent cavities holding Mg flakes (the condensed precursor to the reactive gas). Upon heating to 650 deg. C, the Mg evaporated and reacted with the SiO{sub 2} inside the sealed chamber. By passing incident and diffracted x rays through the vertical side walls of the chamber and by blocking undesired graphite-diffracted x rays with platinum, the Mg(g)/SiO{sub 2}(s) displacement reaction could be tracked with time. This is the first use of dynamic high-temperature x-ray diffraction analysis to monitor the progress of a displacement reaction involving a reactant gas that was generated and confined within a closed reaction chamber.

OSTI ID:
20778494
Journal Information:
Review of Scientific Instruments, Vol. 76, Issue 12; Other Information: DOI: 10.1063/1.2136076; (c) 2005 American Institute of Physics; Country of input: International Atomic Energy Agency (IAEA); ISSN 0034-6748
Country of Publication:
United States
Language:
English