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Review of Scientific Instruments / Volume 76 / Issue 12 / NOTES

Rev. Sci. Instrum. 76, 126101 (2005); http://dx.doi.org/10.1063/1.2136076 (4 pages)

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

Michael S. Haluska1, Robert L. Snyder1, Kenneth H. Sandhage1, and Scott T. Misture2

1School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, Georgia 30350
2New York State College of Ceramics at Alfred University, Alfred, New York 14802

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(Received 6 June 2005; accepted 1 August 2005; published online 14 December 2005)

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 SiO2 microshells (the reactant oxide) were placed, raised above adjacent cavities holding Mg flakes (the condensed precursor to the reactive gas). Upon heating to 650 °C, the Mg evaporated and reacted with the SiO2 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)/SiO2(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.

© 2005 American Institute of Physics

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KEYWORDS and PACS

Keywords

magnesium, reaction kinetics, oxidation, reduction (chemical), chemical exchanges, X-ray chemical analysis, silicon compounds, X-ray diffraction

PACS

  • 82.40.-g

    Chemical kinetics and reactions: special regimes and techniques

  • 82.30.Hk

    Chemical exchanges (substitution, atom transfer, abstraction, disproportionation, and group exchange)

  • 82.20.-w

    Chemical kinetics and dynamics

  • 82.80.Ej

    X-ray, Mössbauer, and other γ-ray spectroscopic analysis methods

ARTICLE DATA

Digital Object Identifier
http://dx.doi.org/10.1063/1.2136076

PUBLICATION DATA

ISSN

0034-6748 (print)  
1089-7623 (online)

Publisher

$abstract.society.value is a Member of CrossRef American Institute of Physics

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