A gas-tight Cu K alpha x-ray transparent reaction chamber for high-temperature x-ray diffraction analyses of halide gas/solid reactions

The Review of Scientific Instruments
Samuel Shian, Kenneth H Sandhage

Abstract

An externally heated, x-ray transparent reaction chamber has been developed to enable the dynamic high temperature x-ray diffraction (HTXRD) analysis of a gas/solid [TiF(4)(g)/SiO(2)(s)] reaction involving a halide gas reactant formed at elevated temperatures (up to 350 degrees C) from a condensed source (TiF(4) powder) sealed within the chamber. The reaction chamber possessed x-ray transparent windows comprised of a thin (13 microm) internal layer of Al foil and a thicker (125 microm) external Kapton film. After sealing the SiO(2) specimens (diatom frustules or Stober spheres) above TiF(4) powder within the reaction chamber, the chamber was heated to a temperature in the range of 160-350 degrees C to allow for internal generation of TiF(4)(g). The TiF(4)(g) underwent a metathetic reaction with the SiO(2) specimen to yield a TiOF(2)(s) product. HTXRD analysis, using Cu K alpha x rays passed through the Kapton/Al windows of the chamber, was used to track the extent of SiO(2) consumption and/or TiOF(2) formation with time. The Al foil inner layer of the windows protected the Kapton film from chemical attack by TiF(4)(g), whereas the thicker, more transparent Kapton film provided the mechanical strength needed to contain this gas....Continue Reading

References

Sep 14, 1973·Science·R W Powell, Y S Touloukian

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Citations

Jan 30, 2016·Inorganic Chemistry·Claudio EvangelistiFabio Piccinelli

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Methods Mentioned

BETA
x-ray diffraction

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