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Externally controlled pressure and temperature microreactor for in situ x-ray diffraction, visual and spectroscopic reaction investigations under supercritical and subcritical conditions

Rev. Sci. Instrum. 76, 015103 (2005); doi:10.1063/1.1831254

Published 20 December 2004

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Jason Diefenbacher, Michael McKelvy, and Andrew V.G. Chizmeshya
Center for Solid State Science, Arizona State University, Tempe, Arizona 85287-1704

George H. Wolf
Department of Chemistry and Biochemistry, Arizona State University, Tempe, Arizona 85287-1504
A microreactor has been developed for in situ, spectroscopic investigations of materials and reaction processes with full external pressure and temperature control from ambient conditions to 400 °C and 310 bar. The sample chamber is in direct contact with an external manifold, whereby gases, liquids or fluids can be injected and their activities controlled prior to and under investigation conditions. The microreactor employs high strength, single crystal moissanite windows which allow direct probe beam interaction with a sample to investigate in situ reaction processes and other materials properties. The relatively large volume of the cell, along with full optical accessibility and external temperature and pressure control, make this reaction cell well suited for experimental investigations involving any combination of gas, fluid, and solid interactions. The microreactor's capabilities are demonstrated through an in situ x-ray diffraction study of the conversion of a meta-serpentine sample to magnesite under high pressure and temperature. Serpentine is one of the mineral candidates for the implementation of mineral carbonation, an intriguing carbon sequestration candidate technology. ©2005 American Institute of Physics
History: Received 16 September 2004; accepted 11 October 2004; published 20 December 2004
Permalink: http://link.aip.org/link/?RSINAK/76/015103/1
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KEYWORDS and PACS

Keywords
PACS
  • 07.10.Cm
    Micromechanical devices and systems
  • 07.05.Dz
    Control systems in physics
  • 07.85.Nc
    X-ray and gamma-ray spectrometers
  • 61.10.Nz
    X-ray diffraction
  • 07.35.+k
    High-pressure apparatus; shock tubes; diamond anvil cells
  • 07.20.Ka
    High-temperature instrumentation; pyrometers
  • 82.40.-g
    Chemical kinetics and reactions: special regimes and techniques
  • YEAR: 2005

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PUBLICATION DATA

ISSN:
0034-6748 (print)   1089-7623 (online)
Publisher:
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