Versatile in-situ powder X-ray diffraction cells for solid-gas investigations

Jensen, T.R.;Nielsen, T.K.;Filinchuk, Yaroslav;Jorgensen, J.E.;Webb, C.J.;et.al.
(2010) Journal of Applied Crystallography — Vol. 43, n° 6, p. 1456-1463 (2010)

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Authors
  • Jensen, T.R.autre
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  • Nielsen, T.K.autre
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  • Jorgensen, J.E.autre
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  • Webb, C.J.autre
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Abstract
This paper describes new sample cells and techniques for in situ powder X-ray diffraction specifically designed for gas absorption studies up to ca 300 bar (1 bar = 100 000 Pa) gas pressure. The cells are for multipurpose use, in particular the study of solid-gas reactions in dosing or flow mode, but can also handle samples involved in solid-liquid-gas studies. The sample can be loaded into a single-crystal sapphire (Al2O3) capillary, or a quartz (SiO2) capillary closed at one end. The advantages of a sapphire single-crystal cell with regard to rapid pressure cycling are discussed, and burst pressures are calculated and measured to be ~300 bar. An alternative and simpler cell based on a thin-walled silicate or quartz glass capillary, connected to a gas source via a VCR fitting, enables studies up to ~100 bar. Advantages of the two cell types are compared and their applications are illustrated by case studies.
Affiliations
  • ESRF, Grenoble (France)Chimie

Citations

Jensen, T. R., Nielsen, T. K., Filinchuk, Y., Jorgensen, J. E., Cerenius, Y., Gray, E. Mac. A., & Webb, C. J. (2010). Versatile in-situ powder X-ray diffraction cells for solid-gas investigations. Journal of Applied Crystallography, 43(6), 1456-1463. https://doi.org/10.1107/S0021889810038148 (Original work published 2010)