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

Jensen, Torben R.; Nielsen, Thomas K.; Filinchuk, Yaroslav; Jorgensen, Jens-Erik; Cerenius, Yngve LU ; Gray, Evan MacA and Webb, Colin J. (2010) In Journal of Applied Crystallography 43. p.1456-1463
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 similar to 300 bar. An alternative and simpler cell based on a thin-walled silicate or quartz glass... (More)
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 similar to 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 similar to 100 bar. Advantages of the two cell types are compared and their applications are illustrated by case studies. (Less)
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author
organization
publishing date
type
Contribution to journal
publication status
published
subject
keywords
solid-gas reactions, powder X-ray diffraction, X-ray diffraction cells, hydrogen absorption
in
Journal of Applied Crystallography
volume
43
pages
1456 - 1463
publisher
Wiley-Blackwell
external identifiers
  • wos:000284550900022
  • scopus:78649498419
ISSN
1600-5767
DOI
10.1107/S0021889810038148
language
English
LU publication?
yes
id
c780ede7-e94b-4133-8aee-f2164a50c12e (old id 1773745)
date added to LUP
2011-02-02 11:24:18
date last changed
2018-06-24 03:02:34
@article{c780ede7-e94b-4133-8aee-f2164a50c12e,
  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 similar to 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 similar to 100 bar. Advantages of the two cell types are compared and their applications are illustrated by case studies.},
  author       = {Jensen, Torben R. and Nielsen, Thomas K. and Filinchuk, Yaroslav and Jorgensen, Jens-Erik and Cerenius, Yngve and Gray, Evan MacA and Webb, Colin J.},
  issn         = {1600-5767},
  keyword      = {solid-gas reactions,powder X-ray diffraction,X-ray diffraction cells,hydrogen absorption},
  language     = {eng},
  pages        = {1456--1463},
  publisher    = {Wiley-Blackwell},
  series       = {Journal of Applied Crystallography},
  title        = {Versatile in situ powder X-ray diffraction cells for solid-gas investigations},
  url          = {http://dx.doi.org/10.1107/S0021889810038148},
  volume       = {43},
  year         = {2010},
}