In situ X-ray diffraction environments for high-pressure reactions

Publication: Research - peer-reviewJournal article

  • Bjarne R. S. Hansen
  • Kasper Trans Møller
  • Mark Paskevicius
  • Ann-Christin Dippel
  • Peter Walter
    Peter WalterDeutsches Elektronen-Synchrotron (DESY), 22607 HamburgGermany
  • Colin James Webb
    Colin James WebbGriffith UniversityAustralia
  • Claudio Pistidda
    Claudio PistiddaInstitute of Materials Research, Materials Technology, Helmholtz−Zentrum GeesthachtGermany
  • Nils Bergemann
    Nils BergemannInstitute of Materials Research, Helmholtz-Zentrum Geesthacht, D-21502 GeesthachtGermany
  • Martin Dornheim
    Martin DornheimInstitute of Materials Research, Materials Technology, Helmholtz−Zentrum GeesthachtGermany
  • Thomas Klassen
    Thomas KlassenInstitute of Materials Research, Materials Technology, Helmholtz−Zentrum GeesthachtGermany
  • Jens-Erik Jørgensen
  • Torben René Jensen
New sample environments and techniques specifically designed for in situ
powder X-ray diffraction studies up to 1000 bar (1 bar = 105 Pa) gas pressure are reported and discussed. The cells can be utilized for multiple purposes in a range of research fields. Specifically, investigations of gas–solid reactions and sample handling under inert conditions are undertaken here. Sample containers
allowing the introduction of gas from one or both ends are considered, enabling
the possibility of flow-through studies. Various containment materials are
evaluated, e.g. capillaries of single-crystal sapphire (Al2O3), quartz glass (SiO2),
stainless steel (S316) and glassy carbon (Sigradur K), and burst pressures are
calculated and tested for the different tube materials. In these studies, high
hydrogen pressure is generated with a metal hydride hydrogen compressor
mounted in a closed system, which allows reuse of the hydrogen gas. The
advantages and design considerations of the in situ cells are discussed and their
usage is illustrated by a case study.
Original languageEnglish
JournalJournal of Applied Crystallography
Volume48
Pages (from-to)1234-1241
Number of pages8
ISSN0021-8898
DOIs
StatePublished - 2015

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