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An in situ powder diffraction cell for high‐pressure hydrogenation experiments using laboratory X‐ray diffractometers
Author(s) -
Moury Romain,
Hauschild Klaus,
Kersten Wolfgang,
Ternieden Jan,
Felderhoff Michael,
Weidenthaler Claudia
Publication year - 2015
Publication title -
journal of applied crystallography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.429
H-Index - 162
ISSN - 1600-5767
DOI - 10.1107/s1600576714025692
Subject(s) - in situ , diffraction , powder diffraction , materials science , hydrogen , x ray crystallography , high pressure , hydrogen storage , analytical chemistry (journal) , chemical engineering , crystallography , chemistry , thermodynamics , optics , chromatography , organic chemistry , physics , engineering
An in situ diffraction cell is presented which has been designed and constructed for in‐house powder diffraction experiments under high gas pressures up to 30 MPa. For a proof of principle, the in situ cell has been tested for several hydrogenation experiments under elevated pressures and temperatures. LaNi 5 was chosen as an example for hydrogenation, applying simultaneously 5.5 MPa H 2 pressure at a temperature of 423 K. For testing the high‐pressure–temperature suitability of the in situ cell, pressure–temperature experiments up to 14 MPa at 373 K were performed, studying the rehydrogenation of NaH and Al to NaAlH 4 . The experimental setup enables recording of in situ X‐ray diffraction data on laboratory instruments with short data acquisition times at elevated hydrogen pressures and temperatures.