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Metal hydride formation in palladium and palladium rich intermetallic compounds studied by in situ neutron diffraction

Published online by Cambridge University Press:  14 November 2013

H. Kohlmann*
Affiliation:
Institute of Inorganic Chemistry, Leipzig University, Leipzig, Germany
N. Kurtzemann
Affiliation:
Institute of Inorganic Solid State Chemistry, Saarland University, Saarbrücken, Germany
T. C. Hansen
Affiliation:
Institut Laue-Langevin, Grenoble, France
*
*Correspondence author, holger.kohlmann@uni-leipzig.de, +49 341 97 36201

Abstract

In order to investigate the hydrogenation of intermetallic compounds, a gas pressure cell for in situ neutron powder diffraction based on a sapphire crystal tube was constructed. By proper orientation of the single crystal Bragg peaks of the container material can be avoided, resulting in a very low diffraction background. Using a laser heating and gas pressure controller, the hydrogenation (deuteration) of palladium and palladium rich intermetallics was studied in real time up to 8 MPa gas pressure and 700 K. Crystal structure parameters of palladium deuterides could be obtained under various deuterium gas pressures, corresponding to compositional ranges of 0.04≤x≤0.11 for the α-phase and 0.52≤x≤0.72 for the β-phase at 446 K. In situ neutron powder diffraction of the deuteration of a thallium lead palladium intermetallic Tl1-xPbxPd3 shows two superstructures of the cubic closest packing (ccp) to transform independently into a AuCu3 type structure. This proves a direct reaction to the deuterium filled AuCu3 type structure instead of a reaction cascade involving different ccp superstructures and thus gives new insights into the reaction pathways of palladium rich intermetallic compounds.

Type
Technical Articles
Copyright
Copyright © International Centre for Diffraction Data 2013 

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