Crystal structure and formation of TlPd3 and its new hydride TlPd3H
Résumé
TlPd3 was synthesized from the elements in evacuated silica tubes at 600°C. Alternatively, TlPd3 was yielded by reduction of the TlPd3O4 in N2 gas atmosphere. Reduction of the oxide in H2 gas atmosphere resulted in the formation of the new hydride TlPd3H. The structure of tetragonal TlPd3 (ZrAl3 type, space group I 4/mmm, a = 410.659(9) pm, c = 1530.28(4) pm) was reinvestigated by X-ray and also by neutron powder diffraction as well as the structure of its previously unknown hydride TlPd3H (cubic anti-perovskite type structure, space group Pm-3m, a = 406.313(1) pm). In situ DSC measurements of TlPd3 in hydrogen gas atmosphere showed a broad exothermic signal over a wide temperature range with maxima at 280°C and another at 370°C resulting in TlPd3H as product. A dependency of lattice parameter of the intermetallic phase on reaction conditions is observed and discussed. Results of hydrogenation experiments at room temperature with gas pressure up to 280 bar hydrogen and at elevated temperatures with very low hydrogen gas pressures (1-2 bar) as well as results of dehydrogenation of the hydrides under vacuum will be discussed.
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