A sapphire single-crystal cell for in situ neutron powder diffraction of solid-gas reactions

Add time:08/15/2019    Source:sciencedirect.com

Solid-gas reactions play an important role in many technologically important processes from ore smelting to hydrogen storage and the synthesis of functional materials. In situ investigations are very useful for unraveling basic steps of such reactions, rationalizing them and gaining control. For investigating time-resolved solid-gas reactions, we have constructed a gas pressure cell for elastic neutron diffraction. By proper orientation of a single-crystal sapphire tube as sample holder, Bragg peaks from the container material can be completely avoided, thus yielding high-quality powder diffraction data with very clean diffraction background. This enables the extraction of high precision crystal structure data as a function of gas pressure and temperature (laser heating) in time-resolved studies. The potential of the gas pressure cell is demonstrated by in situ studies of the reaction of solids with hydrogen, which yielded detailed models of the reaction pathways including high quality crystal structures of reaction intermediates and products. These were used to predict successfully the existence of further metal hydrides, to explain unusual bonding properties, and to optimize the synthesis of metastable compounds.

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