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Published in

International Union of Crystallography, Journal of Applied Crystallography, 1(49), p. 110-119, 2016

DOI: 10.1107/s1600576715022621

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Low-temperature powder X-ray diffraction measurements in vacuum: analysis of the thermal displacement of copper

This paper was not found in any repository, but could be made available legally by the author.
This paper was not found in any repository, but could be made available legally by the author.

Full text: Unavailable

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Preprint: archiving allowed
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Postprint: archiving allowed
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Published version: archiving allowed
Data provided by SHERPA/RoMEO

Abstract

A serious limitation of the all-in-vacuum diffractometer reported by Straasø, Dippel, Becker & Als-Nielsen [J. Synchrotron Rad.(2014),21, 119–126] has so far been the inability to cool samples to near-cryogenic temperatures during measurement. The problem is solved by placing the sample in a jet of helium gas cooled by liquid nitrogen. The resulting temperature change is quantified by determining the change in unit-cell parameter and atomic displacement parameter of copper. The cooling proved successful, with a resulting temperature of ∼95 (3) K. The measured powder X-ray diffraction data are of superb quality and high resolution [up to sinθ/λ = 2.2 Å−1], permitting an extensive modelling of the thermal displacement. The anharmonic displacement of copper was modelled by a Gram–Charlier expansion of the temperature factor. As expected, the corresponding probability distribution function shows an increased probability away from neighbouring atoms and a decreased probability towards them.