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Use of a miniature diamond-anvil cell in high-pressure single-crystal neutron Laue diffraction

The first high-pressure neutron diffraction study in a miniature diamond-anvil cell of a single crystal of size typical for X-ray diffraction is reported. This is made possible by modern Laue diffraction using a large solid-angle image-plate detector. An unexpected finding is that even reflections w...

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Autores principales: Binns, Jack, Kamenev, Konstantin V., McIntyre, Garry J., Moggach, Stephen A., Parsons, Simon
Formato: Online Artículo Texto
Lenguaje:English
Publicado: International Union of Crystallography 2016
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4856139/
https://www.ncbi.nlm.nih.gov/pubmed/27158503
http://dx.doi.org/10.1107/S2052252516000725
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author Binns, Jack
Kamenev, Konstantin V.
McIntyre, Garry J.
Moggach, Stephen A.
Parsons, Simon
author_facet Binns, Jack
Kamenev, Konstantin V.
McIntyre, Garry J.
Moggach, Stephen A.
Parsons, Simon
author_sort Binns, Jack
collection PubMed
description The first high-pressure neutron diffraction study in a miniature diamond-anvil cell of a single crystal of size typical for X-ray diffraction is reported. This is made possible by modern Laue diffraction using a large solid-angle image-plate detector. An unexpected finding is that even reflections whose diffracted beams pass through the cell body are reliably observed, albeit with some attenuation. The cell body does limit the range of usable incident angles, but the crystallographic completeness for a high-symmetry unit cell is only slightly less than for a data collection without the cell. Data collections for two sizes of hexamine single crystals, with and without the pressure cell, and at 300 and 150 K, show that sample size and temperature are the most important factors that influence data quality. Despite the smaller crystal size and dominant parasitic scattering from the diamond-anvil cell, the data collected allow a full anisotropic refinement of hexamine with bond lengths and angles that agree with literature data within experimental error. This technique is shown to be suitable for low-symmetry crystals, and in these cases the transmission of diffracted beams through the cell body results in much higher completeness values than are possible with X-rays. The way is now open for joint X-ray and neutron studies on the same sample under identical conditions.
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spelling pubmed-48561392016-05-06 Use of a miniature diamond-anvil cell in high-pressure single-crystal neutron Laue diffraction Binns, Jack Kamenev, Konstantin V. McIntyre, Garry J. Moggach, Stephen A. Parsons, Simon IUCrJ Research Papers The first high-pressure neutron diffraction study in a miniature diamond-anvil cell of a single crystal of size typical for X-ray diffraction is reported. This is made possible by modern Laue diffraction using a large solid-angle image-plate detector. An unexpected finding is that even reflections whose diffracted beams pass through the cell body are reliably observed, albeit with some attenuation. The cell body does limit the range of usable incident angles, but the crystallographic completeness for a high-symmetry unit cell is only slightly less than for a data collection without the cell. Data collections for two sizes of hexamine single crystals, with and without the pressure cell, and at 300 and 150 K, show that sample size and temperature are the most important factors that influence data quality. Despite the smaller crystal size and dominant parasitic scattering from the diamond-anvil cell, the data collected allow a full anisotropic refinement of hexamine with bond lengths and angles that agree with literature data within experimental error. This technique is shown to be suitable for low-symmetry crystals, and in these cases the transmission of diffracted beams through the cell body results in much higher completeness values than are possible with X-rays. The way is now open for joint X-ray and neutron studies on the same sample under identical conditions. International Union of Crystallography 2016-02-26 /pmc/articles/PMC4856139/ /pubmed/27158503 http://dx.doi.org/10.1107/S2052252516000725 Text en © Jack Binns et al. 2016 http://creativecommons.org/licenses/by/2.0/uk/ This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
spellingShingle Research Papers
Binns, Jack
Kamenev, Konstantin V.
McIntyre, Garry J.
Moggach, Stephen A.
Parsons, Simon
Use of a miniature diamond-anvil cell in high-pressure single-crystal neutron Laue diffraction
title Use of a miniature diamond-anvil cell in high-pressure single-crystal neutron Laue diffraction
title_full Use of a miniature diamond-anvil cell in high-pressure single-crystal neutron Laue diffraction
title_fullStr Use of a miniature diamond-anvil cell in high-pressure single-crystal neutron Laue diffraction
title_full_unstemmed Use of a miniature diamond-anvil cell in high-pressure single-crystal neutron Laue diffraction
title_short Use of a miniature diamond-anvil cell in high-pressure single-crystal neutron Laue diffraction
title_sort use of a miniature diamond-anvil cell in high-pressure single-crystal neutron laue diffraction
topic Research Papers
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4856139/
https://www.ncbi.nlm.nih.gov/pubmed/27158503
http://dx.doi.org/10.1107/S2052252516000725
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