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用于中子衍射的双壁蓝宝石单晶气压室(III型)。

A double-walled sapphire single-crystal gas-pressure cell (type III) for neutron diffraction.

作者信息

Finger Raphael, Hansen Thomas C, Kohlmann Holger

机构信息

Inorganic Chemistry, Leipzig University, Johanisallee 29, Leipzig, 04103, Germany.

Institut Laue-Langevin, 71 avenue des Martyrs, Grenoble, 38000, France.

出版信息

J Appl Crystallogr. 2022 Feb 1;55(Pt 1):67-73. doi: 10.1107/S1600576721012048.

DOI:10.1107/S1600576721012048
PMID:35145356
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC8805162/
Abstract

neutron diffraction is an important characterization technique for the investigation of many functional materials, for hydrogen uptake and release in hydrogen storage materials. A new sapphire single-crystal gas-pressure cell for elastic neutron scattering has been developed and evaluated; it allows conditions of 298 K and 9.5 MPa hydrogen pressure and 1110 K at ambient pressure. The pressure vessel consists of a sapphire single-crystal tube of 35 mm radius and a sapphire single-crystal crucible as sample holder. Heating is realized by two 100 W diode lasers. It is optimized for the D20 diffractometer, ILL, Grenoble, France, and requires the use of a radial oscillating collimator. Its advantages over earlier sapphire single-crystal gas-pressure cells are higher maximum temperatures and lower background at low and high diffraction angles. The deuterium uptake in palladium was followed for validation, proving the potential of the type-III gas-pressure cell for neutron diffraction on solid-gas reactions.

摘要

中子衍射是研究许多功能材料,特别是储氢材料中氢的吸收和释放的重要表征技术。一种用于弹性中子散射的新型蓝宝石单晶气压室已被开发和评估;它允许在298 K和9.5 MPa氢气压力以及常压下1110 K的条件下使用。该压力容器由半径为35 mm的蓝宝石单晶管和作为样品架的蓝宝石单晶坩埚组成。加热由两台100 W二极管激光器实现。它针对法国格勒诺布尔ILL的D20衍射仪进行了优化,并且需要使用径向振荡准直器。与早期的蓝宝石单晶气压室相比,它的优点是最高温度更高,在低衍射角和高衍射角下的背景更低。跟踪了钯中氘的吸收情况以进行验证,证明了III型气压室用于固体-气体反应中子衍射的潜力。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/443471e28eb0/j-55-00067-fig12.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/9762ef5c0038/j-55-00067-fig1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/5efcf1bf9a23/j-55-00067-fig2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/5bc90a2cc76f/j-55-00067-fig3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/2c63a2671df4/j-55-00067-fig4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/3aceee7ac315/j-55-00067-fig5.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/67109a6e6024/j-55-00067-fig6.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/82ad9ba594f8/j-55-00067-fig7.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/053e4a3c8fec/j-55-00067-fig8.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/6597665c1971/j-55-00067-fig9.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/a6fe6ed50fb0/j-55-00067-fig10.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/28ca91de8429/j-55-00067-fig11.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/443471e28eb0/j-55-00067-fig12.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/9762ef5c0038/j-55-00067-fig1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/5efcf1bf9a23/j-55-00067-fig2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/5bc90a2cc76f/j-55-00067-fig3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/2c63a2671df4/j-55-00067-fig4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/3aceee7ac315/j-55-00067-fig5.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/67109a6e6024/j-55-00067-fig6.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/82ad9ba594f8/j-55-00067-fig7.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/053e4a3c8fec/j-55-00067-fig8.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/6597665c1971/j-55-00067-fig9.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/a6fe6ed50fb0/j-55-00067-fig10.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/28ca91de8429/j-55-00067-fig11.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebc1/8805162/443471e28eb0/j-55-00067-fig12.jpg

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J Appl Crystallogr. 2021 May 25;54(Pt 3):839-846. doi: 10.1107/S1600576721002685. eCollection 2021 Jun 1.
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Real-time powder diffraction studies of energy materials under non-equilibrium conditions.非平衡条件下含能材料的实时粉末衍射研究
IUCrJ. 2017 Sep 1;4(Pt 5):540-554. doi: 10.1107/S2052252517010363.
3
In situ analyses for ion storage materials.用于离子存储材料的原位分析。
Chem Soc Rev. 2016 Oct 21;45(20):5717-5770. doi: 10.1039/c5cs00734h. Epub 2016 Jul 21.
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In-situ monitoring of the formation of crystalline solids.原位监测晶体固体的形成。
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