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Reducing the background of ultra-low-temperature X-ray diffraction data through new methods and advanced materials

Lookup NU author(s): Dr Charlie McMonagleORCiD, Professor Mike ProbertORCiD

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This work is licensed under a Creative Commons Attribution 4.0 International License (CC BY 4.0).

Abstract

New methods and advanced materials that significantly reduce the background when collecting single-crystal X-ray diffraction data at ultra-low temperatures using a closed-cycle helium refrigerator are presented here. These include a magnetically controlled internal beamstop and a separate internal collimator that together completely remove the scattering contribution to the background from the beryllium vacuum chamber. Additionally, a new radiation shield made from flexible graphite significantly reduces the background and maintains excellent thermal properties. In combination these improvements have led to a sixfold reduction in the average intensity and a 15-fold reduction in peak intensity of the background observed for diffraction experiments conducted with a closed-cycle helium refrigerator. Moreover, access to ultra-low base temperatures, 2.05 K, has been maintained. The design and implementation of these methods are discussed along with a case study of vitamin C to demonstrate the effectiveness of the improvements.

Publication metadata

Author(s): McMonagle CJ, Probert MR

Publication type: Article

Publication status: Published

Journal: Journal of Applied Crystallography

Year: 2019

Volume: 52

Issue: 2

Pages: 445-450

Print publication date: 01/04/2019

Acceptance date: 28/02/2019

Date deposited: 24/04/2019

ISSN (print): 0021-8898

ISSN (electronic): 1600-5767

Publisher: Wiley-Blackwell

URL: https://doi.org/10.1107/S1600576719003078

DOI: 10.1107/S1600576719003078

Notes: Gold Open Access

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