N2–O2 Icing in Single-Crystal In-House X-ray Diffraction Experiments Using an Open-Flow Helium Cryostat | Sciact - CRIS-система Института катализа

N2–O2 Icing in Single-Crystal In-House X-ray Diffraction Experiments Using an Open-Flow Helium Cryostat Научная публикация

Журнал

Journal of Applied Crystallography
ISSN: 0021-8898 , E-ISSN: 1600-5767

Вых. Данные

Год: 2021, Том: 54, Страницы: 1271-1275 Страниц : 5 DOI: 10.1107/S1600576721006440

Ключевые слова

helium open-flow cryostat; cryocrystallography; single-crystal X-ray diffraction; icing

Авторы

Zakharov Boris A. ^1,2 , Miletich Ronald ³ , Bogdanov Nikita E. ^1,2 , Boldyreva Elena V. ^1,2

Организации

1	Boreskov Institute of Catalysis, Siberian Branch of the Russian Academy of Sciences, Lavrentieva Avenue 5, Novosibirsk 630090, Russian Federation
2	Novosibirsk State University, Pirogova Street 2, Novosibirsk 630090, Russian Federation
3	Department of Mineralogy and Crystallography, University of Vienna, Althanstraße 14, Vienna A-1090, Austria

Информация о финансировании (3)

1	Министерство науки и высшего образования Российской Федерации (с 15 мая 2018)	0239-2021-0002
2	Universitat Wien	BE532003
3	FWF Austrian Science Fund	P 29149-N29

This note reports a study of the coating of a crystal with ‘ice’ at temperatures below 45 K during single-crystal in-house diffraction experiments when using an open-flow helium cryostat. The ‘ice’ consists mainly of crystalline oxygen and nitrogen. This suggests completely different techniques for avoiding this type of icing compared with water icing. With appropriate choices of crystal mount, crystal position with respect to the nozzle and gas flow conditions, it is possible to avoid detectable condensation. However, sometimes this can not be achieved in practice (poor diffraction from a smaller crystal, necessity of positioning the crystal in certain orientations to achieve desired data completeness, need to reduce helium consumption etc.). The problem of icing seems to be less common for powder experiments where the laminar gas flow is parallel to the capillary containing the sample, and for synchrotron experiments where the sample is comparably small and almost continuously rotated, which facilitates the ice covering being removed by the gas flow. This last technique can in principle also be applied to single-crystal X-ray diffraction using laboratory diffractometers – periodic rapid rotation of the crystal can help to minimize any icing, but this technique will not work when the condensation rate is comparable with or faster than one frame of data collection. The coating around a sample crystal not only reduces the quality of the diffraction data, but the temperature at the sample below the coating may also differ significantly from that at the cryostat nozzle reported by the instrument.

Zakharov B.A. , Miletich R. , Bogdanov N.E. , Boldyreva E.V.
N2–O2 Icing in Single-Crystal In-House X-ray Diffraction Experiments Using an Open-Flow Helium Cryostat
Journal of Applied Crystallography. 2021. V.54. P.1271-1275. DOI: 10.1107/S1600576721006440 WOS Scopus РИНЦ CAPlus OpenAlex

Поступила в редакцию:	12 мар. 2021 г.
Принята к публикации:	21 июн. 2021 г.
Опубликована online:	29 июл. 2021 г.
Опубликована в печати:	1 авг. 2021 г.

Web of science:	WOS:000683118400027
Scopus:	2-s2.0-85120962822
РИНЦ:	47541407
Chemical Abstracts:	2021:1771408
OpenAlex:	W3188806204

БД	Цитирований
Web of science	1
Scopus	1
РИНЦ	2
OpenAlex	1