Development of a liquid-helium free cryogenic sample holder with mK temperature control for autonomous electron microscopy

He, X.; Kostin, R.; Knight, E.; Han, M. G.; Mun, J.; Bozovic, I.; Jing, C.; Zhu, Y.

doi:10.1016/j.ultramic.2024.114037

Development of a liquid-helium free cryogenic sample holder with mK temperature control for autonomous electron microscopy

Journal Article · Sat Sep 07 00:00:00 EDT 2024 · Ultramicroscopy

DOI:https://doi.org/10.1016/j.ultramic.2024.114037· OSTI ID:2566987

^[1]; Kostin, R. ^[2]; Knight, E. ^[2]; Han, M. G. ^[1]; Mun, J. ^[1]; Bozovic, I. ^[1]; Jing, C. ^[2]; ^[1]

Brookhaven National Laboratory (BNL), Upton, NY (United States)
Euclid Techlabs LLC, Bolingbrook, IL (United States)

The automated and autonomous cryogenic transmission electron microscopy (Cryo-EM) demands a sample holder capable of maintaining temperatures below 10 K with precise control, long holding times, and minimal helium use. Rising to this challenge, we initiated an ambitious project to develop a novel closed-cycle cryocooler-based cryogenic sample holder that operates without the use of liquid helium and the consumption of gaseous helium. Here, this article presents the design, construction, and experimental testing of the initial prototype, which achieves an ultimate temperature of 5.6 K with exceptional stability close to 1mK, while providing a wide temperature control range from 295 K to 5.6 K, marking a clear advancement in cryo-EM holder development. While the prototype was not designed for atomic resolution imaging and thus lacks a sturdy support system to mitigate mechanical vibrations from the cryocooler's pulsed tube, this innovative approach successfully demonstrates proof of concept. It offers unprecedented capabilities for state-of-the-art cryogenic microscopy and microanalysis in materials and biological sciences.

View Accepted Manuscript (DOE)

Research Organization:: Brookhaven National Laboratory (BNL), Upton, NY (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division (MSE)

Grant/Contract Number:: SC0012704

OSTI ID:: 2566987

Report Number(s):: BNL--228185-2025-JAAM

Journal Information:: Ultramicroscopy, Journal Name: Ultramicroscopy Vol. 267; ISSN 0304-3991

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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Development of a liquid-helium free cryogenic sample holder with mK temperature control for autonomous electron microscopy

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