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用于自主电子显微镜的具有毫开尔文温度控制的无液氦低温样品架的研制。

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

作者信息

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

机构信息

Condensed Matter Physics and Material Science Department, Brookhaven National Laboratory, Upton, NY 11973, USA.

Euclid Techlabs LLC, 365 Remington Blvd., Bolingbrook, IL 60440, USA.

出版信息

Ultramicroscopy. 2024 Dec;267:114037. doi: 10.1016/j.ultramic.2024.114037. Epub 2024 Sep 7.

DOI:10.1016/j.ultramic.2024.114037
PMID:39378698
Abstract

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. 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.

摘要

自动化和自主式低温透射电子显微镜(Cryo-EM)需要一个能够精确控制温度、长时间保持低温且氦气使用量最少的样品架,样品架需能将温度维持在10 K以下。为应对这一挑战,我们启动了一个雄心勃勃的项目,旨在开发一种基于新型闭环低温制冷机的低温样品架,该样品架无需使用液氦和气态氦的消耗。本文介绍了初始原型的设计、构造和实验测试,该原型实现了5.6 K的极限温度,具有接近1 mK的卓越稳定性,同时提供从295 K到5.6 K的宽温度控制范围,标志着低温电子显微镜样品架开发取得了明显进展。虽然该原型并非为原子分辨率成像而设计,因此缺乏一个坚固的支撑系统来减轻低温制冷机脉冲管产生的机械振动,但这种创新方法成功地证明了概念。它为材料和生物科学中的先进低温显微镜和微分析提供了前所未有的能力。

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