Ultralow-temperature cryogenic transmission electron microscopy using a new helium flow cryostat stage

Young Hoon Kim; Fehmi Sami Yasin; Na Yeon Kim; Max Birch; Xiuzhen Yu; Akiko Kikkawa; Yasujiro Taguchi; Jiaqiang Yan; Miaofang Chi

doi:10.1016/j.ultramic.2025.114263

Ultralow-temperature cryogenic transmission electron microscopy using a new helium flow cryostat stage

Young Hoon Kim
, Fehmi Sami Yasin
, Na Yeon Kim
, Max Birch
, Xiuzhen Yu
, Akiko Kikkawa
, Yasujiro Taguchi
, Jiaqiang Yan
, Miaofang Chi

Research output: Contribution to journal › Article › peer-review

Abstract

Advances in cryogenic electron microscopy have opened new avenues for probing quantum phenomena in correlated materials. This study reports the installation and performance of a new side-entry condenZero cryogenic cooling system for JEOL (Scanning) Transmission Electron Microscopes (S/TEM), utilizing compressed liquid helium (LHe) and designed for imaging and spectroscopy at ultra-low temperatures. The system includes an external dewar mounted on a vibration-damping stage and a pressurized, low-noise helium transfer line with a remotely controllable needle valve, ensuring stable and efficient LHe flow with minimal thermal and mechanical noise. Performance evaluation demonstrates a stable base temperature of 4.37 K measured using a Cernox bare chip sensor on the holder with temperature fluctuations within ±0.004 K. Complementary in-situ electron energy-loss spectroscopy (EELS) via aluminum bulk plasmon analysis was used to measure the local specimen temperature and validate cryogenic operation during experiments. The integration of cryogenic cooling with other microscopy techniques, including electron diffraction and Lorentz TEM, was demonstrated by resolving charge density wave (CDW) transitions in NbSe₂ using electron diffraction, and imaging nanometric magnetic skyrmions in MnSi via Lorentz TEM. This platform provides reliable cryogenic operation below 7 K, establishing a low-drift route for direct visualization of electronic and magnetic phase transformations in quantum materials.

Original language	English
Article number	114263
Journal	Ultramicroscopy
Volume	280
DOIs	https://doi.org/10.1016/j.ultramic.2025.114263
State	Published - Feb 2026

Funding

This work was supported by the U.S. Department of Energy, Office of Basic Energy Sciences, Division of Materials Sciences and Engineering . Microscopy technique development (Y.-H.K.) was partially supported by the U.S. BES, Early Career Research Program (KC040304-ERKCZ55). Experiments were performed at the Center for Nanophase Materials Sciences, a U.S. DOE Office of Science User Facility at Oak Ridge National Laboratory (ORNL). Research sponsored by the Laboratory Directed Research and Development Program of ORNL, managed by UT-Battelle, LLC, for the US DOE. X. Z. Y and Y. T acknowledge the support of the Japan Science and Technology Agency (JST) CREST program ( # JPMJCR20T1 ) and the RIKEN TRIP initiative . The authors thank CondenZero GmbH for their support and valuable discussions. Notice: This manuscript has been authored by UT-Battelle, LLC, under contract DE-AC05-00OR22725 with the US Department of Energy (DOE). The US government retains and the publisher, by accepting the article for publication, acknowledges that the US government retains a nonexclusive, paid-up, irrevocable, worldwide license to publish or reproduce the published form of this manuscript, or allow others to do so, for US government purposes. DOE will provide public access to these results of federally sponsored research in accordance with the DOE Public Access Plan ( https://www.energy.gov/doe-public-access-plan ).

Keywords

Charge density wave
Cryogenic S/TEM
Liquid helium
Side-entry
Skyrmion
Sub-7K

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10.1016/j.ultramic.2025.114263

Cite this

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title = "Ultralow-temperature cryogenic transmission electron microscopy using a new helium flow cryostat stage",

abstract = "Advances in cryogenic electron microscopy have opened new avenues for probing quantum phenomena in correlated materials. This study reports the installation and performance of a new side-entry condenZero cryogenic cooling system for JEOL (Scanning) Transmission Electron Microscopes (S/TEM), utilizing compressed liquid helium (LHe) and designed for imaging and spectroscopy at ultra-low temperatures. The system includes an external dewar mounted on a vibration-damping stage and a pressurized, low-noise helium transfer line with a remotely controllable needle valve, ensuring stable and efficient LHe flow with minimal thermal and mechanical noise. Performance evaluation demonstrates a stable base temperature of 4.37 K measured using a Cernox bare chip sensor on the holder with temperature fluctuations within ±0.004 K. Complementary in-situ electron energy-loss spectroscopy (EELS) via aluminum bulk plasmon analysis was used to measure the local specimen temperature and validate cryogenic operation during experiments. The integration of cryogenic cooling with other microscopy techniques, including electron diffraction and Lorentz TEM, was demonstrated by resolving charge density wave (CDW) transitions in NbSe2 using electron diffraction, and imaging nanometric magnetic skyrmions in MnSi via Lorentz TEM. This platform provides reliable cryogenic operation below 7 K, establishing a low-drift route for direct visualization of electronic and magnetic phase transformations in quantum materials.",

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AU - Yu, Xiuzhen

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AB - Advances in cryogenic electron microscopy have opened new avenues for probing quantum phenomena in correlated materials. This study reports the installation and performance of a new side-entry condenZero cryogenic cooling system for JEOL (Scanning) Transmission Electron Microscopes (S/TEM), utilizing compressed liquid helium (LHe) and designed for imaging and spectroscopy at ultra-low temperatures. The system includes an external dewar mounted on a vibration-damping stage and a pressurized, low-noise helium transfer line with a remotely controllable needle valve, ensuring stable and efficient LHe flow with minimal thermal and mechanical noise. Performance evaluation demonstrates a stable base temperature of 4.37 K measured using a Cernox bare chip sensor on the holder with temperature fluctuations within ±0.004 K. Complementary in-situ electron energy-loss spectroscopy (EELS) via aluminum bulk plasmon analysis was used to measure the local specimen temperature and validate cryogenic operation during experiments. The integration of cryogenic cooling with other microscopy techniques, including electron diffraction and Lorentz TEM, was demonstrated by resolving charge density wave (CDW) transitions in NbSe2 using electron diffraction, and imaging nanometric magnetic skyrmions in MnSi via Lorentz TEM. This platform provides reliable cryogenic operation below 7 K, establishing a low-drift route for direct visualization of electronic and magnetic phase transformations in quantum materials.

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Ultralow-temperature cryogenic transmission electron microscopy using a new helium flow cryostat stage

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