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Related Concept Videos

Preparation of Samples for Electron Microscopy01:20

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To be visualized by an electron microscope, either transmission or scanning, biological samples need to be fixed (stabilized) so the electron beam does not destroy them and dried thoroughly (desiccated/dehydrated) so the vacuum does not affect them. Fixation needs to be done as quickly as possible because the sample properties will start changing as soon as it is removed from its natural environment. For example, in a tissue sample, the oxygen levels begin decreasing, causing an altered...
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Related Experiment Video

Updated: Jul 12, 2025

Optimizing Sample Preparation for Cryogenic Electron Microscopy
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A Versatile and Reproducible Cryo-sample Preparation Methodology for Atom Probe Studies.

Eric V Woods1, Mahander P Singh1, Se-Ho Kim1

  • 1Mikrostrukturphysik und Legierungsdesign, Max-Planck-Institut für Eisenforschung GmbH, Max-Planck-Straße 1, Düsseldorf 40237, Germany.

Microscopy and Microanalysis : the Official Journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada
|October 19, 2023
PubMed
Summary

Preparing cryogenic specimens for atom probe tomography (APT) is now reliable. A new workflow with in situ capping layers improves data quality for diverse materials, especially battery cathodes.

Keywords:
atom probe tomographybattery cathodescryo-focused ion beamfrozen liquids

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Area of Science:

  • Materials Science
  • Analytical Chemistry
  • Nanotechnology

Background:

  • Cryogenic specimen preparation for atom probe tomography (APT) is difficult, hindering reliable analysis.
  • Existing protocols lack a generalized workflow for site-specific preparation and in situ capping.

Purpose of the Study:

  • To develop and validate a generalized workflow for cryogenic specimen preparation for APT.
  • To improve the success rate and data quality of APT analysis for challenging materials.

Main Methods:

  • Utilized focused ion beam (FIB) for site-specific lift-out of cryogenic specimens.
  • Implemented in situ deposition of metallic capping layers to strengthen and protect specimens.
  • Applied the workflow to various materials including metals, oxides, frozen liquids, and battery materials.

Main Results:

  • Demonstrated repeatable and reliable cryogenic specimen preparation across diverse material types.
  • Showcased significant improvement in APT data quality using in situ deposited metallic capping layers.
  • Successfully analyzed challenging battery cathode materials, mitigating delithiation issues during APT.

Conclusions:

  • The developed generalized workflow enhances the reliability and data quality of cryogenic APT analysis.
  • In situ capping layer deposition is crucial for analyzing high-stress and sensitive materials like battery cathodes.
  • The versatile workflow is transferable to various instruments and material systems.