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Updated: Sep 14, 2025
06:32
Optimizing Sample Preparation for Cryogenic Electron Microscopy
Published on: April 11, 2025
597
Look What You Made Me Glue: SEMGlu™ Enabled Alternative Cryogenic Sample Preparation Process for Cryogenic Atom Probe
Neil Mulcahy1, James O Douglas1, Michele Shelly Conroy1
1Department of Materials, London Centre of Nanotechnology, Imperial Henry Royce Institute, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2AZ, UK.
Summary
This study introduces a new cryogenic workflow for atom probe tomography sample preparation using SEMGlu™, an electron beam curing adhesive. This method simplifies cryo-lift-out and mounting, enabling analysis of challenging samples.
Area of Science:
- Materials Science
- Analytical Chemistry
- Microscopy
Background:
- Cryogenic sample preparation for atom probe tomography (APT) is challenging, especially for site-specific lift-out without gas injection systems (GIS).
- Existing GIS-free workflows often rely on redeposition techniques, but cryogenic GIS use can cause deposition issues.
- Developing robust and accessible cryogenic sample preparation methods is crucial for advanced materials analysis.
Purpose of the Study:
- To present a novel, GIS-free workflow for cryogenic sample preparation for APT.
- To demonstrate the utility of SEMGlu™, an electron beam curing adhesive, for cryogenic lift-out and mounting.
- To enable APT analysis of challenging samples, including beam-sensitive and complex geometries, under cryogenic conditions.
Main Methods:
- Utilized SEMGlu™, a cryogenic-compatible electron beam curing adhesive, for sample lift-out and mounting.
- Developed a GIS-free redeposition welding technique for cryogenic sample preparation.
- Prepared silicon samples using the new workflow for both laser pulsing and voltage mode APT analysis.
Main Results:
- Successfully prepared and analyzed silicon samples using the SEMGlu™-based cryogenic workflow.
- Achieved comparable analytical performance to conventional presharpened microtip coupons.
- Demonstrated the workflow's applicability for correlative liquid cell transmission electron microscopy (LC-TEM) and cryogenic APT.
Conclusions:
- The SEMGlu™-based workflow offers an effective alternative for GIS-free cryogenic sample preparation in APT.
- This method is particularly advantageous for beam-sensitive samples, easily milled materials, and samples with intricate geometries.
- The workflow facilitates advanced correlative microscopy techniques involving cryogenic APT.
