Abstract¶
Accessing and preparing representative cross-sections of complex, often beam-sensitive, heterogeneous systems for high-resolution electron microscopy presents a significant bottleneck for materials analysis. These challenges are compounded when multiphase systems (e.g., batteries) must be disassembled to enable nanoscale characterization, and critical interfacial information is likely to be lost. In this work, we detail the advanced methodology employing cryogenic ultra-short pulsed laser ablation in conjunction with plasma focused ion beam milling (cryo-Laser PFIB) that we developed in 2019 to overcome these challenges. While our previous work focused on outcomes of our efforts, here we will discuss in-depth the principles and optimization of this approach for obtaining 2D-area and 3D-volume characterization, combining rapid material removal by laser and precision PFIB polishing milling under cryogenic conditions. This combined technique minimizes artifacts that otherwise may result from sources like mechanical or thermal processing, preserving the delicate microstructures and interfaces that may be inherent in heterogeneous systems. Furthermore, we highlight recent technological developments in instrumentation and workflows that significantly enhance the capabilities and broaden the applicability of cryo-Laser PFIB beyond specific material types. By showcasing the potential of this evolved technique, we highlight it’s growing importance as a powerful tool for characterizing internal architectures and understanding structure-property relationships across a wide range of scientific and technological domains.
Competing Interests¶
The authors declare that they have no known competing interests.
Acknowledgments¶
Acknowledgements¶
This work was authored in part by the National Renewable Energy Laboratory (NREL) for the U.S. Department of Energy (DOE) under Contract No. DE-AC36-08GO28308. Support for this work was also provided by U.S. DOE Office of Energy Efficiency and Renewable Energy Vehicle Technologies Office Vehicle Technologies Office within the Earth-abundant Cathode Active Materials (EaCAM) consortium under Carine Steinway, Tien Duong, and Brian Cunningham, is gratefully acknowledged. This work was performed, in part, at the Center for Integrated Nanotechnologies, an Office of Science User Facility operated for the U.S. DOE Office of Science. Sandia National Laboratories is a multimission laboratory managed and operated by National Technology & Engineering Solutions of Sandia, LLC, a wholly owned subsidiary of Honeywell International, Inc., for the U.S. DOE’s National Nuclear Security Administration under contract DE-NA-0003525. This paper describes objective technical results and analysis. Any subjective views or opinions that might be expressed in the paper do not necessarily represent the views of the U.S. DOE or the United States Government. This article has been authored in part by an employee of National Technology & Engineering Solutions of Sandia, LLC under Contract No. DE-NA0003525 with the U.S. DOE. The employee owns all right, title and interest in and to the article and is solely responsible for its contents. The United States Government retains and the publisher, by accepting the article for publication, acknowledges that the United States Government retains a non-exclusive, paid-up, irrevocable, world-wide license to publish or reproduce the published form of this article or allow others to do so, for United States Government purposes. The DOE will provide public access to these results of federally sponsored research in accordance with the DOE Public Access Plan https://
This work was performed, in part, at the Center for Integrated Nanotechnologies, an Office of Science User Facility operated for the U.S. Department of Energy (DOE) Office of Science. Sandia National Laboratories is a multimission laboratory managed and operated by National Technology & Engineering Solutions of Sandia, LLC, a wholly owned subsidiary of Honeywell International, Inc., for the U.S. DOE’s National Nuclear Security Administration under contract DE-NA-0003525. This paper describes objective technical results and analysis. Any subjective views or opinions that might be expressed in the paper do not necessarily represent the views of the U.S. Department of Energy or the United States Government. This article has been authored in part by an employee of National Technology & Engineering Solutions of Sandia, LLC under Contract No. DE-NA0003525 with the U.S. Department of Energy (DOE). The employee owns all right, title and interest in and to the article and is solely responsible for its contents. The United States Government retains and the publisher, by accepting the article for publication, acknowledges that the United States Government retains a non-exclusive, paid-up, irrevocable, world-wide license to publish or reproduce the published form of this article or allow others to do so, for United States Government purposes. The DOE will provide public access to these results of federally sponsored research in accordance with the DOE Public Access Plan https://
The authors acknowledge that certain figures were adapted or reprinted with permission from “Formation Mechanisms and Structure of Interfaces in Materials Via Electron Microscopy Techniques” by Renae Gannon, 2022, University of Oregon. Copyright 2022 by Renae Gannon.
