Nanoscale Elemental Mapping of Intact Solid-Liquid Interfaces and Reactive Materials in Energy Devices Enabled by Cryo-FIB/SEM

Michael Zachman, Zhengyuan Tu, Lynden A. Archer, Lena F. Kourkoutis

Research output: Contribution to journalArticlepeer-review

26 Scopus citations


Many modern energy devices rely on solid-liquid interfaces, highly reactive materials, or both, for their operation and performance. The difficulty of characterizing such materials means these devices often lack high-resolution characterization in an unaltered state. Here, we demonstrate how cryogenic sample preparation and transfer can extend the capabilities of FIB/SEM techniques to the solid-liquid interfaces and reactive materials common to energy devices by preserving their integrity through all stages of preparation and characterization. We additionally show how cryo-FIB/SEM paired with energy dispersive X-ray spectroscopy enables nanoscale elemental mapping of cross-sections produced in these materials and discuss strategies to achieve optimal results. Finally, we consider current limitations of the technique and propose future developments that could enhance its capabilities. Our results illustrate that cryo-FIB/SEM will be a useful technique for fields where solid-liquid interfaces or reactive materials play an important role and could, thus far, not be characterized at high resolution.
Original languageEnglish (US)
Pages (from-to)1224-1232
Number of pages9
JournalACS Energy Letters
StatePublished - Mar 16 2020
Externally publishedYes

Bibliographical note

KAUST Repository Item: Exported on 2020-10-01
Acknowledged KAUST grant number(s): KUS-C1-018-02
Acknowledgements: We would like to thank Colin Heikes, Julia A. Mundy, Zhe Wang and Darrel G. Schlom for providing the oxide sample, and John Grazul for his assistance with the method for preparing theaqueous solution droplets. M.J.Z. and L.F.K. acknowledge support by the NSF (DMR-1654596), the Center for Alkaline-Based Energy Solutions (CABES), part of the Energy Frontier Research Center (EFRC) program supported by the U.S. Department of Energy, under grant DE-SC0019445, and the Packard Foundation. This work made use of the Cornell Center for Materials Research (CCMR) Shared Facilities with funding from the NSF MRSEC program (DMR1719875). Additional support for the FIB/SEM cryo-stage and transfer system was provided by the Kavli Institute at Cornell and the Energy Materials Center at Cornell, DOE EFRC BES (DESC0001086). The work also made use of electrochemical characterization facilities in the KAUSTCU Center for Energy and Sustainability, supported by the King Abdullah University of Science and Technology (KAUST) through Award # KUS-C1-018-02.
This publication acknowledges KAUST support, but has no KAUST affiliated authors.


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