Operando Freezing Cryogenic Electron Microscopy of Active Battery Materials

Dutta, Nikita S.; Carroll, Gerard Michael; Neale, Nathan R.; Han, Sang-Don; Al-Jassim, Mowafak; Jungjohann, Katherine

doi:10.1093/mam/ozae097

Title: Operando Freezing Cryogenic Electron Microscopy of Active Battery Materials

Journal Article · 07 October 2024 · Microscopy and Microanalysis

DOI: https://doi.org/10.1093/mam/ozae097 · OSTI ID:2459368

; Carroll, Gerard Michael; Neale, Nathan R.;

; Al-Jassim, Mowafak; Jungjohann, Katherine

Abstract Understanding structural and chemical evolution of battery materials during operation is critical to achieving safe, efficient, and long-lasting energy storage. Cryogenic electron microscopy (cryo-EM) has become a valuable tool in battery characterization, leveraging low temperatures to improve stability of sensitive materials under electron beam irradiation. However, typical cryo-EM sample preparations leave extended time between the electrochemical point of interest and ex situ freezing of samples, during which active structures may relax, degrade, or otherwise evolve. Here, we detail a method for operando freezing cryo-EM to preserve and characterize native electrode and interfacial structures that arise during battery cycling, based on an operando plunge freezer and cold sample removal process. We validate the method on multiple electrode materials and quantify and discuss the freezing rate achieved. Operando freezing cryo-EM can be used to directly visualize transient features that arise at active electrochemical interfaces, to enable deeper understanding of structural evolution and interfacial chemistry in batteries and other electrochemical systems.

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Sponsoring Organization:: USDOE

Grant/Contract Number:: 89233218CNA000001; NA0003525

OSTI ID:: 2459368

Journal Information:: Microscopy and Microanalysis, Journal Name: Microscopy and Microanalysis Journal Issue: 5 Vol. 30; ISSN 1431-9276

Publisher:: Oxford University PressCopyright Statement

Country of Publication:: United States

Language:: English

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