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Lithium Self-Discharge and Its Prevention: Direct Visualization through In Situ Electrochemical Scanning Transmission Electron Microscopy

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    Lithium Self-Discharge and Its Prevention: Direct Visualization through In Situ Electrochemical Scanning Transmission Electron Microscopy
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    † § †Joint Center for Energy Storage Research, ‡Nanoscale Sciences, ⊥MESA Fabrication Operations, and §Center for Integrated Nanotechnologies, Sandia National Laboratories, Albuquerque, New Mexico 87123, United States
    ∥ Argonne National Laboratory, Lemont, Illinois 60439, United States
    # Energy & Environmental Directorate, Pacific Northwest National Laboratory, Richland, Washington 99352, United States
    *E-mail: [email protected]
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    ACS Nano

    Cite this: ACS Nano 2017, 11, 11, 11194–11205
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    https://doi.org/10.1021/acsnano.7b05513
    Published November 7, 2017
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    To understand the mechanism that controls low-aspect-ratio lithium deposition morphologies for Li-metal anodes in batteries, we conducted direct visualization of Li-metal deposition and stripping behavior through nanoscale in situ electrochemical scanning transmission electron microscopy (EC-STEM) and macroscale-cell electrochemistry experiments in a recently developed and promising solvate electrolyte, 4 M lithium bis(fluorosulfonyl)imide in 1,2-dimethoxyethane. In contrast to published coin cell studies in the same electrolyte, our experiments revealed low Coulombic efficiencies and inhomogeneous Li morphology during in situ observation. We conclude that this discrepancy in Coulombic efficiency and morphology of the Li deposits was dependent on the presence of a compressed lithium separator interface, as we have confirmed through macroscale (not in the transmission electron microscope) electrochemical experiments. Our data suggests that cell compression changed how the solid-electrolyte interphase formed, which is likely responsible for improved morphology and Coulombic efficiency with compression. Furthermore, during the in situ EC-STEM experiments, we observed direct evidence of nanoscale self-discharge in the solvate electrolyte (in the state of electrical isolation). This self-discharge was duplicated in the macroscale, but it was less severe with electrode compression, likely due to a more passivating and corrosion-resistant solid-electrolyte interphase formed in the presence of compression. By combining the solvate electrolyte with a protective LiAl0.3S coating, we show that the Li nucleation density increased during deposition, leading to improved morphological uniformity. Furthermore, self-discharge was suppressed during rest periods in the cycling profile with coatings present, as evidenced through EC-STEM and confirmed with coin cell data.

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    • Additional figures and discussion regarding the setup and electrochemistry related to Figures 2 and 4 are provided; additional details on image dose calculations, as well as scanning electron microscopy images and electrochemistry comparing Li deposition onto current collectors with and without LiAl0.3S films (PDF)

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    This article is cited by 59 publications.

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    Cite this: ACS Nano 2017, 11, 11, 11194–11205
    Click to copy citationCitation copied!
    https://doi.org/10.1021/acsnano.7b05513
    Published November 7, 2017
    Copyright © 2017 American Chemical Society
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