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    Toward Unraveling the Origin of Lithium Fluoride in the Solid Electrolyte Interphase
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    • Chuntian Cao
      Chuntian Cao
      SSRL Materials Science Division, SLAC National Accelerator Laboratory, Menlo Park, California 94025, United States
      Department of Chemical and Biological Engineering, University of Colorado Boulder, Boulder, Colorado 80309, Untied States
      University of Colorado Boulder, Joint Center for Energy Storage Research (JCESR), Boulder, Colorado 80309, United States
      SLAC National Accelerator Laboratory, Joint Center for Energy Storage Research (JCESR), Menlo Park, California 94025, United States
      More by Chuntian Cao
    • Travis P. Pollard
      Travis P. Pollard
      Battery Science Branch, Sensor and Electron Devices Directorate, U.S. Army Research Laboratory, Adelphi, Maryland 20783, United States
      U.S. Army Research Laboratory, Joint Center for Energy Storage Research (JCESR), Adelphi, Maryland 20783, United States
      More by Travis P. Pollard
    • Oleg Borodin
      Oleg Borodin
      Battery Science Branch, Sensor and Electron Devices Directorate, U.S. Army Research Laboratory, Adelphi, Maryland 20783, United States
      U.S. Army Research Laboratory, Joint Center for Energy Storage Research (JCESR), Adelphi, Maryland 20783, United States
      More by Oleg Borodin
      Orcidhttps://orcid.org/0000-0002-9428-5291
    • Julian E. Mars
      Julian E. Mars
      SSRL Materials Science Division, SLAC National Accelerator Laboratory, Menlo Park, California 94025, United States
      Department of Chemical and Biological Engineering, University of Colorado Boulder, Boulder, Colorado 80309, Untied States
      University of Colorado Boulder, Joint Center for Energy Storage Research (JCESR), Boulder, Colorado 80309, United States
      SLAC National Accelerator Laboratory, Joint Center for Energy Storage Research (JCESR), Menlo Park, California 94025, United States
      More by Julian E. Mars
    • Yuchi Tsao
      Yuchi Tsao
      Department of Chemistry, Stanford University, Stanford, California 94305, United States
      More by Yuchi Tsao
    • Maria R. Lukatskaya
      Maria R. Lukatskaya
      SSRL Materials Science Division, SLAC National Accelerator Laboratory, Menlo Park, California 94025, United States
      SLAC National Accelerator Laboratory, Joint Center for Energy Storage Research (JCESR), Menlo Park, California 94025, United States
      Department of Mechanical and Process Engineering, ETH Zürich, 8092 Zürich, Switzerland
      More by Maria R. Lukatskaya
      Orcidhttps://orcid.org/0000-0002-2794-4322
    • Robert M. Kasse
      Robert M. Kasse
      SSRL Materials Science Division, SLAC National Accelerator Laboratory, Menlo Park, California 94025, United States
      Department of Materials Science and Engineering, Stanford University, Stanford, California 94305, United States
      More by Robert M. Kasse
    • Marshall A. Schroeder
      Marshall A. Schroeder
      Battery Science Branch, Sensor and Electron Devices Directorate, U.S. Army Research Laboratory, Adelphi, Maryland 20783, United States
      U.S. Army Research Laboratory, Joint Center for Energy Storage Research (JCESR), Adelphi, Maryland 20783, United States
      More by Marshall A. Schroeder
    • Kang Xu
      Kang Xu
      Battery Science Branch, Sensor and Electron Devices Directorate, U.S. Army Research Laboratory, Adelphi, Maryland 20783, United States
      U.S. Army Research Laboratory, Joint Center for Energy Storage Research (JCESR), Adelphi, Maryland 20783, United States
      More by Kang Xu
    • Michael F. Toney*
      Michael F. Toney
      SSRL Materials Science Division, SLAC National Accelerator Laboratory, Menlo Park, California 94025, United States
      Department of Chemical and Biological Engineering, University of Colorado Boulder, Boulder, Colorado 80309, Untied States
      University of Colorado Boulder, Joint Center for Energy Storage Research (JCESR), Boulder, Colorado 80309, United States
      SLAC National Accelerator Laboratory, Joint Center for Energy Storage Research (JCESR), Menlo Park, California 94025, United States
      *Email: [email protected]
      More by Michael F. Toney
      Orcidhttps://orcid.org/0000-0002-7513-1166
    • Hans-Georg Steinrück*
      Hans-Georg Steinrück
      SSRL Materials Science Division, SLAC National Accelerator Laboratory, Menlo Park, California 94025, United States
      SLAC National Accelerator Laboratory, Joint Center for Energy Storage Research (JCESR), Menlo Park, California 94025, United States
      Department Chemie, Universität Paderborn, 33098 Paderborn, Germany
      *Email: [email protected]
      More by Hans-Georg Steinrück
      Orcidhttps://orcid.org/0000-0001-6373-0877
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    Chemistry of Materials

    Cite this: Chem. Mater. 2021, 33, 18, 7315–7336
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    https://doi.org/10.1021/acs.chemmater.1c01744
    Published September 14, 2021
    Copyright © 2021 American Chemical Society
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    Abstract

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    The solid electrolyte interphase (SEI) is an integral part of Li-ion batteries and their performance, representing the key enabler for reversibility and also serving as a major source of capacity loss and dictating the cell kinetics. In the pervasive LiPF6-containing electrolytes, LiF is one of the SEI’s major components; however, its formation mechanism remains unclear. Electrochemically, two separate reduction pathways could lead to LiF, either via direct anion reduction or electrocatalytic transformation of HF. This work aims to shed light on understanding the role played by these pathways. In a multimodal experimental and theoretical approach, we carried out operando structural characterization on an inert model single crystalline N-doped SiC working electrode during voltammetric scans in LiPF6 baseline electrolytes and complemented these with ex situ chemical characterization. These results were supplemented by cyclic voltammetry measurements using a variety of electrolyte formulations under different cycling rates as well as quantum chemical calculations and Born–Oppenheimer molecular dynamics simulations. Our results reveal that the reductive formation of LiF in these systems is likely a combined mechanism, which concomitantly involves both direct anion reduction and electrocatalytic transformation of HF. Specifically, LiF nucleates via the electrocatalytic transformation of HF followed by significant anion reduction.

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    • (Figure S1) All datasets from LP30 at 0.16 mV/s and confidence interval approach; (Figure S2) additional XPS; (Figure S3) electrochemistry for several cycles and with different scan rates; (Figure S4) electrochemistry for several cycles and with different scan rate, with current normalized by sweep rate; (Figure S5) electrochemistry for several cycles and with different scan rates, with current normalized by sweep rate, plotted with different y-axis scales; (Figure S6) all parameters from all XRR data; (Figure S7) selected XRD results from operando XRD experiment on the SiC electrode during CV; (Figure S8) electrochemistry of Li plating and stripping on SiC substrate; (Table S1) breakdown of all reactions observed over 24.0 ps trajectories; (Figure S9) BOMD snapshots; (Movies r1–r6) BOMD animations; and (Figure S10) all XRR data sets (PDF)

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    Cite this: Chem. Mater. 2021, 33, 18, 7315–7336
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    https://doi.org/10.1021/acs.chemmater.1c01744
    Published September 14, 2021
    Copyright © 2021 American Chemical Society
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