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Persistent and partially mobile oxygen vacancies in Li-rich layered oxides

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Abstract

Increasing the energy density of layered oxide battery electrodes is challenging as accessing high states of delithiation often triggers voltage degradation and oxygen release. Here we utilize transmission-based X-ray absorption spectromicroscopy and ptychography on mechanically cross-sectioned Li1.18–xNi0.21Mn0.53Co0.08O2–δ electrodes to quantitatively profile the oxygen deficiency over cycling at the nanoscale. The oxygen deficiency penetrates into the bulk of individual primary particles (~200 nm) and is well-described by oxygen vacancy diffusion. Using an array of characterization techniques, we demonstrate that, surprisingly, bulk oxygen vacancies that persist within the native layered phase are indeed responsible for the observed spectroscopic changes. We additionally show that the arrangement of primary particles within secondary particles (~5 μm) causes considerable heterogeneity in the extent of oxygen release between primary particles. Our work merges an ensemble of length-spanning characterization methods and informs promising approaches to mitigate the deleterious effects of oxygen release in lithium-ion battery electrodes.

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Fig. 1: Electrochemical voltage depression linked to cation disordering and TM reduction.
Fig. 2: Spatial dependence of the Mn oxidation state within primary particles.
Fig. 3: Structural consequences of oxygen release.
Fig. 4: Oxidation state heterogeneity on the secondary particle scale.
Fig. 5: Oxidation state heterogeneity in the charged state.

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Data availability

Data supporting the main text figures can be found at https://doi.org/10.5281/zenodo.4697951. Data supporting the Supplementary Information figures can be found at https://doi.org/10.5281/zenodo.4697955.

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Acknowledgements

The battery component of this work was supported by the Assistant Secretary for Energy Efficiency and Renewable Energy, Office of Vehicle Technologies, Battery Materials Research Program, US Department of Energy (DOE), and by Samsung Advanced Institute of Technology Global Research Outreach program. STXM and X-ray ptychography development was supported by the DOE, Office of Basic Energy Sciences, Division of Materials Sciences and Engineering (contract DE-AC02-76SF00515). This research used resources of the ALS, a DOE Office of Science User Facility under contract no. DE-AC02-05CH11231. This work was partially supported by STROBE, a National Science Foundation Science and Technology Center under award DMR1548924. Use of the SSRL, SLAC National Accelerator Laboratory, is supported by the US Department of Energy, Office of Science, Office of Basic Energy Sciences under contract no. DE-AC02-76SF00515. A portion of this research used resources at the Spallation Neutron Source, a DOE Office of Science User Facility operated by the Oak Ridge National Laboratory. Part of this work was performed at the Stanford Nano Shared Facilities, supported by the National Science Foundation under award ECCS-1542152. P.M.C. acknowledges support through the Stanford Graduate Fellowship as a Winston and Fu-Mei Chen fellow and through the National Science Foundation Graduate Research Fellowship under Grant no. DGE-1656518. W.E.G. was supported additionally by the ALS Doctoral Fellowship. Y.L. and R.S. acknowledge the financial support from the Toyota Research Institute—Accelerated Materials Design and Discovery (TRI-AMDD) program (Stanford University). We thank L. Echávez, L. Schelhas, T. Mefford, M. Lattimer and B. Enders for helpful discussions and/or experimental support. We acknowledge R. Chin for performing the FIB electrode cross-sectioning for the TEM experiments. We also acknowledge R. Kim for experimental TEM support and helpful discussions.

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Authors and Affiliations

  1. Department of Materials Science and Engineering, Stanford University, Stanford, CA, USA

    Peter M. Csernica, Samanbir S. Kalirai, William E. Gent, Kipil Lim, Yunzhi Liu, Emma Kaeli, **n Xu, Robert Sinclair & William C. Chueh

  2. Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA, USA

    Samanbir S. Kalirai, Young-Sang Yu & David A. Shapiro

  3. Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, Menlo Park, CA, USA

    Kipil Lim, Kevin H. Stone & Michael F. Toney

  4. Energy Lab, Samsung Advanced Institute of Technology, Suwon-si, South Korea

    Sung-** Ahn

  5. Stanford Nano Shared Facilities, Stanford University, Stanford, CA, USA

    Ann F. Marshall

  6. Department of Chemical and Biological Engineering, University of Colorado Boulder, Boulder, CO, USA

    Michael F. Toney

  7. Stanford Institute for Materials and Energy Sciences, SLAC National Accelerator Laboratory, Menlo Park, CA, USA

    William C. Chueh

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  1. Peter M. Csernica
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Contributions

P.M.C., S.S.K., W.E.G., D.A.S., M.F.T. and W.C.C. conceived the study. S.S.K. and E.K. performed the ultramicrotomy sectioning. P.M.C., S.S.K., W.E.G., Y.-S.Y. and D.A.S. collected ex situ STXM and ptychography images and analysed the data. P.M.C., K.L. and K.H.S. collected the SXRD data. P.M.C. collected the neutron diffraction data. P.M.C., K.L., K.H.S. and M.F.T. analysed the diffraction data. S.-J.A. synthesized the material and cycled the mini-18650 cells. P.M.C. performed the ICP-MS, scanning electron microscopy and pycnometry experiments. P.M.C. collected TM K-edge spectra and K.L., W.E.G. and M.F.T. contributed to the interpretation. P.M.C. and W.C.C. developed the diffusion and two-phase core–shell models used. Y.L. and X.X. collected TEM images. Y.L., X.X., P.M.C., A.F.M., R.S. and W.C.C. analysed the TEM data. P.M.C, W.C.C. and M.F.T. wrote the manuscript and all the authors revised the manuscript.

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Correspondence to David A. Shapiro, Michael F. Toney or William C. Chueh.

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Supplementary Figs. 1–54, Tables 1–12, Notes 1–9 and Methods.

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Csernica, P.M., Kalirai, S.S., Gent, W.E. et al. Persistent and partially mobile oxygen vacancies in Li-rich layered oxides. Nat Energy 6, 642–652 (2021). https://doi.org/10.1038/s41560-021-00832-7

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