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Published August 31, 2017 | Supplemental Material
Journal Article Open

X-ray nanotomography analysis of the microstructural evolution of LiMn_2 O_4 electrodes

Abstract

One of the greatest challenges for advancing lithium-ion battery (LIB) technology is to minimize cell degradation during operation for long-term stability. To this end, it is important to understand how cell performance during operation relates to complex LIB microstructures. In this report, transmission X-ray microscopy (TXM) nanotomography is used to gain quantitative three-dimensional (3D) microstructure-performance correlations of LIB cathodes during cycling. The 3D microstructures of LiMn_2O_4 (LMO) electrodes, cycled under different conditions, including cycle number, operating voltage, and temperature, are characterized via TXM and statistically analyzed to investigate the impact of cycling conditions on the electrode microstructural evolution and cell performance. It is found that the number of cracks formed within LMO particles correlated with capacity fade. For the cell cycled at elevated temperatures, which exhibits the most severe capacity fade among all cells tested, mechanical cracking observed in TXM is not the only dominant contributor to the observed degradation. Mn^(2+) dissolution, as verified by detection of Mn on the counter electrode by energy dispersive spectrometry, also contributed. The current work demonstrate 3D TXM nanotomography as a powerful tool to help probe in-depth understanding of battery failure mechanisms, which could be applicable to electrode structure optimization for advancing LIB development.

Additional Information

© 2017 Elsevier B.V. Received 4 April 2017, Revised 3 June 2017, Accepted 9 June 2017, Available online 17 June 2017. The authors gratefully acknowledge financial support from the Office of Naval Research Grant #N00014-12-1-0713. Analysis and modeling of the data was partially supported as part of the Center for Electrochemical Energy Science, an Energy Frontier Research Center funded by the U.S. Department of Energy, Office of Science, Basic Energy Sciences. ZL acknowledges support from a Northwestern University Cabell Terminal Year Fellowship. SEM/EDS was performed in the EPIC facility of the NUANCE Center at Northwestern University. The NUANCE Center has received support from the Soft and Hybrid Nanotechnology Experimental (SHyNE) Resource (NSF ECCS-1542205); the MRSEC program (NSF DMR-1121262) at the Materials Research Center; the International Institute for Nanotechnology (IIN); the Keck Foundation; and the State of Illinois, through the IIN. The author also acknowledge Use of the National Synchrotron Light Source, BNL, was supported by the U.S. (DOE, BES), under Contract No. DE-AC02-98CH10886.

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August 19, 2023
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