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Three-dimensional morphological measurements of LiCoO_2 and LiCoO_2/Li (Ni_(1/3)Mn_(1/3)Co_(1/3))O_2 lithium-ion battery cathodes

Liu, Zhao and Cronin, J. Scott and Chen-Wiegart, Yu-chen K. and Wilson, James R. and Yakal-Kremski, Kyle J. and Wang, Jun and Faber, Katherine T. and Barnett, Scott A. (2013) Three-dimensional morphological measurements of LiCoO_2 and LiCoO_2/Li (Ni_(1/3)Mn_(1/3)Co_(1/3))O_2 lithium-ion battery cathodes. Journal of Power Sources, 227 . pp. 267-274. ISSN 0378-7753.

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The three-dimensional (3D) morphologies of two types of lithium-ion battery cathodes, LiCoO_2 (LCO) and LiCoO_2/Li (Ni_(1/3)Mn_(1/3)Co_(1/3))O_2 (LCO/NMC) composites, have been measured using focused ion beam scanning electron microscopy (FIB-SEM) and transmission X-ray microscopy (TXM). TXM measurements were taken at X-ray energies that can provide clear contrast between LCO and NMC particles in the composite cathodes. Multiple three-dimensional image volumes were collected and statistical analyses were done to assess the accuracy and spatial variation of structural parameters including oxide volume fractions, surface areas, and particle size distributions. Comparisons of un-cycled and cycled batteries showed small changes in structure, but spatial and cell-to-cell microstructural variations, found especially in the LCO/NMC cathodes, were large enough to limit the ability to distinguish actual cycling-induced structure changes. The observation of cathode metal cations on the battery anode after cycling may explain, at least in part, the observed 30% capacity loss.

Item Type:Article
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URLURL TypeDescription
Liu, Zhao0000-0003-0370-2406
Faber, Katherine T.0000-0001-6585-2536
Alternate Title:Three-dimensional morphological measurements of LiCoO2 and LiCoO2/Li (Ni1/3Mn1/3Co1/3)O2 lithium-ion battery cathodes
Additional Information:Copyright © 2012 Elsevier. Received 24 September 2012. Received in revised form 14 November 2012. Accepted 15 November 2012. Available online 23 November 2012. The authors acknowledge the financial support from the National Science Foundation Ceramics program (DMR-0907639), the MRSEC program (DMR-1121262) of Northwestern University and Office of Naval Research Grant #N00014-12-1-0713. We thank Dr. Stephen J. Harris for providing battery samples studied in this report, Mr. Jiangtao Gou (Department of Statistics Northwestern Univ.) for useful suggestions in statistics, Mr. Benjamin Myer (Northwestern Univ.) and Dr. Fernando Camino (BNL) for assisting SEM imaging and the development of the sample preparation procedure using FIB-SEM. The FIB-SEM (Zeiss) was accomplished at the Electron Microscopy Center for Materials Research at Argonne National Laboratory under the guidance of Dr. Dean J. Miller and Dr. Jon M. Hiller, a U.S. Department of Energy Office of Science Laboratory operated under Contract No. DE-AC02-06CH11357 by UChicago Argonne, LLC. FIB-SEM (FEI) was performed in the EPIC facility of NUANCE Center at Northwestern University. NUANCE Center is supported by NSF-NSEC, NSF-MRSEC, Keck Foundation, the State of Illinois, and Northwestern University. The X-ray nanotomography and its FIB sample preparation were carried out at Brookhaven National Laboratory, which is supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-98CH10886.
Funding AgencyGrant Number
Office of Naval Research (ONR)N00014-12-1-0713
Department of Energy (DOE)DE-AC02-06CH11357
W. M. Keck FoundationUNSPECIFIED
State of IllinoisUNSPECIFIED
Northwestern UniversityUNSPECIFIED
Department of Energy (DOE)DE-AC02-98CH10886
Subject Keywords:Lithium-ion battery; Tomography; Microstructure; Statistical analysis
Record Number:CaltechAUTHORS:20140908-181319398
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Official Citation:Zhao Liu, J. Scott Cronin, Yu-chen K. Chen-Wiegart, James R. Wilson, Kyle J. Yakal-Kremski, Jun Wang, Katherine T. Faber, Scott A. Barnett, Three-dimensional morphological measurements of LiCoO2 and LiCoO2/Li(Ni1/3Mn1/3Co1/3)O2 lithium-ion battery cathodes, Journal of Power Sources, Volume 227, 1 April 2013, Pages 267-274, ISSN 0378-7753, (
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:49366
Deposited By: George Porter
Deposited On:09 Sep 2014 16:12
Last Modified:09 Mar 2020 13:19

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