Identifying the Structure of the Intermediate, Li 2/3 CoPO 4 , Formed during Electrochemical Cycling of LiCoPO 4

Strobridge, Fiona C.; Clément, Raphaële J.; Leskes, Michal; Middlemiss, Derek S.; Borkiewicz, Olaf J.; Wiaderek, Kamila M.; Chapman, Karena W.; Chupas, Peter J.; Grey, Clare P.

doi:10.1021/cm502680w

Title: Identifying the Structure of the Intermediate, Li _2/3 CoPO ₄ , Formed during Electrochemical Cycling of LiCoPO ₄

Journal Article · Mon Nov 03 00:00:00 EST 2014 · Chemistry of Materials

DOI:https://doi.org/10.1021/cm502680w· OSTI ID:1171657

Strobridge, Fiona C. ^[1]; Clément, Raphaële J. ^[1]; Leskes, Michal ^[1]; Middlemiss, Derek S. ^[1]; Borkiewicz, Olaf J. ^[2]; Wiaderek, Kamila M. ^[2]; Chapman, Karena W. ^[2]; Chupas, Peter J. ^[2]; Grey, Clare P. ^[3]

Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge, Cambridgeshire CB2 1EW, United Kingdom
X-ray Science Division, Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439, United States
Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge, Cambridgeshire CB2 1EW, United Kingdom, Department of Chemistry, State University of New York at Stony Brook, Stony Brook, New York 11794-3400, United States

In situ synchrotron diffraction measurements and subsequent Rietveld refinements are used to show that the high energy density cathode material LiCoPO₄ (space group Pnma) undergoes two distinct two-phase reactions upon charge and discharge, both occurring via an intermediate Li_2/3(Co²⁺)_2/3(Co³⁺)_1/3PO₄ phase. Two resonances are observed for Li_2/3CoPO₄ with intensity ratios of 2:1 and 1:1 in the ³¹P and ⁷Li NMR spectra, respectively. An ordering of Co²⁺/Co³⁺ oxidation states is proposed within a (a × 3b × c) supercell, and Li⁺/vacancy ordering is investigated using experimental NMR data in combination with first-principles solid-state DFT calculations. In the lowest energy configuration, both the Co³⁺ ions and Li vacancies are found to order along the b-axis. Two other low energy Li⁺/vacancy ordering schemes are found only 5 meV per formula unit higher in energy. All three configurations lie below the LiCoPO₄–CoPO₄ convex hull and they may be readily interconverted by Li⁺ hops along the b-direction.

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Research Organization:: Argonne National Lab. (ANL), Argonne, IL (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: AC02-06CH11357

OSTI ID:: 1171657

Alternate ID(s):: OSTI ID: 1213696

Journal Information:: Chemistry of Materials, Journal Name: Chemistry of Materials Vol. 26 Journal Issue: 21; ISSN 0897-4756

Publisher:: American Chemical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 48 works

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