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ACS Appl Mater Interfaces. 2016 Jan 13;8(1):371-80. doi: 10.1021/acsami.5b08902. Epub 2015 Dec 29.

Identification of Li-Ion Battery SEI Compounds through (7)Li and (13)C Solid-State MAS NMR Spectroscopy and MALDI-TOF Mass Spectrometry.

ACS applied materials & interfaces

Laura A Huff, Hadi Tavassol, Jennifer L Esbenshade, Wenting Xing, Yet-Ming Chiang, Andrew A Gewirth

Affiliations

  1. Department of Chemistry, University of Illinois at Urbana-Champaign , 600 South Mathews Avenue, Urbana, Illinois 61801, United States.
  2. Department of Materials Science and Engineering, Massachusetts Institute of Technology , Cambridge, Massachusetts 02139, United States.

PMID: 26653886 DOI: 10.1021/acsami.5b08902

Abstract

Solid-state (7)Li and (13)C MAS NMR spectra of cycled graphitic Li-ion anodes demonstrate SEI compound formation upon lithiation that is followed by changes in the SEI upon delithiation. Solid-state (13)C DPMAS NMR shows changes in peaks associated with organic solvent compounds (ethylene carbonate and dimethyl carbonate, EC/DMC) upon electrochemical cycling due to the formation of and subsequent changes in the SEI compounds. Solid-state (13)C NMR spin-lattice (T1) relaxation time measurements of lithiated Li-ion anodes and reference poly(ethylene oxide) (PEO) powders, along with MALDI-TOF mass spectrometry results, indicate that large-molecular-weight polymers are formed in the SEI layers of the discharged anodes. MALDI-TOF MS and NMR spectroscopy results additionally indicate that delithiated anodes exhibit a larger number of SEI products than is found in lithiated anodes.

Keywords: Li-ion battery; MALDI TOF MS; NMR; SEI; graphite anode

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