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EELS Spectroscopy of Iron Fluorides and FeFx/C Nanocomposite Electrodes Used in Li-Ion Batteries

Published online by Cambridge University Press:  15 February 2007

Frederic Cosandey ,
Jafar F. Al-Sharab ,
Fadwa Badway ,
Glenn G. Amatucci  and
Pierre Stadelmann
Frederic Cosandey
Affiliation:
Department of Materials Science and Engineering, Rutgers, The State University of New Jersey, Piscataway, NJ 08854-8065, USA
Jafar F. Al-Sharab
Affiliation:
Department of Materials Science and Engineering, Rutgers, The State University of New Jersey, Piscataway, NJ 08854-8065, USA
Fadwa Badway
Affiliation:
Department of Materials Science and Engineering, Rutgers, The State University of New Jersey, Piscataway, NJ 08854-8065, USA Energy Storage Research Group, Rutgers, The State University of New Jersey, Piscataway, NJ 08854-8065, USA
Glenn G. Amatucci
Affiliation:
Department of Materials Science and Engineering, Rutgers, The State University of New Jersey, Piscataway, NJ 08854-8065, USA Energy Storage Research Group, Rutgers, The State University of New Jersey, Piscataway, NJ 08854-8065, USA
Pierre Stadelmann
Affiliation:
Centre Interdepartemental de Microscopie Electronique, Ecole Polytechnique Federale de Lausanne, Switzerland
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Abstract

A new type of positive electrode for Li-ion batteries has been developed recently based on FeF3/C and FeF2/C nanocomposites. The microstructural and redox evolution during discharge and recharge processes was followed by electron energy loss spectroscopy (EELS) to determine the valence state of Fe by measuring the Fe L3 line energy shift and from Fe L3/L2 line intensity ratios. In addition, transition metal fluorides were found to be electron beam sensitive, and the effect of beam exposure on EELS spectra was also investigated. The EELS results indicate that for both FeF3/C and FeF2/C nanocomposite systems, a complete reduction of iron to FeO is observed upon discharge to 1.5 V with the formation of a finer FeO/LiF subnanocomposite (∼7 nm). Upon complete recharging to 4.5 V, EELS data reveal a reoxidation process to a Fe2+ state with the formation of a carbon metal fluoride nanocomposite related to the FeF2 structure.

Keywords

EELSiron fluoridesirradiation damageLi-ion batteries
Type
MATERIALS APPLICATIONS
Information
Microscopy and Microanalysis , Volume 13 , Issue 2 , April 2007 , pp. 87 - 95
Copyright
© 2007 Microscopy Society of America

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