Journal
JOURNAL OF POWER SOURCES
Volume 246, Issue -, Pages 512-521Publisher
ELSEVIER
DOI: 10.1016/j.jpowsour.2013.08.003
Keywords
LiFePO4; TEM; Electron energy loss spectroscopy; Phase transformation
Funding
- U.S. Department of Energy through the Sandia Laboratory Directed research and Development program
- Office of Basic Energy Science, Division of Materials Sciences and Engineering
- Office of Science, Office of Basic Energy Sciences, of the U.S. Department of Energy [DE-AC02-05CH11231]
- U.S. Department of Energy's National Nuclear Security Administration [DE-AC04-94AL85000]
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We demonstrate an ex situ method for analyzing the chemistry of battery electrode particles after electrochemical cycling using the transmission electron microscope (TEM). The arrangement of particles during our analysis is the same as when the particles are being cycled. We start by sectioning LiFePO4 battery electrodes using an ultramicrotome. We then show that mapping of the Fe2+ and Fe3+ oxidation state using energy-filtered TEM (EFTEM) and multivariate statistical analysis techniques can be used to determine the spatial distribution of Li in the particles. This approach is validated by comparison with scanning transmission X-ray microscopy (STXM) analysis of the same samples [Chueh et al. Nanoletters, 13 (3) (2013) 866-72]. EFTEM uses a parallel electron beam and reduces the electron-beam dose (and potential beam-induced damage) to the sample when compared to alternate techniques that use a focused probe (e.g. STEM-EELS). Our analysis confirms that under the charging conditions of the analyzed battery, mixed phase particles are rare and thus Li intercalation is limited by the nucleation of new phases. (C) 2013 Elsevier B.V. All rights reserved.
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