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Title: Chemical and Structural Stability of Lithium-Ion Battery Electrode Materials under Electron Beam

Our investigation of chemical and structural dynamics in battery materials is essential to elucidation of structure-property relationships for rational design of advanced battery materials. Spatially resolved techniques, such as scanning/transmission electron microscopy (S/TEM), are widely applied to address this challenge. But, battery materials are susceptible to electron beam damage, complicating the data interpretation. In this study, we demonstrate that, under electron beam irradiation, the surface and bulk of battery materials undergo chemical and structural evolution equivalent to that observed during charge-discharge cycling. In a lithiated NiO nanosheet, a Li2CO3-containing surface reaction layer (SRL) was gradually decomposed during electron energy loss spectroscopy (EELS) acquisition. For cycled LiNi 0.4Mn 0.4Co 0.18Ti 0.02O 2 particles, repeated electron beam irradiation induced a phase transition from an R$$\bar{3}$$m layered structure to an rock-salt structure, which is attributed to the stoichiometric lithium and oxygen removal from R$$\bar{3}$$m 3a and 6c sites, respectively. Nevertheless, it is still feasible to preserve pristine chemical environments by minimizing electron beam damage, for example, in using fast electron imaging and spectroscopy. Finally, the present study provides examples of electron beam damage on lithium-ion battery materials and suggests that special attention is necessary to prevent misinterpretation of experimental results.
Authors:
 [1] ;  [2] ;  [1] ;  [3]
  1. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Environmental Energy Technologies Division
  2. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Environmental Energy Technologies Division; Univ. of California, Berkeley, CA (United States). Dept. of Materials Science and Engineering
  3. Brookhaven National Lab. (BNL), Upton, NY (United States). Center for Functional Nanomaterials
Publication Date:
Report Number(s):
LBNL-181657
Journal ID: ISSN 2045-2322; ir:181657
Grant/Contract Number:
AC02-05CH11231; AC02-98CH10886
Type:
Accepted Manuscript
Journal Name:
Scientific Reports
Additional Journal Information:
Journal Volume: 4; Journal Issue: 1; Journal ID: ISSN 2045-2322
Publisher:
Nature Publishing Group
Research Org:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Org:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22); USDOE Office of Energy Efficiency and Renewable Energy (EERE), Vehicle Technologies Office (EE-3V)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 25 ENERGY STORAGE; batteries; optical spectroscopy
OSTI Identifier:
1371720

Lin, Feng, Markus, Isaac M., Doeff, Marca M., and Xin, Huolin L.. Chemical and Structural Stability of Lithium-Ion Battery Electrode Materials under Electron Beam. United States: N. p., Web. doi:10.1038/srep05694.
Lin, Feng, Markus, Isaac M., Doeff, Marca M., & Xin, Huolin L.. Chemical and Structural Stability of Lithium-Ion Battery Electrode Materials under Electron Beam. United States. doi:10.1038/srep05694.
Lin, Feng, Markus, Isaac M., Doeff, Marca M., and Xin, Huolin L.. 2014. "Chemical and Structural Stability of Lithium-Ion Battery Electrode Materials under Electron Beam". United States. doi:10.1038/srep05694. https://www.osti.gov/servlets/purl/1371720.
@article{osti_1371720,
title = {Chemical and Structural Stability of Lithium-Ion Battery Electrode Materials under Electron Beam},
author = {Lin, Feng and Markus, Isaac M. and Doeff, Marca M. and Xin, Huolin L.},
abstractNote = {Our investigation of chemical and structural dynamics in battery materials is essential to elucidation of structure-property relationships for rational design of advanced battery materials. Spatially resolved techniques, such as scanning/transmission electron microscopy (S/TEM), are widely applied to address this challenge. But, battery materials are susceptible to electron beam damage, complicating the data interpretation. In this study, we demonstrate that, under electron beam irradiation, the surface and bulk of battery materials undergo chemical and structural evolution equivalent to that observed during charge-discharge cycling. In a lithiated NiO nanosheet, a Li2CO3-containing surface reaction layer (SRL) was gradually decomposed during electron energy loss spectroscopy (EELS) acquisition. For cycled LiNi0.4Mn0.4Co0.18Ti0.02O2 particles, repeated electron beam irradiation induced a phase transition from an R$\bar{3}$m layered structure to an rock-salt structure, which is attributed to the stoichiometric lithium and oxygen removal from R$\bar{3}$m 3a and 6c sites, respectively. Nevertheless, it is still feasible to preserve pristine chemical environments by minimizing electron beam damage, for example, in using fast electron imaging and spectroscopy. Finally, the present study provides examples of electron beam damage on lithium-ion battery materials and suggests that special attention is necessary to prevent misinterpretation of experimental results.},
doi = {10.1038/srep05694},
journal = {Scientific Reports},
number = 1,
volume = 4,
place = {United States},
year = {2014},
month = {7}
}

Works referenced in this record:

A review of the features and analyses of the solid electrolyte interphase in Li-ion batteries
journal, September 2010

In Situ Observation of the Electrochemical Lithiation of a Single SnO2 Nanowire Electrode
journal, December 2010