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Title: Characterization of Sulfur and Nanostructured Sulfur Battery Cathodes in Electron Microscopy Without Sublimation Artifacts

Abstract

Abstract Lithium sulfur (Li–S) batteries have the potential to provide higher energy storage density at lower cost than conventional lithium ion batteries. A key challenge for Li–S batteries is the loss of sulfur to the electrolyte during cycling. This loss can be mitigated by sequestering the sulfur in nanostructured carbon–sulfur composites. The nanoscale characterization of the sulfur distribution within these complex nanostructured electrodes is normally performed by electron microscopy, but sulfur sublimates and redistributes in the high-vacuum conditions of conventional electron microscopes. The resulting sublimation artifacts render characterization of sulfur in conventional electron microscopes problematic and unreliable. Here, we demonstrate two techniques, cryogenic transmission electron microscopy (cryo-TEM) and scanning electron microscopy in air (airSEM), that enable the reliable characterization of sulfur across multiple length scales by suppressing sulfur sublimation. We use cryo-TEM and airSEM to examine carbon–sulfur composites synthesized for use as Li–S battery cathodes, noting several cases where the commonly employed sulfur melt infusion method is highly inefficient at infiltrating sulfur into porous carbon hosts.

Authors:
; ; ; ; ORCiD logo; ; ; ; ; ; ; ;
Publication Date:
Research Org.:
Energy Frontier Research Centers (EFRC) (United States). Energy Materials Center at Cornell (EMC2)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
OSTI Identifier:
1397223
DOE Contract Number:  
SC0001086
Resource Type:
Journal Article
Journal Name:
Microscopy and Microanalysis
Additional Journal Information:
Journal Volume: 23; Journal Issue: 01; Related Information: Emc2 partners with Cornell University (lead); Lawrence Berkeley National Laboratory; Journal ID: ISSN 1431-9276
Publisher:
Microscopy Society of America (MSA)
Country of Publication:
United States
Language:
English
Subject:
25 ENERGY STORAGE; 36 MATERIALS SCIENCE

Citation Formats

Levin, Barnaby D. A., Zachman, Michael J., Werner, Jörg G., Sahore, Ritu, Nguyen, Kayla X., Han, Yimo, Xie, Baoquan, Ma, Lin, Archer, Lynden A., Giannelis, Emmanuel P., Wiesner, Ulrich, Kourkoutis, Lena F., and Muller, David A. Characterization of Sulfur and Nanostructured Sulfur Battery Cathodes in Electron Microscopy Without Sublimation Artifacts. United States: N. p., 2017. Web. doi:10.1017/s1431927617000058.
Levin, Barnaby D. A., Zachman, Michael J., Werner, Jörg G., Sahore, Ritu, Nguyen, Kayla X., Han, Yimo, Xie, Baoquan, Ma, Lin, Archer, Lynden A., Giannelis, Emmanuel P., Wiesner, Ulrich, Kourkoutis, Lena F., & Muller, David A. Characterization of Sulfur and Nanostructured Sulfur Battery Cathodes in Electron Microscopy Without Sublimation Artifacts. United States. doi:10.1017/s1431927617000058.
Levin, Barnaby D. A., Zachman, Michael J., Werner, Jörg G., Sahore, Ritu, Nguyen, Kayla X., Han, Yimo, Xie, Baoquan, Ma, Lin, Archer, Lynden A., Giannelis, Emmanuel P., Wiesner, Ulrich, Kourkoutis, Lena F., and Muller, David A. Wed . "Characterization of Sulfur and Nanostructured Sulfur Battery Cathodes in Electron Microscopy Without Sublimation Artifacts". United States. doi:10.1017/s1431927617000058.
@article{osti_1397223,
title = {Characterization of Sulfur and Nanostructured Sulfur Battery Cathodes in Electron Microscopy Without Sublimation Artifacts},
author = {Levin, Barnaby D. A. and Zachman, Michael J. and Werner, Jörg G. and Sahore, Ritu and Nguyen, Kayla X. and Han, Yimo and Xie, Baoquan and Ma, Lin and Archer, Lynden A. and Giannelis, Emmanuel P. and Wiesner, Ulrich and Kourkoutis, Lena F. and Muller, David A.},
abstractNote = {Abstract Lithium sulfur (Li–S) batteries have the potential to provide higher energy storage density at lower cost than conventional lithium ion batteries. A key challenge for Li–S batteries is the loss of sulfur to the electrolyte during cycling. This loss can be mitigated by sequestering the sulfur in nanostructured carbon–sulfur composites. The nanoscale characterization of the sulfur distribution within these complex nanostructured electrodes is normally performed by electron microscopy, but sulfur sublimates and redistributes in the high-vacuum conditions of conventional electron microscopes. The resulting sublimation artifacts render characterization of sulfur in conventional electron microscopes problematic and unreliable. Here, we demonstrate two techniques, cryogenic transmission electron microscopy (cryo-TEM) and scanning electron microscopy in air (airSEM), that enable the reliable characterization of sulfur across multiple length scales by suppressing sulfur sublimation. We use cryo-TEM and airSEM to examine carbon–sulfur composites synthesized for use as Li–S battery cathodes, noting several cases where the commonly employed sulfur melt infusion method is highly inefficient at infiltrating sulfur into porous carbon hosts.},
doi = {10.1017/s1431927617000058},
journal = {Microscopy and Microanalysis},
issn = {1431-9276},
number = 01,
volume = 23,
place = {United States},
year = {2017},
month = {2}
}

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