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

Published online by Cambridge University Press:  23 February 2017

Barnaby D.A. Levin
Affiliation:
School of Applied and Engineering Physics, Cornell University, Ithaca, NY 14853, USA
Michael J. Zachman
Affiliation:
School of Applied and Engineering Physics, Cornell University, Ithaca, NY 14853, USA
Jörg G. Werner
Affiliation:
Department of Materials Science and Engineering, Cornell University, Ithaca, NY 14853, USA
Ritu Sahore
Affiliation:
Department of Materials Science and Engineering, Cornell University, Ithaca, NY 14853, USA
Kayla X. Nguyen
Affiliation:
School of Applied and Engineering Physics, Cornell University, Ithaca, NY 14853, USA
Yimo Han
Affiliation:
School of Applied and Engineering Physics, Cornell University, Ithaca, NY 14853, USA
Baoquan Xie
Affiliation:
Department of Materials Science and Engineering, Cornell University, Ithaca, NY 14853, USA
Lin Ma
Affiliation:
Department of Materials Science and Engineering, Cornell University, Ithaca, NY 14853, USA
Lynden A. Archer
Affiliation:
School of Chemical and Biomolecular Engineering, Cornell University, Ithaca, NY 14853, USA
Emmanuel P. Giannelis
Affiliation:
Department of Materials Science and Engineering, Cornell University, Ithaca, NY 14853, USA
Ulrich Wiesner
Affiliation:
Department of Materials Science and Engineering, Cornell University, Ithaca, NY 14853, USA
Lena F. Kourkoutis
Affiliation:
School of Applied and Engineering Physics, Cornell University, Ithaca, NY 14853, USA Kavli Institute for Nanoscale Science, Cornell University, Ithaca, NY 14853, USA
David A. Muller
Affiliation:
School of Applied and Engineering Physics, Cornell University, Ithaca, NY 14853, USA Kavli Institute for Nanoscale Science, Cornell University, Ithaca, NY 14853, USA
Corresponding
E-mail address:

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.

Type
Materials Applications
Copyright
© Microscopy Society of America 2017 

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