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Title: Coupling In Situ TEM and Ex Situ Analysis to Understand Heterogeneous Sodiation of Antimony

Abstract

Here, we employed an in situ electrochemical cell in the transmission electron microscope (TEM) together with ex situ time-of-flight, secondary-ion mass spectrometry (TOF-SIMS) depth profiling, and FIB–helium ion scanning microscope (HIM) imaging to detail the structural and compositional changes associated with Na/Na+ charging/discharging of 50 and 100 nm thin films of Sb. TOF-SIMS on a partially sodiated 100 nm Sb film gives a Na signal that progressively decreases toward the current collector, indicating that sodiation does not proceed uniformly. This heterogeneity will lead to local volumetric expansion gradients that would in turn serve as a major source of intrinsic stress in the microstructure. In situ TEM shows time-dependent buckling and localized separation of the sodiated films from their TiN-Ge nanowire support, which is a mechanism of stress-relaxation. Localized horizontal fracture does not occur directly at the interface, but rather at a short distance away within the bulk of the Sb. HIM images of FIB cross sections taken from sodiated half-cells, electrically disconnected, and aged at room temperature, demonstrate nonuniform film swelling and the onset of analogous through-bulk separation. TOF-SIMS highlights time-dependent segregation of Na within the structure, both to the film-current collector interface and to the film surface where amore » solid electrolyte interphase (SEI) exists, agreeing with the electrochemical impedance results that show time-dependent increase of the films’ charge transfer resistance. We propose that Na segregation serves as a secondary source of stress relief, which occurs over somewhat longer time scales.« less

Authors:
 [1];  [1];  [2];  [1];  [3];  [4];  [5];  [4];  [3];  [6]
+ Show Author Affiliations
  1. Univ. of Alberta, Edmonton, AB (Canada). Chemical and Materials Engineering
  2. Univ. of Alberta, Edmonton, AB (Canada). nanoFAB Fabrication and Characterization Facility
  3. Univ. of Connecticut, Storrs, CT (United States). Dept. of Materials Science and Engineering
  4. Sandia National Lab. (SNL-NM), Albuquerque, NM (United States). Center for Integrated Nanotechnologies
  5. Univ. of Alberta, Edmonton, AB (Canada). Dept. of Chemistry
  6. Clarkson Univ., Potsdam, NY (United States). Chemical & Biomolecular Engineering and Mechanical Engineering
Publication Date:
Research Org.:
Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
Sponsoring Org.:
USDOE National Nuclear Security Administration (NNSA)
OSTI Identifier:
1512876
Report Number(s):
SAND-2015-2969J
Journal ID: ISSN 1530-6984; 662092
Grant/Contract Number:  
AC04-94AL85000
Resource Type:
Accepted Manuscript
Journal Name:
Nano Letters
Additional Journal Information:
Journal Volume: 15; Journal Issue: 10; Journal ID: ISSN 1530-6984
Publisher:
American Chemical Society
Country of Publication:
United States
Language:
English
Subject:
25 ENERGY STORAGE; antimony; in situ TEM; lithium ion battery; operando; sodium ion battery

Citation Formats

Li, Zhi, Tan, Xuehai, Li, Peng, Kalisvaart, Peter, Janish, Matthew T., Mook, William M., Luber, Erik J., Jungjohann, Katherine L., Carter, C. Barry, and Mitlin, David. Coupling In Situ TEM and Ex Situ Analysis to Understand Heterogeneous Sodiation of Antimony. United States: N. p., 2015. Web. doi:10.1021/acs.nanolett.5b03373.
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Li, Zhi, Tan, Xuehai, Li, Peng, Kalisvaart, Peter, Janish, Matthew T., Mook, William M., Luber, Erik J., Jungjohann, Katherine L., Carter, C. Barry, & Mitlin, David. Coupling In Situ TEM and Ex Situ Analysis to Understand Heterogeneous Sodiation of Antimony. United States. https://doi.org/10.1021/acs.nanolett.5b03373
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Li, Zhi, Tan, Xuehai, Li, Peng, Kalisvaart, Peter, Janish, Matthew T., Mook, William M., Luber, Erik J., Jungjohann, Katherine L., Carter, C. Barry, and Mitlin, David. Mon . "Coupling In Situ TEM and Ex Situ Analysis to Understand Heterogeneous Sodiation of Antimony". United States. https://doi.org/10.1021/acs.nanolett.5b03373. https://www.osti.gov/servlets/purl/1512876.
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@article{osti_1512876,
title = {Coupling In Situ TEM and Ex Situ Analysis to Understand Heterogeneous Sodiation of Antimony},
author = {Li, Zhi and Tan, Xuehai and Li, Peng and Kalisvaart, Peter and Janish, Matthew T. and Mook, William M. and Luber, Erik J. and Jungjohann, Katherine L. and Carter, C. Barry and Mitlin, David},
abstractNote = {Here, we employed an in situ electrochemical cell in the transmission electron microscope (TEM) together with ex situ time-of-flight, secondary-ion mass spectrometry (TOF-SIMS) depth profiling, and FIB–helium ion scanning microscope (HIM) imaging to detail the structural and compositional changes associated with Na/Na+ charging/discharging of 50 and 100 nm thin films of Sb. TOF-SIMS on a partially sodiated 100 nm Sb film gives a Na signal that progressively decreases toward the current collector, indicating that sodiation does not proceed uniformly. This heterogeneity will lead to local volumetric expansion gradients that would in turn serve as a major source of intrinsic stress in the microstructure. In situ TEM shows time-dependent buckling and localized separation of the sodiated films from their TiN-Ge nanowire support, which is a mechanism of stress-relaxation. Localized horizontal fracture does not occur directly at the interface, but rather at a short distance away within the bulk of the Sb. HIM images of FIB cross sections taken from sodiated half-cells, electrically disconnected, and aged at room temperature, demonstrate nonuniform film swelling and the onset of analogous through-bulk separation. TOF-SIMS highlights time-dependent segregation of Na within the structure, both to the film-current collector interface and to the film surface where a solid electrolyte interphase (SEI) exists, agreeing with the electrochemical impedance results that show time-dependent increase of the films’ charge transfer resistance. We propose that Na segregation serves as a secondary source of stress relief, which occurs over somewhat longer time scales.},
doi = {10.1021/acs.nanolett.5b03373},
journal = {Nano Letters},
number = 10,
volume = 15,
place = {United States},
year = {Mon Sep 21 00:00:00 EDT 2015},
month = {Mon Sep 21 00:00:00 EDT 2015}
}
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https://doi.org/10.1021/acs.nanolett.5b03373
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Figures / Tables:

Figure 1 Figure 1: (a) Illustration for the setup of the in-situ transmission electron microscopy (TEM) open-cell experiment. (b) Bright field TEM micrograph of a single TiN coated Ge nanowire, with the associated indexed (polycrystalline TiN and single crystal Ge) selected area diffraction pattern being inserted. (c) SEM micrograph of 50 nmmore » Sb on TiN/Ge nanowire, hereafter labeled as 50nmSb/NW. The Sb film fully wets the TiN surface. (d) and (e) HAADF micrograph and XEDS line scan for 50nmSb/NW.« less
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    • DOI: 10.1038/ncomms15806
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