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

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

doi:10.1021/acs.nanolett.5b03373

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

Journal Article · Mon Sep 21 00:00:00 EDT 2015 · Nano Letters

DOI:https://doi.org/10.1021/acs.nanolett.5b03373· OSTI ID:1512876

Li, Zhi ^[1]; Tan, Xuehai ^[1]; Li, Peng ^[2]; Kalisvaart, Peter ^[1]; Janish, Matthew T. ^[3]; Mook, William M. ^[4]; Luber, Erik J. ^[5]; Jungjohann, Katherine L. ^[4]; Carter, C. Barry ^[3]; Mitlin, David ^[6]

Univ. of Alberta, Edmonton, AB (Canada). Chemical and Materials Engineering
Univ. of Alberta, Edmonton, AB (Canada). nanoFAB Fabrication and Characterization Facility
Univ. of Connecticut, Storrs, CT (United States). Dept. of Materials Science and Engineering
Sandia National Lab. (SNL-NM), Albuquerque, NM (United States). Center for Integrated Nanotechnologies
Univ. of Alberta, Edmonton, AB (Canada). Dept. of Chemistry
Clarkson Univ., Potsdam, NY (United States). Chemical & Biomolecular Engineering and Mechanical Engineering

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.

View Accepted Manuscript (DOE)

Research Organization:: Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)

Sponsoring Organization:: USDOE National Nuclear Security Administration (NNSA)

Grant/Contract Number:: AC04-94AL85000

OSTI ID:: 1512876

Report Number(s):: SAND--2015-2969J; 662092

Journal Information:: Nano Letters, Journal Name: Nano Letters Journal Issue: 10 Vol. 15; ISSN 1530-6984

Publisher:: American Chemical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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