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Direct Visualization of Solid Electrolyte Interphase Formation in Lithium-Ion Batteries with In Situ Electrochemical Transmission Electron Microscopy
Raymond R. Unocic, Xiao-Guang Sun, Robert L. Sacci, Leslie A. Adamczyk, Daan Hein Alsem, Sheng Dai, Nancy J. Dudney, Karren L. More
Journal: Microscopy and Microanalysis / Volume 20 / Issue 4 / August 2014
Published online by Cambridge University Press: 04 July 2014, pp. 1029-1037
Print publication: August 2014
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Complex, electrochemically driven transport processes form the basis of electrochemical energy storage devices. The direct imaging of electrochemical processes at high spatial resolution and within their native liquid electrolyte would significantly enhance our understanding of device functionality, but has remained elusive. In this work we use a recently developed liquid cell for in situ electrochemical transmission electron microscopy to obtain insight into the electrolyte decomposition mechanisms and kinetics in lithium-ion (Li-ion) batteries by characterizing the dynamics of solid electrolyte interphase (SEI) formation and evolution. Here we are able to visualize the detailed structure of the SEI that forms locally at the electrode/electrolyte interface during lithium intercalation into natural graphite from an organic Li-ion battery electrolyte. We quantify the SEI growth kinetics and observe the dynamic self-healing nature of the SEI with changes in cell potential.

Quantitative Electrochemical Measurements Using In Situ ec-S/TEM Devices
Raymond R. Unocic, Robert L. Sacci, Gilbert M. Brown, Gabriel M. Veith, Nancy J. Dudney, Karren L. More, Franklin S. Walden II, Daniel S. Gardiner, John Damiano, David P. Nackashi
Journal: Microscopy and Microanalysis / Volume 20 / Issue 2 / April 2014
Published online by Cambridge University Press: 11 March 2014, pp. 452-461
Print publication: April 2014
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Insight into dynamic electrochemical processes can be obtained with in situ electrochemical-scanning/transmission electron microscopy (ec-S/TEM), a technique that utilizes microfluidic electrochemical cells to characterize electrochemical processes with S/TEM imaging, diffraction, or spectroscopy. The microfluidic electrochemical cell is composed of microfabricated devices with glassy carbon and platinum microband electrodes in a three-electrode cell configuration. To establish the validity of this method for quantitative in situ electrochemistry research, cyclic voltammetry (CV), choronoamperometry (CA), and electrochemical impedance spectroscopy (EIS) were performed using a standard one electron transfer redox couple [Fe(CN)6]3−/4−-based electrolyte. Established relationships of the electrode geometry and microfluidic conditions were fitted with CV and chronoamperometic measurements of analyte diffusion coefficients and were found to agree with well-accepted values that are on the order of 10−5 cm2/s. Influence of the electron beam on electrochemical measurements was found to be negligible during CV scans where the current profile varied only within a few nA with the electron beam on and off, which is well within the hysteresis between multiple CV scans. The combination of experimental results provides a validation that quantitative electrochemistry experiments can be performed with these small-scale microfluidic electrochemical cells provided that accurate geometrical electrode configurations, diffusion boundary layers, and microfluidic conditions are accounted for.

TEM Specimen Preparation of Thin Interfacial Coatings on Continuous Ceramic Fibers Using the Focused Ion Beam (FIB) Technique
Dorothy W. Coffey, Karren L. More, Tracie Brummett
Journal: Microscopy and Microanalysis / Volume 10 / Issue S02 / August 2004
Published online by Cambridge University Press: 01 August 2004, pp. 1160-1161
Print publication: August 2004
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Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.

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In operando Transmission Electron Microscopy Imaging of SEI Formation and Structure in Li-Ion and Li-Metal Batteries

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Direct Visualization of Solid Electrolyte Interphase Formation in Lithium-Ion Batteries with In Situ Electrochemical Transmission Electron Microscopy

Quantitative Electrochemical Measurements Using In Situ ec-S/TEM Devices

TEM Specimen Preparation of Thin Interfacial Coatings on Continuous Ceramic Fibers Using the Focused Ion Beam (FIB) Technique

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