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Title: In situ electrochemical scanning/transmission electron microscopy of electrode–electrolyte interfaces

Journal Article · · MRS Bulletin
DOI:https://doi.org/10.1557/mrs.2020.226· OSTI ID:1736005
ORCiD logo [1];  [2];  [3];  [3];  [4]
  1. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Sciences (CNMS)
  2. Sandia National Lab. (SNL-NM), Albuquerque, NM (United States). Center for Integrated Nanotechnologies (CINT)
  3. Univ. of Liverpool (United Kingdom)
  4. Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

Insights into the dynamics of electrochemical processes are critically needed to improve our fundamental understanding of electron, charge, and mass transfer mechanisms and reaction kinetics that influence a broad range of applications, from the functionality of electrical energy-storage and conversion devices (e.g., batteries, fuel cells, and supercapacitors), to materials degradation issues (e.g., corrosion and oxidation), and materials synthesis (e.g., electrodeposition). To unravel these processes, in situ electrochemical scanning/transmission electron microscopy (ec-S/TEM) was developed to permit detailed site-specific characterization of evolving electrochemical processes that occur at electrode–electrolyte interfaces in their native electrolyte environment, in real time and at high-spatial resolution. This approach utilizes “closed-form” microfabricated electrochemical cells that couple the capability for quantitative electrochemical measurements with high spatial and temporal resolution imaging, spectroscopy, and diffraction. Here, we review the state-of-the-art instrumentation for in situ ec-S/TEM and how this approach has resulted in new observations of electrochemical processes.

Research Organization:
Pacific Northwest National Laboratory (PNNL), Richland, WA (United States). Environmental Molecular Sciences Laboratory (EMSL); Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States). Center for Integrated Nanotechnologies (CINT); Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
Sponsoring Organization:
USDOE National Nuclear Security Administration (NNSA); Faraday Institution; USDOE Laboratory Directed Research and Development (LDRD) Program; USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE Office of Energy Efficiency and Renewable Energy (EERE), Transportation Office. Vehicle Technologies Office; USDOE Office of Science (SC), Biological and Environmental Research (BER)
Grant/Contract Number:
AC05-76RL01830; NA0003525; AC05-00OR22725
OSTI ID:
1736005
Alternate ID(s):
OSTI ID: 1770661
Report Number(s):
PNNL-SA-153779
Journal Information:
MRS Bulletin, Vol. 45, Issue 9; ISSN 0883-7694
Publisher:
Materials Research SocietyCopyright Statement
Country of Publication:
United States
Language:
English

References (60)

Design of a Heated Liquid Cell for in-situ Transmission Electron Microscopy journal August 2015
Investigating local oxidation processes in Fe thin films in a water vapor environment by in situ liquid cell TEM journal February 2020
Application of In Situ Liquid Cell Transmission Electron Microscopy in Corrosion Studies: A Critical Review of Challenges and Achievements journal November 2019
Replicating Bulk Electrochemistry in Liquid Cell Microscopy journal August 2018
In Liquid Observation and Quantification of Nucleation and Growth of Gold Nanostructures Using in Situ Transmission Electron Microscopy journal March 2017
Localized corrosion of low-carbon steel at the nanoscale journal April 2019
Challenges for Rechargeable Li Batteries journal February 2010
Electrochemical Measurements in In Situ TEM Experiments journal January 2017
Advanced microelectromechanical systems-based nanomechanical testing: Beyond stress and strain measurements journal June 2019
Nanoscale Imaging of Lithium Ion Distribution During In Situ Operation of Battery Electrode and Electrolyte journal February 2014
Quantitative Electrochemical Measurements Using In Situ ec-S/TEM Devices journal March 2014
Determination of Redox Reaction Rates and Orders by In Situ Liquid Cell Electron Microscopy of Pd and Au Solution Growth journal November 2014
Defining the radiation chemistry during liquid cell electron microscopy to enable visualization of nanomaterial growth and degradation dynamics: DEFINING THE RADIATION CHEMISTRY DURING LCEM journal December 2016
Demonstration of an Electrochemical Liquid Cell for Operando Transmission Electron Microscopy Observation of the Lithiation/Delithiation Behavior of Si Nanowire Battery Anodes journal November 2013
Nanoscale Imaging of Fundamental Li Battery Chemistry: Solid-Electrolyte Interphase Formation and Preferential Growth of Lithium Metal Nanoclusters journal February 2015
Lithium Electrodeposition Dynamics in Aprotic Electrolyte Observed in Situ via Transmission Electron Microscopy journal February 2015
In-Situ Transmission Electron Microscopic Observation of Corrosion-Enhanced Dislocation Emission and Crack Initiation of Stress Corrosion journal May 2000
Controlling the spatio-temporal dose distribution during STEM imaging by subsampled acquisition: In-situ observations of kinetic processes in liquids journal August 2019
Liquid Cell TEM of the Corrosion of Metal Films in Aqueous Solutions journal July 2012
The Impact of Li Grain Size on Coulombic Efficiency in Li Batteries journal October 2016
In Situ Liquid Cell TEM Study of Morphological Evolution and Degradation of Pt–Fe Nanocatalysts During Potential Cycling journal September 2014
Opportunities and challenges in liquid cell electron microscopy journal December 2015
Liquid cell transmission electron microscopy observation of lithium metal growth and dissolution: Root growth, dead lithium and lithium flotsams journal February 2017
Dynamic microscopy of nanoscale cluster growth at the solid–liquid interface journal July 2003
Observation and Quantification of Nanoscale Processes in Lithium Batteries by Operando Electrochemical (S)TEM journal February 2015
Critical differences in 3D atomic structure of individual ligand-protected nanocrystals in solution journal April 2020
Liquid Cell Transmission Electron Microscopy Sheds Light on The Mechanism of Palladium Electrodeposition journal January 2019
In Situ Transmission Electron Microscopy of Lead Dendrites and Lead Ions in Aqueous Solution journal June 2012
Localised corrosion in aluminium alloy 2024-T3 using in situ TEM journal January 2013
In situ TEM study of the Li–Au reaction in an electrochemical liquid cell journal January 2014
Corrosion and Protection of Metals journal April 2020
Probing the Degradation Mechanisms in Electrolyte Solutions for Li-Ion Batteries by in Situ Transmission Electron Microscopy journal February 2014
Cryo-STEM mapping of solid–liquid interfaces and dendrites in lithium-metal batteries journal August 2018
In Situ Electron Diffraction Tomography Using a Liquid-Electrochemical Transmission Electron Microscopy Cell for Crystal Structure Determination of Cathode Materials for Li-Ion batteries journal September 2018
Structural and Morphological Evolution of Lead Dendrites during Electrochemical Migration journal November 2013
Control of Growth Front Evolution by Bi Additives during ZnAu Electrodeposition journal January 2018
Current Density Distribution in Electrochemical Cells with Small Cell Heights and Coplanar Thin Electrodes as Used in ec-S/TEM Cell Geometries journal January 2019
The morphology and nucleation kinetics of copper islands during electrodeposition journal May 2006
Metastable Structures in Al Thin Films Before the Onset of Corrosion Pitting as Observed using Liquid Cell Transmission Electron Microscopy journal February 2014
In Situ Study of Lithiation and Delithiation of MoS 2 Nanosheets Using Electrochemical Liquid Cell Transmission Electron Microscopy journal July 2015
Importance and Challenges of Electrochemical in Situ Liquid Cell Electron Microscopy for Energy Conversion Research journal August 2016
Ror2 signaling regulates Golgi structure and transport through IFT20 for tumor invasiveness journal January 2017
Charging/Discharging Nanomorphology Asymmetry and Rate-Dependent Capacity Degradation in Li–Oxygen Battery journal November 2015
Direct visualization of initial SEI morphology and growth kinetics during lithium deposition by in situ electrochemical transmission electron microscopy journal January 2014
Quantifying Electrochemical Nucleation and Growth of Nanoscale Clusters Using Real-Time Kinetic Data journal February 2006
Real-time imaging of activation and degradation of carbon supported octahedral Pt–Ni alloy fuel cell catalysts at the nanoscale using in situ electrochemical liquid cell STEM journal January 2019
Studying localized corrosion using liquid cell transmission electron microscopy journal January 2015
Direct Visualization of Solid Electrolyte Interphase Formation in Lithium-Ion Batteries with In Situ Electrochemical Transmission Electron Microscopy journal July 2014
A Sealed Liquid Cell for In Situ Transmission Electron Microscopy of Controlled Electrochemical Processes journal August 2015
Electron-stimulated purification of platinum nanostructures grown via focused electron beam induced deposition journal January 2015
Operando Monitoring of the Solution-Mediated Discharge and Charge Processes in a Na–O 2 Battery Using Liquid-Electrochemical Transmission Electron Microscopy journal January 2018
In situ analytical techniques for battery interface analysis journal January 2018
Lithium Self-Discharge and Its Prevention: Direct Visualization through In Situ Electrochemical Scanning Transmission Electron Microscopy journal September 2017
Emerging Electron Microscopy Techniques for Probing Functional Interfaces in Energy Materials journal January 2020
The Nanoaquarium: A Platform for In Situ Transmission Electron Microscopy in Liquid Media journal August 2010
In situ electrochemical wet cell transmission electron microscopy characterization of solid–liquid interactions between Ni and aqueous NiCl2 journal January 2012
Atomic structure of sensitive battery materials and interfaces revealed by cryo–electron microscopy journal October 2017
Practical Aspects of Electrochemical Corrosion Measurements During In Situ Analytical Transmission Electron Microscopy (TEM) of Austenitic Stainless Steel in Aqueous Media journal August 2017
Visualization of Electrode–Electrolyte Interfaces in LiPF 6 /EC/DEC Electrolyte for Lithium Ion Batteries via in Situ TEM journal March 2014
Experimental procedures to mitigate electron beam induced artifacts during in situ fluid imaging of nanomaterials journal April 2013