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Interfacial Electrochemical Methods: Overview

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Interfacial electrochemical methods focus on the phenomena occurring at the boundary between an electrode and a solution, as opposed to bulk methods that concentrate on the solution's overall properties. These interfacial methods are classified as either static or dynamic based on the presence of a nonzero current in the electrochemical cell and the consistency of analyte concentrations. Static methods, such as potentiometry, measure the cell's potential without any significant current...

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Updated: Sep 20, 2025

Nanoscale Characterization of Liquid-Solid Interfaces by Coupling Cryo-Focused Ion Beam Milling with Scanning Electron Microscopy and Spectroscopy

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Published on: July 14, 2022

Operando Heating and Cooling Electrochemical 4D-STEM Probing Nanoscale Dynamics at Solid-Liquid Interfaces.

Sungin Kim¹, Valentin Briega-Martos¹, Shikai Liu¹

¹Department of Chemistry and Chemical Biology, Baker Lab, Cornell University, Ithaca, New York 14853, United States.

Journal of the American Chemical Society

|May 23, 2025

Summary

This summary is machine-generated.

We developed a new operando heating and cooling electrochemical liquid-cell scanning transmission electron microscopy (EC-STEM) to study nanoscale electrochemical processes. This powerful tool allows for precise control of temperature and electrochemistry, enabling the investigation of energy materials in extreme climates.

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Area of Science:

Materials Science
Electrochemistry
Analytical Chemistry

Background:

Operando/in situ methods, such as transmission electron microscopy (TEM), allow real-time observation of chemical and structural changes at interfaces.
Existing electrochemical liquid-cell TEM often lacks simultaneous thermal control, limiting studies of materials under varying temperatures.
Understanding nanoscale electrochemical dynamics under diverse thermal conditions is crucial for developing advanced energy technologies.

Purpose of the Study:

To develop and demonstrate an operando heating and cooling electrochemical liquid-cell scanning TEM (EC-STEM) system.
To investigate the temperature dependence of electrochemical processes and material growth at the nanoscale.
To enable the study of energy materials under realistic, extreme climate conditions.

Main Methods:

Integration of a three-electrode electrochemical circuit and a two-electrode thermal circuit into a liquid-cell scanning TEM.
Utilizing copper electrodeposition/stripping as a model system for quantitative electrochemistry from -40 to 95 °C.
Employing machine learning-assisted quantitative 4D-STEM for structural analysis at -40 °C.

Main Results:

Demonstrated quantitative electrochemistry in aqueous and organic solutions across a wide temperature range (-40 to 95 °C).
Observed a distinct two-stage growth mechanism of copper nanostructures (mossy islands followed by dendrites) at -40 °C.
Characterized the temperature and pH dependence of a platinum pseudoreference electrode, confirming its stability.

Conclusions:

The developed operando heating/cooling EC-STEM is a powerful tool for fundamental nanoscale electrochemistry research.
This technique facilitates the investigation of energy materials operating in extreme climates, advancing battery and catalyst technologies.
The findings provide insights into temperature-controlled nanoscale electrochemical phenomena and material morphology evolution.