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Electrochemical Behavior of Carbon Electrodes for In Situ Redox Studies in a Transmission Electron Microscope

Published online by Cambridge University Press:  24 October 2019

Robin Girod ,
Nikolaos Nianias  and
Vasiliki Tileli Open the ORCID record for Vasiliki Tileli [Opens in a new window]
Robin Girod
Affiliation:
Institute of Materials, Ecole Polytechnique Fédérale de Lausanne, Lausanne CH-1015, Switzerland
Nikolaos Nianias
Affiliation:
Institute of Materials, Ecole Polytechnique Fédérale de Lausanne, Lausanne CH-1015, Switzerland
Vasiliki Tileli*
Affiliation:
Institute of Materials, Ecole Polytechnique Fédérale de Lausanne, Lausanne CH-1015, Switzerland
*
*Author for correspondence: Vasiliki Tileli, E-mail: vasiliki.tileli@epfl.ch
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Abstract

Electrochemical liquid cell transmission electron microscopy (TEM) is a unique technique for probing nanocatalyst behavior during operation for a range of different electrocatalytic processes, including hydrogen evolution reaction (HER), oxygen evolution reaction (OER), oxygen reduction reaction (ORR), or electrochemical CO2 reduction (eCO2R). A major challenge to the technique's applicability to these systems has to do with the choice of substrate, which requires a wide inert potential range for quantitative electrochemistry, and is also responsible for minimizing background gas generation in the confined microscale environment. Here, we report on the feasibility of electrochemical experiments using the standard redox couple Fe(CN)63−/4− and microchips featuring carbon-coated electrodes. We electrochemically assess the in situ performance with respect to flow rate, liquid volume, and scan rate. Equally important with the choice of working substrate is the choice of the reference electrode. We demonstrate that the use of a modified electrode setup allows for potential measurements relatable to bulk studies. Furthermore, we use this setup to demonstrate the inert potential range for carbon-coated electrodes in aqueous electrolytes for HER, OER, ORR, and eCO2R. This work provides a basis for understanding electrochemical measurements in similar microscale systems and for studying gas-generating reactions with liquid electrochemical TEM.

Keywords

carbon microelectrodeseCO2Relectrocatalysisin situ TEMORR
Type
Software and Instrumentation
Information
Microscopy and Microanalysis , Volume 25 , Issue 6 , December 2019 , pp. 1304 - 1310
Copyright
Copyright © Microscopy Society of America 2019 

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