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ORIGINAL RESEARCH article

Front. Chem.
Sec. Catalytic Reactions and Chemistry
Volume 13 - 2025 | doi: 10.3389/fchem.2025.1525245
This article is part of the Research Topic Seeing Atomic Dynamics of Nanocatalysts during Reactions View all articles

In-Situ/Operando Study of Cu-based Nanocatalysts for CO2 Electroreduction Using Electrochemical Liquid Cell TEM

Provisionally accepted
Jiawei Wan Jiawei Wan 1,2Qiubo Zhang Qiubo Zhang 1Ershuai Liu Ershuai Liu 1Yi Chen Yi Chen 1,2Jiana Zheng Jiana Zheng 1,2Amy Ren Amy Ren 1Walter Drisdell Walter Drisdell 1Haimei Zheng Haimei Zheng 1*
  • 1 Lawrence Berkeley National Laboratory, Berkeley, United States
  • 2 University of California, Berkeley, Berkeley, California, United States

The final, formatted version of the article will be published soon.

    The structure of a nanocatalyst during electrocatalytic reactions often deviates from its pristine structure due to intrinsic properties, or physical and chemical adsorption at the catalytic surfaces. Taking Cu-based catalysts for CO2 electroreduction reactions (CO2RR) as an example, they often experience segregation, leaching, and alloying during reactions. With the recent breakthrough development of high-resolution polymer electrochemical liquid cells, in-situ electrochemical liquid cell transmission electron microscopy (EC-TEM) alongside other advanced microscopy techniques, has become a powerful platform for revealing electrocatalysts restructuring at the atomic level. Considering the complex reactions involving electrified solid-liquid interfaces and catalyst structural evolution with intermediates, systematic studies with multimodal approaches are crucial. In this article, we demonstrate a research protocol for the study of electrocatalysts structural evolution during reactions using the in-situ EC-TEM platform. Using Cu and CuAg nanowire catalysts for CO2RR as model systems, we describe the experimental procedures and findings. We highlight the platform's crucial role in elucidating atomic-scale pathways of nanocatalyst restructuring and identifying active catalytic sites, as well as avoiding potential artifacts to ensure unbiased conclusions. Using the multimodal characterization toolbox provides the opportunity to correlate the structure of a working catalyst with the performance. Finally, we discuss advancements as well as the remaining gap in elucidating the structural-performance relationship of working catalysts. We expect this article will assist in establishing guidelines for future investigations of complex electrochemical reactions, such as CO₂RR and other catalytic processes, using the in-situ EC-TEM platform.

    Keywords: electrochemical liquid cell TEM1, in-situ2, operando3, nanocatalysts4, Cu-based catalysts5, CO2 electroreduction6, nanocatalyst restructuring7

    Received: 09 Nov 2024; Accepted: 14 Jan 2025.

    Copyright: © 2025 Wan, Zhang, Liu, Chen, Zheng, Ren, Drisdell and Zheng. This is an open-access article distributed under the terms of the Creative Commons Attribution License (CC BY). The use, distribution or reproduction in other forums is permitted, provided the original author(s) or licensor are credited and that the original publication in this journal is cited, in accordance with accepted academic practice. No use, distribution or reproduction is permitted which does not comply with these terms.

    * Correspondence: Haimei Zheng, Lawrence Berkeley National Laboratory, Berkeley, United States

    Disclaimer: All claims expressed in this article are solely those of the authors and do not necessarily represent those of their affiliated organizations, or those of the publisher, the editors and the reviewers. Any product that may be evaluated in this article or claim that may be made by its manufacturer is not guaranteed or endorsed by the publisher.