In-situ/operando study of Cu-based nanocatalysts for CO2 electroreduction using electrochemical liquid cell TEM

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 expe...

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Main Authors: Jiawei Wan, Qiubo Zhang, Ershuai Liu, Yi Chen, Jiana Zheng, Amy Ren, Walter S. Drisdell, Haimei Zheng
Format: Article
Language:English
Published: Frontiers Media S.A. 2025-01-01
Series:Frontiers in Chemistry
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Online Access:https://www.frontiersin.org/articles/10.3389/fchem.2025.1525245/full
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author Jiawei Wan
Jiawei Wan
Qiubo Zhang
Ershuai Liu
Ershuai Liu
Yi Chen
Yi Chen
Jiana Zheng
Jiana Zheng
Amy Ren
Walter S. Drisdell
Walter S. Drisdell
Haimei Zheng
Haimei Zheng
author_facet Jiawei Wan
Jiawei Wan
Qiubo Zhang
Ershuai Liu
Ershuai Liu
Yi Chen
Yi Chen
Jiana Zheng
Jiana Zheng
Amy Ren
Walter S. Drisdell
Walter S. Drisdell
Haimei Zheng
Haimei Zheng
author_sort Jiawei Wan
collection DOAJ
description 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 catalytic active sites, as well as avoiding potential artifacts to ensure unbiased conclusions. Using the multimodal characterization toolbox, we provide the opportunity to correlate the structure of a working catalyst with its 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.
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institution Kabale University
issn 2296-2646
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publishDate 2025-01-01
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spelling doaj-art-27650036af974789a883de8dc61cb76d2025-01-30T06:23:04ZengFrontiers Media S.A.Frontiers in Chemistry2296-26462025-01-011310.3389/fchem.2025.15252451525245In-situ/operando study of Cu-based nanocatalysts for CO2 electroreduction using electrochemical liquid cell TEMJiawei Wan0Jiawei Wan1Qiubo Zhang2Ershuai Liu3Ershuai Liu4Yi Chen5Yi Chen6Jiana Zheng7Jiana Zheng8Amy Ren9Walter S. Drisdell10Walter S. Drisdell11Haimei Zheng12Haimei Zheng13Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA, United StatesDepartment of Materials Science and Engineering, University of California, Berkeley, Berkeley, CA, United StatesMaterials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA, United StatesChemical Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA, United StatesLiquid Sunlight Alliance, Lawrence Berkeley National Laboratory, Berkeley, CA, United StatesMaterials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA, United StatesDepartment of Materials Science and Engineering, University of California, Berkeley, Berkeley, CA, United StatesMaterials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA, United StatesDepartment of Materials Science and Engineering, University of California, Berkeley, Berkeley, CA, United StatesMaterials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA, United StatesChemical Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA, United StatesLiquid Sunlight Alliance, Lawrence Berkeley National Laboratory, Berkeley, CA, United StatesMaterials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA, United StatesDepartment of Materials Science and Engineering, University of California, Berkeley, Berkeley, CA, United StatesThe 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 catalytic active sites, as well as avoiding potential artifacts to ensure unbiased conclusions. Using the multimodal characterization toolbox, we provide the opportunity to correlate the structure of a working catalyst with its 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.https://www.frontiersin.org/articles/10.3389/fchem.2025.1525245/fullelectrochemical liquid cell TEMin-situoperandonanocatalystsCu-based catalystsCO2 electroreduction
spellingShingle Jiawei Wan
Jiawei Wan
Qiubo Zhang
Ershuai Liu
Ershuai Liu
Yi Chen
Yi Chen
Jiana Zheng
Jiana Zheng
Amy Ren
Walter S. Drisdell
Walter S. Drisdell
Haimei Zheng
Haimei Zheng
In-situ/operando study of Cu-based nanocatalysts for CO2 electroreduction using electrochemical liquid cell TEM
Frontiers in Chemistry
electrochemical liquid cell TEM
in-situ
operando
nanocatalysts
Cu-based catalysts
CO2 electroreduction
title In-situ/operando study of Cu-based nanocatalysts for CO2 electroreduction using electrochemical liquid cell TEM
title_full In-situ/operando study of Cu-based nanocatalysts for CO2 electroreduction using electrochemical liquid cell TEM
title_fullStr In-situ/operando study of Cu-based nanocatalysts for CO2 electroreduction using electrochemical liquid cell TEM
title_full_unstemmed In-situ/operando study of Cu-based nanocatalysts for CO2 electroreduction using electrochemical liquid cell TEM
title_short In-situ/operando study of Cu-based nanocatalysts for CO2 electroreduction using electrochemical liquid cell TEM
title_sort in situ operando study of cu based nanocatalysts for co2 electroreduction using electrochemical liquid cell tem
topic electrochemical liquid cell TEM
in-situ
operando
nanocatalysts
Cu-based catalysts
CO2 electroreduction
url https://www.frontiersin.org/articles/10.3389/fchem.2025.1525245/full
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