Operando probing dynamic migration of copper carbonyl during electrocatalytic CO2 reduction

Yang, Yao; Feijóo, Julian; Figueras-Valls, Marc; Chen, Chubai; Shi, Chuqiao; Fonseca Guzman, Maria V.; Murhabazi Maombi, Yves; Liu, Shikai; Jain, Pulkit; Briega-Martos, Valentín; Peng, Zhengxing; Shan, Yu; Lee, Geonhui; Rebarchik, Michael; Xu, Lang; Pollock, Christopher J.; Jin, Jianbo; Soland, Nathan E.; Wang, Cheng; Salmeron, Miquel B.; Chen, Zhu; Han, Yimo; Mavrikakis, Manos; Yang, Peidong

doi:10.1038/s41929-025-01359-w

Operando probing dynamic migration of copper carbonyl during electrocatalytic CO₂ reduction

Journal Article · Tue Jun 24 20:00:00 EDT 2025 · Nature Catalysis

DOI:https://doi.org/10.1038/s41929-025-01359-w· OSTI ID:3008732

^[1]; ^[2]; Figueras-Valls, Marc ^[3]; ^[2]; ^[4]; ^[2]; Murhabazi Maombi, Yves ^[5]; Liu, Shikai ^[6]; Jain, Pulkit ^[5]; ^[6]; ^[7]; ^[2]; Lee, Geonhui ^[8]; ^[3]; ^[3]; ^[6]; ^[8]; Soland, Nathan E. ^[8]; Wang, Cheng ^[7]; ^[2] more »

University of California, Berkeley, CA (United States); Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States); Cornell University, Ithaca, NY (United States)
University of California, Berkeley, CA (United States); Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
University of Wisconsin, Madison, WI (United States)
Rice University, Houston, TX (United States)
University of Massachusetts, Amherst, MA (United States)
Cornell University, Ithaca, NY (United States)
Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS)
University of California, Berkeley, CA (United States)

Single crystals and shape-controlled nanocrystals are well known to exhibit facet-dependent catalytic properties. However, few studies have investigated how those nanocrystals evolve and (de)activate during reactions, calling for the development of nanoscale time-resolved operando methods. Here, in this context, we have designed Cu nanocubes as a model system to elucidate the underlying driving force of dynamic nanocatalyst reconstruction during the CO₂ reduction reaction (CO₂RR). Operando electrochemical liquid-cell scanning transmission electron microscopy (EC-STEM) and synchrotron-based X-ray spectroscopy reveal the size- and potential-dependent complete transformation from (100)-oriented Cu@Cu₂O nanocubes to polycrystalline metallic Cu nanograins under CO₂RR conditions. In addition, machine learning-assisted operando four-dimensional STEM reveals that large Cu nanograins derived from nanocubes form mainly crystalline domains, while their smaller counterparts are more amorphous due to faster evolution kinetics. In situ Raman spectroscopy and density functional theory calculations suggest that CO drives the ejection of single Cu atoms, resulting in few-nanometre Cu clusters and the surface migration of highly mobile copper carbonyl (Cu–CO) species. Combined, these multimodal operando methods and theoretical approaches pave the way for understanding the complex structural evolution of energy-related nanocatalysts under electrochemical conditions.

View Accepted Manuscript (DOE)

Research Organization:: Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences & Biosciences Division (CSGB); USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF); National Institutes of Health (NIH); National Science Foundation (NSF); Robert A. Welch Foundation

Grant/Contract Number:: SC0019445; AC02-05CH11231; FG02-05ER15731

OSTI ID:: 3008732

Journal Information:: Nature Catalysis, Journal Name: Nature Catalysis Journal Issue: 6 Vol. 8; ISSN 2520-1158

Publisher:: Springer NatureCopyright Statement

Country of Publication:: United States

Language:: English

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