Tailored Selectivity for CO and C<sub>2+</sub> in CO<sub>2</sub> Reduction: Insights into the Dynamic Evolution of Electrocatalysts

L Lu Liu Y Yuke Li (Department of Mechanical and Industrial Engineering) K Kher Ai Chiaw (Institute of Sustainability for Chemicals, Energy and Environment (ISCE2) Agency of Science, Technology, and Research (A*STAR) Singapore 627833 Singapore) S Shibo Xi S Shuying Cheng (Institute of Sustainability for Chemicals, Energy and Environment (ISCE2) Agency of Science, Technology, and Research (A*STAR) Singapore 627833 Singapore) S Shashikant U. Dighe (Institute of Sustainability for Chemicals, Energy and Environment (ISCE2) Agency of Science, Technology, and Research (A*STAR) Singapore 627833 Singapore) H Huaiyu Chang B Boon Ying Tay (Institute of Sustainability for Chemicals, Energy and Environment (ISCE2) Agency of Science, Technology, and Research (A*STAR) Singapore 627833 Singapore) M Mingwu Tan K Kuo‐Wei Huang (Center for Renewable Energy and Storage Technologies (CREST) KAUST Catalysis Center (KCC) Physical Science and Engineering Division King Abdullah University of Science and Technology Thuwal 23955 Saudi Arabia) L Linfei Lai (Jiangsu Natl Synergist Innovat Ctr, Adv Mat SICAM, Key Lab Flexible Nanjing Tech University Elect, 5 XinMofan Rd Nanjing 210009 P.R China) Y Yingqing Ou (Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore) L Lili Zhang

Abstract

AbstractControlling product selectivity in electrochemical CO2 reduction (eCO2R) is critical for efficient CO2 conversion. However, the dynamic structural changes of Cu‐based catalysts during operation complicate mechanistic understanding. Here, we investigate fluorine‐modified copper pre‐catalysts with varying doping levels and reveal how their structural evolution governs eCO2R activity and selectivity. Through operando spectroscopy characterizations and theoretical simulations, we show that fluorine leaches rapidly during electrolysis, transforming Cu2⁺ precursors into metallic Cu⁰ with distinct local structures. Cu‐F‐4, with the lowest coordination number, exhibits high eCO2R activity and favors CO formation with a Faradaic efficiency (FECO) of 81% at −0.45 V. In contrast, Cu‐F‐1, enriched in grain boundaries and Cu(100) facets, achieves a high FEC2+ of 80% at −0.65 V. Differences in local pH, *OH coverage, and *CO binding energies further modulate catalytic pathways. Our findings highlight the importance of dynamic catalyst reconstruction in steering product selectivity and offer design principles for advancing CO2‐to‐chemicals conversion.

Article Details

Volume / Issue Vol. 64, Issue 40
Published September 26, 2025
ISSN 1433-7851
Publisher Wiley

Journal Info

Angewandte Chemie International Edition

Wiley

ISSN: 1433-7851 Physical Sciences

Authors (13)

L

Lu Liu

Y

Yuke Li

Department of Mechanical and Industrial Engineering

K

Kher Ai Chiaw

Institute of Sustainability for Chemicals, Energy and Environment (ISCE2) Agency of Science, Technology, and Research (A*STAR) Singapore 627833 Singapore

S

Shibo Xi

S

Shuying Cheng

Institute of Sustainability for Chemicals, Energy and Environment (ISCE2) Agency of Science, Technology, and Research (A*STAR) Singapore 627833 Singapore

S

Shashikant U. Dighe

Institute of Sustainability for Chemicals, Energy and Environment (ISCE2) Agency of Science, Technology, and Research (A*STAR) Singapore 627833 Singapore

H

Huaiyu Chang

B

Boon Ying Tay

Institute of Sustainability for Chemicals, Energy and Environment (ISCE2) Agency of Science, Technology, and Research (A*STAR) Singapore 627833 Singapore

M

Mingwu Tan

K

Kuo‐Wei Huang

Center for Renewable Energy and Storage Technologies (CREST) KAUST Catalysis Center (KCC) Physical Science and Engineering Division King Abdullah University of Science and Technology Thuwal 23955 Saudi Arabia

L

Linfei Lai

Jiangsu Natl Synergist Innovat Ctr, Adv Mat SICAM, Key Lab Flexible Nanjing Tech University Elect, 5 XinMofan Rd Nanjing 210009 P.R China

Y

Yingqing Ou

Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore

L

Lili Zhang