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Unveiling the reconstruction of copper bimetallic catalysts during CO2 electroreduction

Nature Catalysis volume 8, pages 697–713 (2025)Cite this article

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Abstract

Efficient electrocatalysts should provide optimal binding sites for intermediates under operating conditions. Atomic rearrangements in catalysts during electrochemical CO2 reduction reaction (CO2RR) alter the original structures of active sites. Here we report a general principle for understanding and predicting the reconstruction of Cu bimetallic catalysts during CO2RR in terms of selective dissolution–redeposition. We categorize the reconstruction trends of Cu bound to a secondary metal (X, where X = Ag, Fe, Zn or Pd) according to the oxophilicity and miscibility of Cu and X. Cross-sectional microscopy analysis of gas diffusion electrodes reveals that the surface states of reconstructed Cu–X are determined by atomic miscibility. We find that CO2RR intermediates alter elemental preferences for dissolution, shifting them away from oxophilicity-governed behaviour and leading to selective Cu dissolution–redeposition in Cu–X. This reconstruction affects spillover in CO2RR, controlling the selectivities of ethylene/ethanol and C1/C2 products. We also develop a methodology for the control of reconstruction dynamics. Our findings provide insights into designing catalysts that undergo reconstruction during electrolysis.

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Fig. 1: Strategies for uncovering Cu bimetallic catalyst reconstruction in MEA-based CO2RR.
Fig. 2: Surface structural evolution of Cu–X catalysts by CO2RR.
Fig. 3: Elemental redistribution of Cu–X catalysts by CO2RR.
Fig. 4: Real-time observation of structural evolution in Cu–X catalysts during CO2RR.
Fig. 5: Mechanistic studies on the reconstruction of Cu–X catalysts.
Fig. 6: Correlation between CO2RR performance and the reconstruction of Cu and Cu–X catalysts.
Fig. 7: Effects of pulsed activation on Cu–X reconstruction and CO2RR selectivity.

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Data availability

The optimized computational models are provided as Supplementary Data. In situ e-LCTEM recordings are provided as Supplementary Videos 1 and 2. Source data are provided with this paper. All other data supporting the findings of this study are available from the corresponding authors upon reasonable request.

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Acknowledgements

This research was supported by National Research Foundation of Korea (NRF) grants funded by the Korean government’s Ministry of Science and ICT (MSIT) (RS-2021-NR061733 and NRF-2021M3D1A2047041 to D.-H.N.). Y.-C.J. acknowledges support from the Creative Materials Discovery Program through the NRF, funded by MSIT and Future Planning (2017M3D1A1040689), as well as from an NRF grant funded by the Korean government’s MSIT (RS-2024-00457199). J.P. acknowledges support from the NRF, funded by MSIT (RS-2024-00421181 and RS-2024-00449965). S.B. acknowledges the support from the Nano and Material Technology Development Program through the NRF funded by MSIT (RS-2024-00406517) and generous supercomputing time from Korea Institute of Science and Technology Information. We acknowledge support received from the Hanwha Solutions Chemical Division. We thank B. Jeon, G. Kim and K. Seob Song of the Catalysis Technology Center of the Hanwha Solutions Chemical Division for valuable support. Material characterization, including grazing incidence XRD, SEM and TEM analyses, was supported by the Research Institute of Advanced Materials and National Center for Inter-University Research Facilities at Seoul National University. ICP-MS, NMR analysis and FIB preparation were supported by the National Instrumentation Center for Environmental Management at Seoul National University. XPS analysis was supported by the Korea Institute of Ceramic Engineering and Technology. Experiments at Pohang Light Source II were supported in part by MSIT and Pohang University of Science and Technology.

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Author notes

  1. Sungin Kim

    Present address: Department of Chemistry and Chemical Biology, Cornell University, Ithaca, NY, USA

  2. These authors contributed equally: Intae Kim, Gi-Baek Lee, Sungin Kim, Hyun Dong Jung.

Authors and Affiliations

  1. Department of Materials Science and Engineering, Seoul National University, Seoul, Republic of Korea

    Intae Kim, Gi-Baek Lee, Ji-Yong Kim, Jaeyeon Jo, Geosan Kang, Sang-Ho Oh, Deokgi Hong, Hyoung Gyun Kim, Unggi Kim, Hyeontae Kim, Miyoung Kim & Young-Chang Joo

  2. Department of Chemical and Biological Engineering, Institute of Chemical Processes, Seoul National University, Seoul, Republic of Korea

    Sungin Kim, Hyesung Choi & Jungwon Park

  3. Center for Nanoparticle Research, Institute for Basic Science, Seoul, Republic of Korea

    Sungin Kim, Hyesung Choi & Jungwon Park

  4. Department of Chemical and Biomolecular Engineering, Institute of Emergent Materials, Sogang University, Seoul, Republic of Korea

    Hyun Dong Jung

  5. Department of Energy Science and Engineering, Daegu Gyeongbuk Institute of Science and Technology, Daegu, Republic of Korea

    Taemin Lee, Woosuck Kwon & Dae-Hyun Nam

  6. Department of Materials Science and Engineering, Korea University, Seoul, Republic of Korea

    Yujin Lee & Dae-Hyun Nam

  7. KU-KIST Graduate School of Converging Science and Technology, Korea University, Seoul, Republic of Korea

    Seoin Back

  8. Department of Integrative Energy Engineering, Korea University, Seoul, Republic of Korea

    Seoin Back

  9. Institute of Engineering Research, College of Engineering, Seoul National University, Seoul, Republic of Korea

    Jungwon Park

  10. Advanced Institute of Convergence Technology, Seoul National University, Suwon, Republic of Korea

    Jungwon Park

  11. Research Institute of Advanced Materials, Seoul National University, Seoul, Republic of Korea

    Young-Chang Joo

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  1. Intae Kim
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Contributions

D.-H.N., Y.-C.J., J.P. and S.B. designed and supervised the overall project. I.K., G.-B.L., S.K. and H.D.J. conceived of the idea and conducted the experiments. I.K. and G.-B.L. carried out electrode fabrication, characterization and electrochemical measurements. S.K. performed the e-LCTEM experiments with assistance from H.C. under the supervision of J.P. H.D.J. conducted the DFT calculations and analyses under the supervision of S.B. J.-Y.K. contributed to CO2RR performance evaluation. T.L. carried out the real-time XAS and Raman analyses with the assistance of Y.L. J.J. performed the high-resolution TEM EDS. H.G.K. contributed to TEM measurement under the supervision of M.K. G.K. contributed to thermodynamic calculations. S.-H.O. contributed to SEM measurement and analysis. W.K. contributed to XPS analysis. D.H. and J.-Y.K. contributed to data analysis. U.K. contributed to fabrication. H.K. contributed to SEM EDS analysis of the segmented electrodes. All authors discussed the results and contributed to writing the paper.

Corresponding authors

Correspondence to Seoin Back, Jungwon Park, Young-Chang Joo or Dae-Hyun Nam.

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Supplementary information

Supplementary Information

Supplementary Notes 1–6, Figs. 1–90 and Tables 1 and 2.

Supplementary Video 1

In situ e-LCTEM of a Cu–Ag thin film during CO2RR using a CO2-saturated 0.1 M KHCO3 electrolyte at an applied potential of −0.8 V (versus the RHE) for 160 s.

Supplementary Video 2

In situ e-LCTEM of a Cu–Zn thin film during CO2RR at an applied potential of −0.8 V (versus the RHE) for 600 s.

Supplementary Data 1

Optimized computational models.

Source data

Source Data Fig. 1

Statistical source data.

Source Data Fig. 4

Statistical source data.

Source Data Fig. 5

Statistical source data.

Source Data Fig. 6

Statistical source data.

Source Data Fig. 7

Statistical source data.

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Kim, I., Lee, GB., Kim, S. et al. Unveiling the reconstruction of copper bimetallic catalysts during CO2 electroreduction. Nat Catal 8, 697–713 (2025). https://doi.org/10.1038/s41929-025-01368-9

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