Electrochemical CO2RR to C2+ products: A vision of dynamic surfaces of Cu-based catalysts

doi:10.1016/S1872-2067(24)60185-3

Abstract

Abstract:

Electrochemical reduction of CO₂ (CO₂RR) to form high-energy-density and high-value-added multicarbon products has attracted much attention. Selective reduction of CO₂ to C₂₊ products face the problems of low reaction rate, complex mechanism and low selectivity. Currently, except for a few examples, copper-based catalysts are the only option capable of achieving efficient generation of C₂₊ products. However, the continuous dynamic reconstruction of the catalyst causes great difficulty in understanding the structure-performance relationship of CO₂RR. In this review, we first discuss the mechanism of C₂₊ product generation. The structural factors promoting C₂₊ product generation are outlined, and the dynamic evolution of these structural factors is discussed. Furthermore, the effects of electrolyte and electrolysis conditions are reviewed in a vision of dynamic surface. Finally, further exploration of the reconstruction mechanism of Cu-based catalysts and the application of emerging robotic AI chemists are discussed.

Key words: Electrocatalysis, CO₂RR, Cu-based catalyst, Reconstruction, Multicarbon product, Structural evolution

Jinxin Wang, Jiaqi Zhang, Chen Chen. Electrochemical CO₂RR to C₂₊ products: A vision of dynamic surfaces of Cu-based catalysts[J]. Chinese Journal of Catalysis, 2025, 68: 83-102.

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Figures/Tables 11

Fig. 1. Overview of catalyst surface reconstruction, its regulation strategies for CO2 reduction reactions, and the evolution mechanisms for CO2RR-to-C2+ products discussed in this review.

Fig. 2. Schematic representation of the possible routes of CO2RR to various value-added products. CO2 is the initial reactant and CO is the key intermediate, with C2 and C3 products formed through coupling between intermediates. Arrows indicate proton and electron transfer to oxygen or carbon sites.

Fig. 3. (a) Catalytic properties of the Cu nanocatalysts with different facets in CO2RR. Reprinted with permission from Ref. [43]. Copyright 2020, American Chemical Society. (b) The activation energy barrier of CO dimerization on different facets. Reprinted with permission from Ref. [42]. Copyright 2016, American Chemical Society. (c) The highest C2+/C1 ratio of polished Cu, 10-cycled Cu and 100-cycled Cu. Reprinted with permission from Ref. [45]. Copyright 2018, Springer Nature. (d) Schematic depiction of the influence of the coverage of *CO. Reprinted with permission from Ref. [41]. Copyright 2017, American Chemical Society. (e) Formation of C2H4 on the (100) facets of c-Cu2O NPs, (111) facets of o-Cu2O NPs, and (100) and (111) facets of t-Cu2O NPs. Reprinted with permission from Ref. [54]. Copyright 2020, John Wiley and Sons.

Fig. 4. (a) CNs of adparticles with different sizes on various crystalline facets. Reprinted with permission from Ref. [58]. Copyright 2018, Springer Nature. (b) Better selectivity of n-propanol obtained on the catalyst with adparticles [46]. Copyright 2024, American Chemical Society. (c,d) Size dependence of catalytic performance of Cu nanocubes [60]. Copyright 2016, John Wiley and Sons. (e) Schematic diagram of manipulating CN via pulsed electrolysis. (f) CNs obtained from EXAFS. Reprinted with permission from Ref. [59]. Copyright 2024, American Chemical Society.

Fig. 5. (a) The synergistic effect of Cu(0) and Cu(I) sites. Reprinted with permission from Ref. [66]. Copyright 2020, American Chemical Society. (b) Selectivity of catalysts with and without molecular doping. Reprinted with permission from Ref. [71]. Copyright 2021, Springer Nature. (c) Long-time catalytic performance with changing ratio of Cu(I). Reprinted with permission from Ref. [69]. Copyright 2015, John Wiley and Sons. (d) The ability to preserve Cu(I) of Cu-on-Cu3N catalyst characterized via in situ XAS. Reprinted with permission from Ref. [72]. Copyright 2018, Springer Nature.

Fig. 6. (a) Schematic diagram of the morphology evolution of terraced field-like Cu electrode. Reprinted with permission from Ref. [78]. Copyright 2020, John Wiley and Sons. (b) Morphology evolution of Cu NCs observed with operando EC-AFM. Reprinted with permission from Ref. [4]. Copyright 2018, John Wiley and Sons. (c) Observation of the grain boundary utilizing SECCM. Reprinted with permission from Ref. [79]. Copyright 2021, Springer Nature. (d) The reconstruction mechanism of Cu NCs with two distinct stages. Reprinted with permission from Ref. [7]. Copyright 2018, Springer Nature. (e) The distortion and aggregation of Cu NPs to nanograins. (f) Size dependence of catalytic performance of Cu NPs. Reprinted with permission from Ref. [74]. Copyright 2023, Springer Nature.

Fig. 7. (a) Ratio of Cu oxidation states with respect to time at ?1.2 V RHE. Reprinted with permission from Ref. [23]. Copyright 2018, Springer Nature. (b) 6O and 18O contents of the Cu plates after 24? h oxidizing corrosion, measured by TOF-SIMS. (c) Schematic diagram of the reoxidation of Cu(0). Reprinted with permission from Ref. [6]. Copyright 2022, Springer Nature. (d) The Pourbaix diagram of Cu with applied potential and pH as variants. (e) EPR spectra of the corresponding solutions containing 100mmol L?1 DMPO after 24 h resting. (f) Raman spectra of surface Cu2O species at ?0.3 V RHE for 10 s in the electrolyte containing KHC16O3 and H218O. (g) Raman spectra of carbonate species on the Cu electrode in different electrolyte. Reprinted with permission from Ref. [6]. Copyright 2022, Springer Nature.

Fig. 8. (a) Reconstruction of CuxO to metallic Cu and the ratio of low-coordinated Cu before/after the reconstruction. Reprinted with permission from Ref. [82]. Copyright 2024, John Wiley and Sons. (b) Simulated final structures for the reconstruction of CuO and Cu2O. Reprinted with permission from Ref. [35]. Copyright 2023, The American Association for the Advancement of Science. (c) Schematic diagram of confined carbon intermediates. Reprinted with permission from Ref. [83]. Copyright 2020, American Chemical Society. (d) SEM images of the Cu2P2O7 catalyst before electrolysis. (e) SEM images of the Cu2P2O7 catalyst after electrolysis. Reprinted with permission from Ref. [84]. Copyright 2021, John Wiley and Sons.

Fig. 9. (a) TEM images of potential-dependent molecular-scale Cu(100) surface structure and corresponding Raman spectra. Reprinted with permission from Ref. [8]. Copyright 2023, Springer Nature. (b) HRTEM image shows three phases. (c) The behaviour of amorphous Cu in ESLIs. (d,e) Atomic-scale mechanism of surface roughening. Reprinted with permission from Ref. [88]. Copyright 2024, Springer Nature. (f) Schematic diagram of the working principle of the quantitative analysis of Cu(I) transient species. (g) Cu concentration quantified via UV-vis and ICP-MS. Reprinted with permission from Ref. [89]. Copyright 2024, Springer Nature. (h) Quasi-kinetic Monte Carlo simulations of *H and *CO coverages evolution (left) and the vertical displacement map of Cu with *H and *CO coverages as variants (right). (i) Structures with rearranged Cu atoms under different coverage of *H and *CO. (j) Possible mechanism of Cu*CO dimerization. Reprinted with permission from Ref. [86]. Copyright 2024, American Chemical Society.

Fig. 10. (a) In situ SEIRAS spectra of adsorbed CO in 0.1 mol L?1 NaHCO3 and 0.1 mol L?1 KHCO3. ΔGs for hydrogenation (b) and dimerization (c) of *CO. Reprinted with permission from Ref. [92]. Copyright 2024, American Chemical Society. In situ ATR-SEIRAS collected in CO2-saturated 0.05 mol L?1 H2SO4 (d) and 0.05 mol L?1 H2SO4 + 1 mol L?1 Na2SO4 (e). Reprinted with permission from Ref. [11]. Copyright 2024, Springer Nature. (f) The dependence of band intensity of adsorbed CO2 on cation concentration. Reprinted with permission from Ref. [11]. Copyright 2024, Springer Nature. (g) Schematic illustration of the influence of different cation on *CO. Reprinted with permission from Ref. [93]. Copyright 2024, American Chemical Society. (h) TEM images showing the alkali cation-induced corrosion. (i) Voltammetric profiles of the Cu NCs recorded after electrolysis in different electrolyte. Reprinted with permission from Ref. [10]. Copyright 2024, Springer Nature.

Fig. 11. (a) FE of ethylene during electrolysis using alternating “on” and “off” segments with PTFE/Cu GDE at the current density of 150 mA cm-2. Reprinted with permission from Ref. [102]. Copyright 2024, American Chemical Society. (b) Schematic diagram of reduction and reoxidation of the catalyst in pulsed electrolysis. (c) FE of C2H4 for a continuous operation and the two pulsed electrolysis experiments. Reprinted with permission from Ref. [103]. Copyright 2024, American Chemical Society. (d) A schematic illustration of the coverages of *OH, *CO and *O in different pulsed modes. Reprinted with permission from Ref. [104]. Copyright 2024, Springer Nature. (e) Mappings of the Raman spectra acquired during pulsed CORR. (f) Evolution of Raman spectra within one pulse cycle. Reprinted with permission from Ref. [105]. Copyright 2023, American Chemical Society. (g) AFM images showing the reconstructed morphology after potentiostatic or pulsed electrolysis. Reprinted with permission from Ref. [106]. Copyright 2020, Springer Nature. (h) Intensity fits of COr, COs, OHad and Cu-Oad bands obtained from SERS. Reprinted with permission from Ref. [104]. Copyright 2024, Springer Nature.

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Electrochemical CO₂RR to C₂₊ products: A vision of dynamic surfaces of Cu-based catalysts

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