Unraveling the Ni-Co synergy in bifunctional hydroxide cocatalysts for better cooperation of CO2 reduction and H2O oxidation in 2D S-scheme photosynthetic systems

doi:10.1016/S1872-2067(24)60174-9

Abstract

Abstract:

Layered transition metal hydroxides show distinct advantages in separately co-catalyzing CO₂ reduction and H₂O oxidation at the electron-accumulating and hole-accumulating sites of wrapped heterojunction photocatalysts, while concurrently preventing side reactions and photocorrosion on the semiconductor surface. Herein, Ni-Co bimetallic hydroxides with varying Ni/Co molar ratios (Ni_xCo_1-_x(OH)₂, x = 1, 0.75, 0.5, 0.25, and 0) were grown in situ on a model 2D/2D S-scheme heterojunction composed of Cu₂O nanosheets and Fe₂O₃ nanoplates to form a series of Cu₂O/Fe₂O₃@Ni_xCo_1-_x(OH)₂ (CF@NiCo) photocatalysts. The combined experimental and theoretical investigation demonstrates that incorporating an appropriate amount of Co into Ni(OH)₂ not only modulates the energy band structure of Ni_xCo_1-_x(OH)₂, balances the electron- and hole-trapping abilities of the bifunctional cocatalyst and maximizes the charge separation efficiency of the heterojunction, but also regulates the d-band center of Ni_xCo_1-_x(OH)₂, reinforcing the adsorption and activation of CO₂ and H₂O on the cocatalyst surface and lowering the rate-limiting barriers in the CO₂-to-CO and H₂O-to-O₂ conversion. Benefiting from the Ni-Co synergy, the redox reactions proceed stoichiometrically. The optimized CF@Ni_0.75Co_0.25 achieves CO and O₂ yields of 552.7 and 313.0 μmol g_cat^-1 h^-1, respectively, 11.3/9.9, 1.6/1.7, and 4.5/5.9-fold higher than those of CF, CF@Ni, and CF@Co. This study offers valuable insights into the design of bifunctional noble-metal-free cocatalysts for high-performance artificial photosynthesis.

Key words: Ni-Co synergy, Bifunctional cocatalyst, CO₂ reduction, H₂O oxidation, 2D/2D heterojunction, S-scheme photosynthetic system

Lingxuan Hu, Yan Zhang, Qian Lin, Fengying Cao, Weihao Mo, Shuxian Zhong, Hongjun Lin, Liyan Xie, Leihong Zhao, Song Bai. Unraveling the Ni-Co synergy in bifunctional hydroxide cocatalysts for better cooperation of CO₂ reduction and H₂O oxidation in 2D S-scheme photosynthetic systems[J]. Chinese Journal of Catalysis, 2025, 68: 311-325.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(24)60174-9

https://www.cjcatal.com/EN/Y2025/V68/I1/311

Figures/Tables 7

Fig. 1. Synthesis and electron-microscopic characterization of CF@NiCo. (a) Schematic illustrating the synthesis of CF@NiCo; TEM (b,c). HRTEM (d), STEM and EDS-mapping (e) images of CF@Ni0.75Co0.25.

Fig. 2. Spectroscopic characterizations of CF@NiCo and reference samples. (a) XRD patterns; (b) UV-vis diffuse reflectance spectra; (c) survey XPS spectra; high-resolution XPS spectra of Cu 2p (d), Fe 2p (e), Ni 2p (f), and Co 2p (g).

Fig. 3. Photocatalytic performance of CF@NiCo. (a) H2, CO, and CH4 evolution rates and CO selectivities of CF and CF@NiCo; (b) comparison of the CO yield and selectivity of CF@Ni0.75Co0.25 with reported Cu2O and Fe2O3 based heterojunctions; (c) mass spectra of the generated 13CO (top) and 13CH4 (bottom) using 13CO2 as the gas source; (d) O2 evolution rates and hole/electron utilization ratios of CF and CF@NiCo; (e) mass spectrum of the generated 18O2 using H218O as the source; (f) recycling tests of CF@Ni0.75Co0.25.

Fig. 4. Charge kinetics analysis of CF@NiCo. Steady-state PL spectra (a), photocurrent densities (b), and average electron lifetimes (c) of CF and CF@NiCo; UPS spectra (d), Tauc plots (e), and energy band structures (f) of Cu2O, Fe2O3, and NixCo1-x(OH)2; (g) schematic illustrating the charge-transfer mechanisms in CF@NiCo samples. In Fig. 4(d)-(g), Ni0.75Co0.25(OH)2, Ni0.5Co0.5(OH)2, and Ni0.25Co0.75(OH)2 are abbreviated as Ni0.75Co0.25, Ni0.5Co0.5, and Ni0.25Co0.75, respectively.

Fig. 5. Charge separation and transfer mechanisms in CF@NiCo. AFM images (left) and KPFM potential images (right) of CF@Ni0.75Co0.25 in the dark (top) and under light irradiation (bottom) (a), and the corresponding line-scanning surface potential curves in the dark and under light irradiation (b); EPR spectra of DMPO-?OH (c) and DMPO-?O2- (d) over Cu2O, Fe2O3, CF and CF@Ni0.75Co0.25 under light irradiation; (e) schematic illustrating the charge separation and transfer mechanism in CF@Ni0.75Co0.25.

Fig. 6. Surface reaction dynamics analysis of CF@Ni, CF@Ni0.75Co0.25, and CF@Co. CO2 (a) and water vapor (d) adsorption isotherms; CO2-TPD (b) and H2O-TPD (e) profiles; LSV curves for CO2 reduction (c) and H2O oxidation (f); (g) in-situ DRIFTS of CF@Ni0.75Co0.25 during CO2 reduction coupled with H2O oxidation.

Fig. 7. DFT calculations on Ni-Co synergistic mechanisms. Charge density difference of Cu2O-NixCo1-x(OH)2 (a) and Fe2O3-NixCo1-x(OH)2 (b) heterointerfaces: Ni(OH)2 (left), Ni0.75Co0.25(OH)2 (middle), and Co(OH)2 (right) (yellow and blue colors represent the electron-accumulation zone and electron-depletion zone, respectively); (c) computed PDOS of Ni(OH)2, Ni0.75Co0.25(OH)2, and Co(OH)2; free energy diagrams and optimized configurations of key intermediates formation for CO2-to-CO reduction (d,e) and H2O-to-O2 oxidation (f,g) over Ni(OH)2, Ni0.75Co0.25(OH)2, and Co(OH) surface (Ni0.75Co0.25(OH)2 is abbreviated as Ni0.75Co0.25 in Figs.7(c), (d) and (f)).

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Unraveling the Ni-Co synergy in bifunctional hydroxide cocatalysts for better cooperation of CO₂ reduction and H₂O oxidation in 2D S-scheme photosynthetic systems

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