Efficient urea synthesis via electrocatalytic CO2 reduction reaction coupled with nucleophilic addition reaction of NH3

doi:10.1016/S1872-2067(26)65213-8

Abstract

Abstract:

The electrocatalytic CO₂ reduction reaction coupled with nucleophilic addition reaction of NH₃ represents a promising route to synthesis urea. Relying on interfacial reactions between surface-adsorbed CO₂^•- from CO₂ reduction and dissolved NH₃. However, its efficiency is limited by competing CO formation and weak NH₃ adsorption, which restrict the C-N coupling efficiency. Thus, achieving synergistic co-adsorption of CO₂^•- and NH₃ while suppressing the CO pathway is essential. This study presents a dual-site catalyst with Pd clusters and Ni single atoms (Pd_1.0/Ni_SAs-N-C). In 0.5 mol·L^-1 NH₄HCO₃ solution at -1.3 V vs. RHE, Pd_1.0/Ni_SAs-N-C achieves a record urea production rate of 3.10 mmol·L^-1·g^-1·h^-1, substantially exceeding Ni_SAs-N-C (0.22 mmol·L^-1·g^-1·h^-1). Experimental and theoretical analyses reveal that electronic interaction between Ni and Pd sites induces charge redistribution, which enhances NH₃ adsorption on Pd via d-p orbital hybridization and optimizes CO₂^•- binding on Ni. This synergy suppresses CO formation and promotes CO₂^•- transfer to Pd sites, thereby increasing the “collision” probability between CO₂^•- and NH₃ and reducing the C-N coupling energy barrier from 0.40 to 0.24 eV, which accelerates the overall kinetics. The “site division-intermediate migration” mechanism offers a new paradigm for electrocatalytic coupling systems.

Key words: Urea, Dual-site catalyst, Competitive reactions, Ammonia adsorption, Intermediate migration

Shuchang Fan, Peize Li, Tianyu Sun, Yan Wei, Zhaoshi Yu, Jiandong Zhang, Mingkui Wang, Yan Shen. Efficient urea synthesis via electrocatalytic CO₂ reduction reaction coupled with nucleophilic addition reaction of NH₃[J]. Chinese Journal of Catalysis, 2026, 91: 135-146.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(26)65213-8

https://www.cjcatal.com/EN/Y2026/V91/I12/135

Figures/Tables 6

Fig. 1. (a) SEM image of Pd1.0/NiSAs-N-C. (b) HAADF-STEM image of Pd1.0/NiSAs-N-C at 50 nm. (c) HAADF-STEM image of Pd1.0/NiSAs-N-C at 5 nm. AC-STEM images of NiSAs-N-C (d) and Pd1.0/NiSAs-N-C (e) (Ni single atoms are marked by red circles, and Pd clusters were marked by yellow circles). (f) HAADF-STEM image and corresponding EDS mapping of Pd1.0/NiSAs-N-C.

Fig. 2. (a) XRD patterns of N-C, NiSAs-N-C, and Pd1.0/NiSAs-N-C. (b) C 1s XPS spectrum of Pd1.0/NiSAs-N-C. (c) N 1s XPS spectrum of Pd1.0/NiSAs-N-C. (d) Ni 2p XPS spectra of NiSAs-N-C and Pd1.0/NiSAs-N-C. (e) Pd 3d XPS spectra of Pd1.0/N-C and Pd1.0/NiSAs-N-C. (f) XRD patterns of Pd0.5/NiSAs-N-C, Pd1.0/NiSAs-N-C, and Pd1.5/NiSAs-N-C.

Fig. 3. Electrochemical tests. (a) LSV curves of the Pd1.0/NiSAs-N-C electrode in different solutions. (b) Urea production rate and FEurea of the Pd1.0/NiSAs-N-C electrode at each potential. (c) The FECO comparison of the Pd1.0/NiSAs-N-C, NiSAs-N-C, N-C electrodes in a CO2-saturated 0.5 mol·L-1 NH4HCO3 solution from -0.7 to -1.7 V (vs. RHE). (d) Urea production rates of Pdx/NiSAs-N-C electrodes (x=0.5, 1.0, 1.5) at -0.7 to -1.7 V (vs. RHE). (e) Stability test of the Pd1.0/NiSAs-N-C electrode at -1.3 V vs. RHE.

Fig. 4. UV-Vis in situ absorption spectra of the NiSAs-N-C electrode (a) and Pd1.0/NiSAs-N-C electrode (b) in a CO2-saturated 0.5 mol·L-1 KHCO3 solution at -0.7 to -1.7 V (vs. RHE). (c) JCO for NiSAs-N-C, Pd1.0/NiSAs-N-C electrodes in CO2 saturated 0.5 mol·L-1 NH4HCO3 solutions at -0.7 to -1.7 V (vs. RHE). (d) UV-vis in-situ absorption spectra of the NiSAs-N-C electrode and (e) Pd1.0/NiSAs-N-C electrode in an Ar-saturated 0.5 mol·L-1 NH4HCO3 solution at -0.7 to -1.7 V (vs. RHE). (f) NH3-TPD spectra of NiSAs-N-C and Pd1.0/NiSAs-N-C.

Fig. 5. In-situ FT-IR test of the Pd1.0/NiSAs-N-C electrode in a CO2-saturated 0.5 mol·L-1 NH4HCO3 solution within the potential range of -0.6 to -1.8 V (vs. RHE) was conducted, with tests in the wavenumber ranges of 2600-3600 cm-1 (a) and 1000-1800 cm-1 (b).

Fig. 6. DFT calculations of electronic property and reaction free energy. (a) PDOS of Ni in NiSAs-N-C and Pd1.0/NiSAs-N-C. (b) After introducing NH3 into Pd1.0/NiSAs-N-C, the PDOS of Pd (d) and N (p). (c) The adsorption energies of CO2•- and NH3 on NiSAs-N-C, as well as those of CO2•- on the Ni sites of Pd1.0/NiSAs-N-C and NH3 on the Pd sites of Pd1.0/NiSAs-N-C. (d) Free energy diagrams of ECRR/NARN on NiSAs-N-C and Pd1.0/NiSAs-N-C. (e) ECRR/NARN reaction mechanism diagram.

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Efficient urea synthesis via electrocatalytic CO₂ reduction reaction coupled with nucleophilic addition reaction of NH₃

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