Collaborative photocatalytic C-C coupling with Cu and P dual sites to produce C2H4 over CuxP/g-C3N4 heterojunction

doi:10.1016/S1872-2067(24)60183-X

Abstract

Abstract:

Light-driven CO₂ reduction reaction (CO₂RR) to value-added ethylene (C₂H₄) holds significant promise for addressing energy and environmental challenges. While the high energy barriers for *CO intermediates hydrogenation and C−C coupling limit the C₂H₄ generation. Herein, Cu_xP/g-C₃N₄ heterojunction prepared by an in-situ phosphating technique, achieved collaborative photocatalytic CO₂ and H₂O, producing CO and C₂H₄ as the main products. Notably, the selectivity of C₂H₄ produced by Cu_xP/g-C₃N₄ attained to 64.25%, which was 9.85 times that of Cu_xP (6.52%). Detailed time-resolution photoluminescence spectra, femtosecond transient absorption spectroscopy tests and density functional theory (DFT) calculation validate the ultra-fast interfacial electron transfer mechanism in Cu_xP/g-C₃N₄ heterojunction. Successive *H on P sites caused by adsorbed H₂O splitting with moderate hydrogenation ability enables the multi-step hydrogenation during CO₂RR process over Cu_xP/g-C₃N₄. With the aid of mediated asymmetric Cu and P dual sites by g-C₃N₄ nanosheet, the produced *CHO shows an energetically favorable for C−C coupling. The coupling formed *CHOCHO further accepts photoexcited efficient e⁻ and *H to deeply produce C₂H₄ according to the C2+ intermediates, which has been detected by in-situ diffuse reflectance infrared Fourier transform spectroscopy and interpreted by DFT calculation. The novel insight mechanism offers an essential understanding for the development of Cu_xP-based heterojunctions for photocatalytic CO₂ to C2+ value-added fuels.

Key words: Photocatalytic CO₂ reduction, C-C coupling, Ethylene, Cu_xP/g-C₃N₄ heterojunction

Dongxiao Wen, Nan Wang, Jiahe Peng, Tetsuro Majima, Jizhou Jiang. Collaborative photocatalytic C-C coupling with Cu and P dual sites to produce C₂H₄ over Cu_xP/g-C₃N₄ heterojunction[J]. Chinese Journal of Catalysis, 2025, 69: 58-74.

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Figures/Tables 9

Fig. 1. DFT calculated work function (Φ) and corresponding electronic structure of g-C3N4 (a), Cu3P (b), and Cu3P/g-C3N4 (c). Charge density difference (d,e) and the mechanism of Φ tuning (f) of Cu3P/g-C3N4. The selected two Cu atom sites (Cu1, Cu2) on Cu3P and Cu3P/g-C3N4 (g). Calculated H2O and CO2 molecules adsorption energy on the different active sites of Cu3P (h) and Cu3P/g-C3N4 (i).

Fig. 2. Rotes of preparation for CuxP/g-C3N4 (a). XRD patterns (b), FTIR (c), Raman spectra (d), HR-XPS spectra of N 1s (e), Cu 2p (f), and P 2p (g) of different photocatalyst.

Fig. 3. SEM (a), TEM (b) and HR-TEM (c,d), HAADF (e-g) and corresponding EDX elemental mapping (h) images of CuxP/g-C3N4. Blue and pink circles in (d) refer to Cu3P with (e) d = 0.21 nm (300), (f) d = 0.19 nm (113), and CuP2 with (g) d = 0.29 nm (-112) respectively.

Fig. 4. Time profiles of the evolution of CO (a), C2H4 (b), and CH4 (c), and r values and product selectivity (d) of different photocatalyst. Different mass ratio of NaH2PO2·H2O:Cu-g-C3N4 (wt%) effect in CuxP/g-C3N4 during photocatalytic CO2RR (e). Time profiles of the productions during the photocatalytic CO2RR using CuxP/g-C3N4 for five consecutive runs (f).

Fig. 5. UV-vis DRS spectra (a) and (inset) Tauc-plots of (αhv)2 vs. energy of the exciting energy. UPS spectra (b), photocurrent responses (c), PL (d) and TR-PL (e) spectra with excitation at 340 nm of different photocatalyst, and the proposed electron transfer mechanism based on the band structures (f).

Fig. 6. The in-situ irradiated HR-XPS spectra of C 1s (a), N 1s (b), Cu 2p (c), and P 2p (d) of CuxP/g-C3N4

Fig. 7. 2D pseudo-color maps of fs-TA spectra (a,d,g), transient fs-TA spectra (b,e,h), kinetic time profiles (c,f,i) of normalized transient absorption at 462 nm, and the decay pathways (j) of photogenerated e- in g-C3N4, CuxP and CuxP/g-C3N4 under 340 nm laser pulse irradiation.

Fig. 8. CO2-TPD results (a), adsorption kinetic adsorption-desorption (b) of D2O at 2536 cm?1. The in-situ DRIFTS spectra of adsorbed CO2 and H2O under dark (c), and photocatalytic CO2RR under light irradiation (d) over CuxP/g-C3N4.

Fig. 9. DFT calculations. Free energy diagram of water splitting (a) over Cu3P and Cu3P/g-C3N4. CO2RR pathways to produce CO over Cu3P (b) and C2H4 over Cu3P/g-C3N4 (c). Proposed steps with optimized geometric structures in mechanism (d) for photocatalytic CO2 to C2H4 over CuxP/g-C3N4.

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Collaborative photocatalytic C-C coupling with Cu and P dual sites to produce C₂H₄ over Cu_xP/g-C₃N₄ heterojunction

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