S-scheme heterojunctions of metal-doped ZnIn2S4/TpPa-1: Regulating H adsorption/desorption and internal electric field for boosted dual-functional photocatalysis

doi:10.1016/S1872-2067(25)64879-0

Abstract

Abstract:

Cooperative coupling of photocatalytic hydrogen generation with oxidative organic synthesis is promising in simultaneously producing sustainable energy and value-added chemicals. However, the photocatalytic activity is constrained by restricted redox potentials and insufficient photocarrier separation and transfer. Herein, we construct S-scheme heterojunctions based on metal-doped ZnIn₂S₄ and covalent organic frameworks, denoted as M-ZIS/TpPa-1 (M = Ni or Mo). Theoretical calculations demonstrated that Mo-ZIS possess optimum H adsorption Gibbs free energies, deeper downshift of sulfur p-band center and higher integrated crystal orbital Hamilton population (ICOHP) value than Ni-ZIS and ZIS to optimize H adsorption/desorption dynamics. Besides, metal-doping reasonably enhanced the interfacial charge transfer in heterostructures, identifying the enlarged internal electric field (IEF) in Mo-ZIS/TpPa-1 than Ni-ZIS/TpPa-1 and ZIS/TpPa-1. Moreover, experimental explorations of photoelectrochemical measurements, femtosecond transient absorption spectroscopy, in-situ irradiated X-ray photoelectron spectroscopy and electron paramagnetic resonance verified the facilitated photocarrier separation and migration in metal-doped S-scheme heterojunctions. Ultimately, Mo_0.01-ZIS/TpPa-1 exhibited visible-light driven H₂ evolution rate of 1648 μmol g⁻¹ h⁻¹ and N-benzylidenebenzylamine formation rate of 1812 μmol g⁻¹ h⁻¹, better than Ni_0.048-ZIS/TpPa-1, and superior to parent ZIS/TpPa-1. This work might provide insights into the modulation of H adsorption/desorption behavior and IEF within S-scheme heterostructures via rational metal-doping strategy for efficient dual-functional photocatalysis.

Key words: Covalent organic frameworks, Metal-doped ZnIn₂S₄, S-scheme heterojunction, H adsorption/desorption, Internal electric field, Dual-functional photocatalysis

Shaodan Wang, Heng Yang, Lijun Xue, Jianjun Zhang, Shuxin Ouyang, Lili Wen. S-scheme heterojunctions of metal-doped ZnIn₂S₄/TpPa-1: Regulating H adsorption/desorption and internal electric field for boosted dual-functional photocatalysis[J]. Chinese Journal of Catalysis, 2026, 80: 159-173.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(25)64879-0

https://www.cjcatal.com/EN/Y2026/V80/I1/159

Figures/Tables 9

Scheme 1. Schematic representation for the synthesis of M-ZIS/TpPa-1 (M = Ni or Mo).

Fig. 1. (a) The calculated Gibbs free energy for H adsorption (ΔGH*) for ZIS, Ni-ZIS and Mo-ZIS. (b) The p-band centers for S 3p of ZIS, Ni-ZIS and Mo-ZIS. (c) COHP calculations of ZIS, Ni-ZIS and Mo-ZIS. (d) Schematic diagram illustrates of the bond formation between the active sulfur sites and Hads.

Fig. 2. SEM images (a,f), TEM images (b,c,g,h), HRTEM images (d,i), and HADDF-STEM, EDS mapping images (e,j) of Mo0.01-ZIS/TpPa-1 and Ni0.048-ZIS/TpPa-1 composites, respectively.

Fig. 3. (a) The XPS survey spectra of TpPa-1, ZIS, Mo0.01-ZIS, Mo0.01-ZIS/TpPa-1, Ni0.048-ZIS and Ni0.048-ZIS/TpPa-1. The high-resolution XPS spectra of C 1s (b), N 1s (c), S 2p (d), In 3d (e) and Zn 2p (f).

Fig. 4. (a) The UV-vis diffuse reflectance spectroscopy, (b) corresponding Tauc-plots and (c) calculated band structures of the photocatalysts.

Fig. 5. The steady-state PL spectra (λex = 380 nm) (a), time-resolved PL spectra (b), Nyquist plots of EIS (c) and transient photocurrent response (d) of synthetized samples.

Fig. 6. 2D pseudocolor TA spectra of ZIS/TpPa-1 (a), Ni0.048-ZIS/TpPa-1 (d) and Mo0.01-ZIS/TpPa-1 (g) using a 340 nm pump pulse. TA spectra of ZIS/TpPa-1 (b), Ni0.048-ZIS/TpPa-1 (e) and Mo0.01-ZIS/TpPa-1 (h) at indicated time delays. GSB recovery kinetics of ZIS/TpPa-1 (c) probed at 390 nm, Ni0.048-ZIS/TpPa-1 probed at 400 nm (f) and Mo0.01-ZIS/TpPa-1 (i) probed at 410 nm within 100 ps.

Fig. 7. Schematic illustration of the S-scheme charge transfer mechanism in ZIS/TpPa-1 (a), Ni0.048-ZIS/TpPa-1 (b), and Mo0.01-ZIS/TpPa-1 (c) for photocatalytic H2 evolution and benzylamine oxidation. The calculated 3D charge density difference of ZIS/TpPa-1 (d), Ni-ZIS/TpPa-1 (e), and Mo-ZIS/TpPa-1 (f). The yellow and cyan areas indicate electron accumulation and depletion, respectively.

Fig. 8. The time-dependent H2 production (a) and N-benzylidenebenzylamine production (b) curves. (c) The photocatalytic performance of different samples. (d) The AQE values of Mo0.01-ZIS/TpPa-1 and Ni0.048-ZIS/TpPa-1. (e) The comparison of photocatalytic activities for H2 production coupled with benzylamine oxidation with different catalysts. (f) The effect of various active species on the photocatalytic performance of Mo0.01-ZIS/TpPa-1. (g) EPR spectra of DMPO-PhCH2NH2?+ from the photocatalytic system with benzylamine. (h) Schematic diagram of the dual-functional photocatalytic mechanism for simultaneous H2 production and benzylamine oxidation on M-ZIS/TpPa-1.

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S-scheme heterojunctions of metal-doped ZnIn₂S₄/TpPa-1: Regulating H adsorption/desorption and internal electric field for boosted dual-functional photocatalysis

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