Synergistic effect of S-doping and nitrogen-vacancy engineering on 2D/3D S-scheme photocatalyst for efficient photosynthesis of H2O2

doi:10.1016/S1872-2067(26)64957-1

Abstract

Abstract:

The green photocatalytic synthesis of hydrogen peroxide (H₂O₂) has attracted considerable attention as an environmentally friendly approach for H₂O₂ production. However, the rapid recombination of photogenerated charge carriers, reliance on sacrificial agents, and low activity and selectivity of photocatalytic H₂O₂ remain major challenges for the further development of this process. In this study, we synthesized an S-scheme composite photocatalyst composed of N-vacancy-tailored, sulfur-modified graphitic carbon nitride (Vr-CNS) and Zn₂In₂S₅ (ZIS) that enabled solar-driven H₂O₂ synthesis, achieving a rate of 475.6 μmol g^-1 h^-1 in pure water and air without sacrificial agents. This represents a five-fold enhancement over pristine graphitic carbon nitride (g-C₃N₄). S-doping mainly altered the electronic structure of g-C₃N₄, resulting in bandgap narrowing and a redshift of the absorption edge. N vacancies (N_V) not only promoted charge separation and reduced charge transfer resistance, but also accelerated surface reactions. Moreover, N_V lowered the energy barrier due to O₂ adsorption, which is the rate-determining step, thereby accelerating the reaction. The S-scheme Vr-CNS/ZIS heterojunction retained the strong reduction ability of Vr-CNS and robust oxidation capability of ZIS. The presence of N_V strengthened the electronic coupling between Vr-CNS and ZIS after heterojunction contact. The synergistic effect of defect engineering (sulfur doping coupled with nitrogen vacancies) and the S-scheme accelerated the reaction kinetics, promoting the migration and separation of the photogenerated carriers. This study provides an effective strategy for the design of multifunctional photocatalysts by exploiting the synergy between defect engineering and S-scheme heterojunctions.

Key words: Photocatalysis, H₂O₂, S-doped g-C₃N₄, Nitrogen vacancies, S-scheme heterojunctions

Chunyuan Chen, Zhongliao Wang, Ying Ma, Bo Weng, Shifu Chen, Sugang Meng. Synergistic effect of S-doping and nitrogen-vacancy engineering on 2D/3D S-scheme photocatalyst for efficient photosynthesis of H₂O₂[J]. Chinese Journal of Catalysis, 2026, 82: 278-291.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(26)64957-1

https://www.cjcatal.com/EN/Y2026/V82/I3/278

Figures/Tables 7

Fig. 1. SEM images of Vr-CNS (a), ZIS (b), and Vr-CNS/ZIS (c). TEM image (d), magnified TEM image (e), and EDX spectrum (f) of Vr-CNS/ZIS. HRTEM images (g,j-l), corresponding FFT images (h,i), and element mapping (m-r) of Vr-CNS/ZIS.

Fig. 2. XRD patterns (a,b), FTIR spectra (c), and EPR spectra (d) of the synthesized ZIS, Vr-CNS, Vp-CNS, Vp-CNS/ZIS, and Vr-CNS/ZIS samples. N 1s (e) and C 1s (f) high-resolution XPS spectra of Vr-CNS and Vp-CNS.

Fig. 3. High-resolution XPS spectra of C 1s (a), N 1s (b), In 3d (c), and S 2p (d) in Vr-CNS/ZIS. The workfunctions for ZIS (001) (e), monolayer Vr-CNS (001) (f), and Vp-CNS (001) (g). Side views of the induced charge density difference of Vp-CNS/ZIS (h) and Vr-CNS/ZIS (i) plotted using an isosurface of 7.9 × 10-4 e ?-3 (charge accumulation is shown in yellow, and charge depletion is shown in cyan).

Fig. 4. UV-vis DRS spectra (a) and band-gap energies (b) of the as-prepared samples. M-S plots of Vr-CNS (c), ZIS (d), and Vp-CNS (e). (f) Relationships between redox potentials of Vr-CNS, Vp-CNS and ZIS, radicals, and H2O2 production.

Fig. 5. (a) DMPO spin-trapping EPR spectra recorded for ?O2? under light irradiation for ZIS, Vr-CNS, Vp-CNS, Vp-CNS/ZIS, and Vr-CNS/ZIS samples. C 1s (b), N1s (c), S 2p (d), and In 3d (e) in-situ XPS spectra of Vr-CNS/ZIS composite in the dark and under visible light. Photocurrent responses (f), EIS spectra (g), PL spectra (h), and the average lifetime (τave) values (i) of ZIS, Vr-CNS, Vp-CNS, and Vp-CNS/ZIS, and Vr-CNS/ZIS composites.

Fig. 6. (a) Standard absorption curve of H2O2. (b) H2O2 production activities of ZIS, Vr-CNS, Vp-CNS, Vp-CNS/ZIS, and Vr-CNS/ZIS composites under visible light illumination. (c) H2O2 production activities of ZIS and Vr-CNS/ZIS composites with different contents of Vr-CNS. (d) Photocatalytic activity of Vr-CNS/ZIS under different wavelengths of light. (e) Cyclic stability test of ZIS, Vr-CNS, and Vr-CNS/ZIS for photocatalytic H2O2 production. Cathodic LSV curves (f) and corresponding Tafel slopes (g), anodic LSV curves (h), and corresponding Tafel slopes (i) of ZIS, CNS, and Vp-CNS/ZIS and Vr-CNS/ZIS composites.

Fig. 7. (a) Single-variable control experiments of species capture. EPR spectra of TEMPO-e? (b), TEMPO-h+ (c), and DMPO-?OH (d) for the as-prepared ZIS, Vr-CNS, Vp-CNS, Vp-CNS/ZIS, and Vr-CNS/ZIS composites upon visible light irradiation. (e) In-situ DRIFTS spectra of Vr-CNS/ZIS. (f) Free-energy diagrams for the reduction of O2 to H2O2 on Vr-CNS and Vp-CNS. (g) Mechanism of photocatalytic H2O2 production over Vr-CNS/ZIS.

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Synergistic effect of S-doping and nitrogen-vacancy engineering on 2D/3D S-scheme photocatalyst for efficient photosynthesis of H₂O₂

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