Exploring the spatially resolved charge transfer mechanism in the Al-doped SrTiO3/C3N5 S-scheme heterojunction for boosted solar-driven photocatalytic hydrogen evolution

doi:10.1016/S1872-2067(26)65226-6

Abstract

Abstract:

Developing highly efficient and low-cost C₃N₅-based photocatalysts for hydrogen production is of great significance. However, research on the surface potential distribution of photogenerated charges in the C₃N₅-based S-scheme heterojunction from a spatial perspective with nanoscale precision is still lacking. In this work, using Al-doped SrTiO₃ (ASTO) with strong oxidation ability and C₃N₅ nanosheets with high reduction ability, a novel S-scheme heterojunction was created. The ASTO/C₃N₅ S-scheme heterojunction was synthesized via a hydrothermal method. It reveals that the polyhedral ASTO particles are in intimate contact with C₃N₅ nanosheets, with a clear and distinct interface observed between them. The optimal 5%-ASTO/C₃N₅ S-scheme heterojunction exhibits a high hydrogen production rate under simulated solar light, surpassing pristine C₃N₅ and ASTO by factors of 2.5 and 37.4, respectively. Light-assisted Kelvin-probe force microscopy was employed to uncover the spatially resolved features of the kinetics of charge transfer in the ASTO/C₃N₅ S-scheme heterojunction. It reveals that photogenerated electrons gather on the surface of C₃N₅ as a reduction photocatalyst in the heterojunction, resulting in a reduced surface photovoltage (SPV) compared to pure C₃N₅, whereas holes accumulate on the surface of ASTO as an oxidation photocatalyst in the heterojunction, providing higher SPV than pure ASTO. Moreover, the large work function difference (0.41 eV) between ASTO and C₃N₅ induces a robust interfacial electric field (IEF). This strong IEF facilitates the photogenerated electrons in ASTO’s conduction band recombine with holes in C₃N₅’s valence band, preserving high redox potentials. Furthermore, active free radical measurement confirms the enhanced •O₂^- and •OH signals for the 5%-ASTO/C₃N₅ heterojunction, confirming the S-scheme mechanism and excluding the type-II mechanism, which is also demonstrated by in-situ X-ray photoelectron spectroscopy. Overall, this work offers some evidence regarding the spatially resolved characteristics of the kinetics of charge transfer in the S-scheme heterojunction.

Key words: Photocatalytic hydrogen production, S-scheme heterojunction, C₃N₅, Al-doped SrTiO₃, Charge transfer mechanism

Xiaoxuan Chen, Kang Li, Zewen Jiang, Haotian Guo, Xuanwen Xu, Pengyu Dong. Exploring the spatially resolved charge transfer mechanism in the Al-doped SrTiO₃/C₃N₅ S-scheme heterojunction for boosted solar-driven photocatalytic hydrogen evolution[J]. Chinese Journal of Catalysis, 2026, 91: 274-289.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(26)65226-6

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Figures/Tables 10

Fig. 1. (a) The proposed procedure for the preparation of ASTO/C3N5 heterojunction. (b) XRD patterns of all as-prepared samples. Raman spectra (c) and N2 adsorption isotherms (d) tested at 77 K of C3N5, ASTO, and 5%-ASTO/C3N5.

Fig. 2. High-resolution XPS spectra comparing C3N5 and the 5%-ASTO/C3N5 heterojunction: C 1s (a) and N 1s (b) regions. High-resolution XPS spectra comparing ASTO and the 5%-ASTO/C3N5 heterojunction: O 1s (c), Al 2p (d), Sr 3d (e), and Ti 2p (f).

Fig. 3. TEM images of C3N5 (a,b), ASTO (c), and 5%-ASTO/C3N5 (d,e). (f) HRTEM image of 5%-ASTO/C3N5. (g) HAADF-STEM and EDS elemental-mapping images of 5%-ASTO/C3N5.

Fig. 4. (a) Graph showing the time-dependent photocatalytic hydrogen production activity over all the as-prepared catalysts. (b) Histogram of hydrogen production rates of pure C3N5, ASTO, and various ASTO/C3N5 heterojunctions. (c) Photocatalytic stability performance of 5%-ASTO/C3N5. (d) AQE and the corresponding UV-vis DRS spectrum of 5%-ASTO/C3N5. (e) Bar chart of hydrogen production rates with different sacrificial reagents. (f) A comparison of photocatalytic H2 evolution over some reported C3N5-based heterojunction photocatalysts. (g) Water contact angles of C3N5, ASTO, and 5%-ASTO/C3N5.

Fig. 5. (a) Each prepared sample's UV-vis DRS spectra. Tauc plots of ASTO (b) and C3N5 (c). Mott-Schottky plots of ASTO (d) and C3N5 (e). (f) Energy band position diagram of C3N5 and ASTO.

Fig. 6. EIS Nyquist plots (illustration showing the equivalent circuit) (a), photocurrent curves (b), LSV curves (c), steady-state PL spectra (at 370 nm of excitation) (d), and TRPL decay profiles (e)

Fig. 7. AFM (a) and KPFM images of pure C3N5 in the dark (b), in the presence of light (c), and the associated potential distribution curves (d). AFM (e) and KPFM images of pure ASTO in the absence of light (f) and in the presence of light (g), together with the matching potential distribution curves (h). AFM (i) and KPFM images of the 5%-ASTO/C3N5 heterojunction in the absence of light (j), in the presence of light (k), and the associated potential distribution curves (l). (m) A comparison of SPV between pure C3N5 (or ASTO) and C3N5-HJ (or ASTO-HJ). (n) Schematic diagram of charge transfer in the ASTO/C3N5 heterojunction under illumination. (o) Proposed ASTO/C3N5 S-scheme heterojunction with the surface state.

Fig. 8. Plane-averaged electrostatic potential of C3N5 (001) (a) and ASTO (110) (b) surfaces. (c) The fabricated ASTO (110)/C3N5 (001) interface model after geometry optimization. (d) The ASTO (110)/C3N5 (001) interface's computed charge density difference distribution, which has an isosurface value of 0.0008 e Å-3. (Yellow: electron buildup; Cyan: electron depletion).

Fig. 9. DMPO spin-trapping EPR spectra for detecting •O2- (a) and •OH (b) signals over the as-prepared ASTO, C3N5, and 5%-ASTO/C3N5 samples. Schematic representation of type-II (c) and S-scheme (d) mechanisms as two possible pathways for ASTO/C3N5 charge tra

Fig. 10. In-situ XPS spectra for C 1s (a), N 1s (b), O 1s (c), Sr 3d (d), and Ti 2p (e) in the 5%-ASTO/C3N5 sample under dark and Xe lamp irradiation. (f) Schematic diagram of binding energy shift and electron density change. (g) Schematic representation of the charge migration pathways of the S-scheme ASTO/C3N5 heterostructure before and after exposure to dark and under simulated sunlight irradiation.

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Exploring the spatially resolved charge transfer mechanism in the Al-doped SrTiO₃/C₃N₅ S-scheme heterojunction for boosted solar-driven photocatalytic hydrogen evolution

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