Band-gap engineered intermolecular S-scheme heterojunctions: π-conjugated acetylenic polymers/g-C3N4 with ultrafast charge transfer for solar-driven H2O2 synthesis

doi:10.1016/S1872-2067(25)64847-9

Abstract

Abstract:

All-organic intermolecular S-scheme heterojunction photocatalysts are promising for efficient and fast carrier separation, yet attaining strong reducing capacity and tracking directional charge transfer remain critical challenges. Herein, we unveiled an intermolecular S-scheme heterojunction through in-situ growth of conjugated poly(1,4-diethynylbenzene) (pDEB, reduction photocatalyst) on graphitic carbon nitride (g-C₃N₄, oxidation photocatalyst), forming the nanofiber-decorated nanosheet-like pDEB/CN architecture via π-conjugated polymer templating. By leveraging the electron-donating effect and the expanded π-electron delocalization range of electron-rich conjugated acetylenic polymers, pDEB with high energy band positions was introduced into the intermolecular S-scheme heterojunction with enhanced reducibility. The directional S-scheme charge migration is mechanistically demonstrated by deploying dual metal oxide cocatalysts as spatially resolved electron donor-acceptor probes, with light-modulated in-situ X-ray photoelectron spectroscopy capturing real-time interfacial charge migration. Femtosecond transient absorption spectroscopy further elucidates accelerated ultrafast electron transfer kinetics mediated by the S-scheme interfacial electric field. The S-scheme heterojunction attained an apparent quantum efficiency of 5.18% at 420 nm during the photocatalytic H₂O₂ production. Notably, pDEB/CN has demonstrated an excellent H₂O₂ yield for the first time in a continuous flow photocatalytic system, reaching 394.27 μmol g^-1 h^-1 within 24 h, which illustrates the stable interfacial charge transfer brought about by the rigid structure. The work demonstrated the transformative potential of architecting directional charge superhighways through band level engineering, while advancing S-scheme heterojunctions design with molecular precision.

Key words: Conjugated polymers, Photocatalysis, Band engineering, S-scheme heterojunctions, Ultrafast charge transfer

Junru Xu, Lei Cheng, Tongming Su, Yawen Tang, Hanjun Sun. Band-gap engineered intermolecular S-scheme heterojunctions: π-conjugated acetylenic polymers/g-C₃N₄ with ultrafast charge transfer for solar-driven H₂O₂ synthesis[J]. Chinese Journal of Catalysis, 2025, 79: 205-218.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(25)64847-9

https://www.cjcatal.com/EN/Y2025/V79/I12/205

Figures/Tables 5

Fig. 1. The morphology and structure characterization of the materials. (a) Structure diagram of pDEB/CN. (b) Solid state 13C CP-MAS NMR spectra of pDEB/CN-4, and pDEB. (c) FT-IR spectra of pDEB, CN, and pDEB/CN-x (x = 3, 4, 5). XPS of N 1s of pDEB, pDEB/CN-4, and CN (d) and C 1s of pDEB/CN-4, and CN (e). (f) Raman spectra of pDEB, pDEB/CN-4 and CN. (g) TEM image of pDEB/CN-4. (h,i) Simulated STM image of pDEB and CN, the inset displays the structural units of pDEB and CN.

Fig. 2. Precise control of electronic band structures by structural design. (a) Scheme of the synthesis and chemical structures of pDEB/CN, pDEP/CN, and pDED/CN. (b) UV-vis diffuse reflection spectroscopy and the inset corresponding color of the CN and CAPs. (c) Schematic illustration of the electronic band structures of the CN and CAPs. (d) In-situ XPS of Pt 4f spectra of pDEB/CN-4@PtMn. (e) In-situ XPS of Mn 2p spectra of pDEB/CN-4@PtMn. (f) Mechanism diagram of photogenerated electron transfer at the interface of pDEB/CN-4@PtMn after bimetallic probe loading.

Fig. 3. Measurement of the decay lifetime of dynamic charge separation in CN and pDEB/CN-4. fs-TAS of CN (a,b) and pDEB/CN-4 (d,e). (c) Kinetic traces of CN probed at 590 and 713 nm, respectively. (f) Kinetic traces of pDEB/CN-4 probed at 560, 600, and 718 nm. (g) Schematic diagram of pDEB/CN-4 decay life based on fs-TAS measurements. (h) Schematic explanation of the band bending and charge transfer mechanism in S-scheme heterojunction.

Fig. 4. Photocatalytic H2O2 production. (a) Photocatalytic activity of pDEB/CN-x (x = 3, 4, 5), CN and pDEB for H2O2 production in pure water. Conditions: λ ≥ 420 nm, 60 mW cm-2, pure water (30 mL), catalyst (15 mg). (b) Stability tests of H2O2 production over pDEB/CN-4. (c) AQY of the pDEB/CN-4. (d) Photocatalytic H2O2 yield by pDEB/CN-4 in different water. (e) Photocatalytic H2O2 yield by different catalysts. (f) Time course of H2O2 production measured in pure water under visible light irradiation by CN, pDEB/CN-4, pDEP/CN-4, and pDED/CN-4. (g) In-situ DRIFTS spectra for H2O2 production over pDEB/CN-4, the local parts of spectra are enlarged on the right side.

Fig. 5. Continuous long-time H2O2 photocatalytic production and reaction mechanisms. (a) Photograph of the homemade continuous flow photocatalytic system in operation. (b) Long-term scaled-up photocatalytic production of H2O2. (c) Schematic diagram of continuous flow photocatalytic reaction system. (d) Photocatalytic mechanism for H2O2 production by pDEB/CN-4.

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Band-gap engineered intermolecular S-scheme heterojunctions: π-conjugated acetylenic polymers/g-C₃N₄ with ultrafast charge transfer for solar-driven H₂O₂ synthesis

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