Self-assembling 3D/2D ZnIn2S4/CN-NH4 to construct S-scheme heterojunctions for the efficient production of H2O2 in pure water

doi:10.1016/S1872-2067(25)64851-0

Abstract

Abstract:

The photocatalytic double-electron oxygen reduction pathway has become a strategic approach for the production of hydrogen peroxide (H₂O₂). In many heterojunction systems, indium zinc sulfide (ZnIn₂S₄) has received increasing attention, but it is limited by its slow REDOX kinetics and the lack of sufficient double-electron oxygen reduction active sites. In this study, low-cost CN-NH₄ fragments were loaded onto flower-like indium zinc sulfide (ZnIn₂S₄) to construct a compact S-scheme, in order to achieve environmentally friendly hydrogen peroxide photosynthesis. The H₂O₂ yield of the ZnIn₂S₄/CN-NH₄ photocatalyst was 2031 µmol g^-1 h^-1, which was 2.84 and 21.39 times that of ZnIn₂S₄ and CN-NH₄, respectively. This is attributed to the contact between ZnIn₂S₄ and CN-NH₄, providing a fast migration channel for electrons, forming a strong internal electric field at the interface, and effectively prolonging the migration lifetime of photogenerated carriers. The introduction of CN-NH₄ enhances the absorption of oxygen by ZnIn₂S₄ and simultaneously reduces the energy barrier of its two-electron oxygen reduction reaction. This study provides a new approach for constructing S-scheme heterojunction materials that can efficiently generate H₂O₂ under solar irradiation.

Key words: Hydrogen peroxide, Oxygen reduction, Pure water, S-scheme heterojunction, Zinc indium sulfide

Congcong Wang, Yongkang Quan, Suili Shi, Guorong Wang, Zhiliang Jin. Self-assembling 3D/2D ZnIn₂S₄/CN-NH₄ to construct S-scheme heterojunctions for the efficient production of H₂O₂ in pure water[J]. Chinese Journal of Catalysis, 2026, 81: 259-271.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(25)64851-0

https://www.cjcatal.com/EN/Y2026/V81/I2/259

Figures/Tables 11

Scheme 1. Schematic illustration of the electrostatic self-assembly process for the preparation of the composite catalyst ZnIn2S4/CN-NH4.

Fig. 1. SEM images of flower-like ZnIn2S4 (a), sheet-like CN-NH4 (b), and ZnIn2S4/CN-NH4 (c). The TEM image (d), locally magnified TEM image (e), HRTEM image and corresponding SAED image (f) of ZnIn2S4/CN-NH4. EDS element mapping images of Zn (h), In (i), S (j), C (k), and N (l).

Fig. 2. XRD patterns of ZnIn2S4, CN-NH4, ZnIn2S4/CN-NH4-20 (a) and samples in various proportions (b). (c) The FT-IR spectra of ZnIn2S4, CN-NH4 and ZnIn2S4/CN-NH4-20. N2 adsorption-desorption isotherms and pore size distribution curves of ZnIn2S4 (d), CN-NH4 (e), and ZnIn2S4/CN-NH4-20 (f).

Table 1 BET surface area (ABET), pore diameter, and pore volume of ZnIn2S4, CN-NH4, and ZnIn2S4/CN-NH4-20.

Sample	A_BET(m² g^‒1)	Pore volume (cm³ g^‒1)	Average pore size (nm)
ZnIn₂S₄	107.13	0.24	4.58
CN-NH₄	37.41	0.20	18.31
ZnIn₂S₄/CN-NH₄-20	40.87	0.16	5.77

Fig. 3. (a) UV-vis DRS spectra of all samples. (b) Band gap diagram of ZnIn2S4 and CN-NH4. The M-S plots of ZnIn2S4 (c) and CN-NH4 (d) at different frequencies.

Fig. 4. In-situ XPS spectra of Zn 2p (a), In 3d (b), S 2p (c), C 1s (d), and N 1s (e). (f) Band structure diagram of ZnIn2S4 and CN-NH4.

Fig. 5. Transient photocurrent responses (a), LSV curves (b) and electrochemical active area plots (c) of ZnIn2S4, CN-NH4 and ZnIn2S4/CN-NH4. CV curves of ZnIn2S4 (d), CN-NH4 (e), and ZnIn2S4/CN-NH4 (f) at different scan rates.

Fig. 6. 2D pseudocolor TA plots of ZnIn2S4 (a), CN-NH4 (b), and ZnIn2S4/CN-NH4-20 (c). TA spectra of ZnIn2S4 (d), CN-NH4 (e), and ZnIn2S4/CN-NH4-20 (f) at indicated time delays. Normalized fs-TA decay curves of ZnIn2S4 at 710 nm (g), CN-NH4 at 388 nm (h), and ZnIn2S4/CN-NH4-20 at 710 nm (i).

Fig. 7. (a) The yield of H2O2 per 15 min of pure ZnIn2S4, CN-NH4 and samples in various proportions (mmol L?1). (b) Comparison of pure ZnIn2S4, CN-NH4 and the performance of the optimal proportion. (c) Comparison of H2O2 production performance for ZnIn2S4/CN-NH4-20 under N2 and O2 atmospheres. (d) XRD patterns of ZnIn2S4/CN-NH4-20 before and after the reaction. (e) Zeta potentials of ZnIn2S4, CN-NH4, and ZnIn2S4/CN-NH4-20. (f) ESR spectra detecting superoxide radicals (•O2?) for ZnIn2S4, CN-NH4, and ZnIn2S4/CN-NH4-20 under dark conditions and after 5 min of light irradiation. (g) A comparison chart of the H2O2 production rate of ZnIn2S4/CN-NH4-20 with some recent works.

Fig. 8. Theoretical calculation model, work function (a), density of states (b) and band gap (c) of ZnIn2S4. Theoretical calculation model, work function (d), density of states (e) and band gap (f) of CN-NH4. (g) Schematic diagram of H2O2 production by 2e? ORR in tight S-scheme ZnIn2S4/CN-NH4. (h) The Gibbs free energy distribution of the 2e? ORR process of ZnIn2S4 and ZnIn2S4/CN-NH4.

Fig. 9. Schematic illustration of the charge transfer of ZnIn2S4/CN-NH4.

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Self-assembling 3D/2D ZnIn₂S₄/CN-NH₄ to construct S-scheme heterojunctions for the efficient production of H₂O₂ in pure water

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