Surface defect engineering of ZnCoS in ZnCdS with twin crystal structure for visible-light-driven H2 production coupled with benzyl alcohol oxidation

doi:10.1016/S1872-2067(24)60197-X

Abstract

Abstract:

Photoredox dual reaction of organic synthesis and H₂ evolution opens up a novel pathway for collaboratively generating clean fuels and high-quality chemicals, providing a more effective approach of solar energy conversion. Herein, a surface defect-engineered ZnCoS/ZnCdS heterostructure with zinc blende (ZB)/wurtzite (WZ) phase junctions is synthesized for photocatalytic cooperative coupling of benzaldehyde (BAD) and H₂ production. This surface defect-engineered ZnCoS/ZnCdS heterostructure elaborately integrates the mixed phase junction advantage of ZnCdS semiconductor and the cocatalytic function of ZnCoS possessing Zn (V_Zn-ZnCoS/ZnCdS) or S vacancies (V_S-ZnCoS/ZnCdS). The optimum V_S-ZnCoS/ZnCdS simultaneously exhibits a superior H₂ production rate of 14.23 mmol h^-1 g^-1 accompanied with BAD formation rate of 12.29 mmol h^-1 g^-1 under visible-light irradiation, which is approximately two-fold greater than that of pristine ZnCdS. Under simulated sunlight irradiation (AM 1.5), V_S-ZnCoS/ZnCdS achieves H₂ evolution (27.43 mmol g_cat^-1 h^-1) with 0.52% of STH efficiency, accompany with 26.31 mmol g_cat^-1 h^-1 of BAD formation rate. The underlying solar-driven mechanism is elucidated by a series of in-situ characterization and control experiments, which reveals the synergistic effect of interfacial ZB/WZ phase junctions in ZnCdS and S vacancies of ZnCoS on enhancement of the photoredox dual reaction. The V_S-ZnCoS/ZnCdS follows a predominant oxygen-centered radical integrating with carbon-centered radical pathways for BAD formation and a simultaneous electron-driven proton reduction for H₂ production. Interestingly, the nature of surface vacancies not only facilitates the separation of photoinduced charge carriers but also able to selectively adjust the mechanism pathway for BAD production via tuning the oxygen-centered radical and carbon-centered radical formation.

Key words: Photoredox dual reaction, Aromatic alcohol conversion, Surface vacancy, Organic synthesis, H₂ production

Tan Ji Siang, Peipei Zhang, Binghui Chen, Wee-Jun Ong. Surface defect engineering of ZnCoS in ZnCdS with twin crystal structure for visible-light-driven H₂ production coupled with benzyl alcohol oxidation[J]. Chinese Journal of Catalysis, 2025, 69: 84-98.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(24)60197-X

https://www.cjcatal.com/EN/Y2025/V69/I2/84

Figures/Tables 12

Fig. 1. (A) XRD patterns of pristine ZnCdS, ZnCoS, VZn-ZnCoS, VS-ZnCoS, ZnCoS/ZnCdS, VZn-ZnCoS/ZnCdS and VS-ZnCoS/ZnCdS specimens. (B) EPR spectra of pristine ZnCdS and ZnCdS-based photocatalysts.

Fig. 2. HRTEM images of pristine ZnCdS (A) and representative ZnCoS/ZnCdS photocatalyst (B) with Insert of interfacial between ZnCdS and ZnCoS phases (C).

Fig. 3. High-resolution XPS spectra corresponding to Zn 2p (A), Cd 3d (B) and S 2p (C) regions of ZnCdS-based photocatalysts.

Fig. 4. (A) UV-vis absorption spectra of pristine ZnCdS, ZnCoS, VZn-ZnCoS, VS-ZnCoS, ZnCoS/ZnCdS, VZn-ZnCoS/ZnCdS and VS-ZnCoS/ZnCdS specimens. (B) Tauc plot of pristine ZnCdS photocatalyst.

Fig. 5. Mott-Schottky plot of pristine ZB-ZnCdS (A) and pure WZ-ZnCdS (B) photocatalysts. (C) Schematic diagram of estimated band structure of ZnCdS photocatalyst with ZB/WZ phase junctions.

Fig. 6. Photoredox dual reaction of benzyl alcohol oxidation and H2 evolution: (A) H2 evolution performance with 4 h-on-stream reaction run and (B) Production rates of H2 and benzaldehyde over pristine ZnCdS and ZnCdS-based photocatalysts under > 420 nm irradiation after 4 h-on-stream reaction run. (C) H2 evolution performance over VS-ZnCoS/ZnCdS photocatalysts under AM 1.5 simulated sunlight irradiation. (D) Wavelength-dependent AQE of VS-ZnCoS/ZnCdS photocatalyst. All reactions were conducted in a close-looped circulation system.

Fig. 7. LSV curves (A), EIS Nyquist plots (B) and transient photocurrent response (C) of ZnCdS-based photocatalysts. (D) Steady-state PL spectra of Pristine ZnCdS (a), ZnCoS/ZnCdS (b), VZn-ZnCoS/ZnCdS (c) and VS-ZnCoS/ZnCdS (d) photocatalysts.（图D中未标出b和c）

Table 1 Comparison of recently reported photocatalysts for photoredox dual reaction of BA oxidation and H2 evolution.

Photocatalyst	Light source wavelength (nm)	Reaction duration (h)	H₂ evolution rate (μmol g⁻¹ h⁻¹)	BAD formation rate (μmol g⁻¹ h⁻¹)	Ref.
V_S-ZnCoS/ZnCdS	> 420	4	14273	12296	this study
V_Zn-ZnCoS/ZnCdS	> 420	4	10539	12776	this study
Ru/g-C₃N₄	simulated sunlight	12	5610	4010	[57]
ZnIn₂S₄	> 420	5	206	—	[58]
VC/CdS	> 420	9	9000	10300	[29]
ZnIn₂S₄/Ni_x-B	> 400	2	8920	8192	[59]
ZnIn₂S₄/NiS	> 400	2	2879	2714	[59]
ZnIn₂S₄/Ni(OH)₂	> 400	2	3372	2832	[59]
ZnIn₂S₄/Pt	> 400	2	1282	1304	[59]
UiO-66-NH₂@CdS	> 350	3	636.7	628.3	[60]
K₃PW₁₂O₄₀/CdS	> 420	3	18500	17300	[61]
P-MoS₂-ZnIn₂S₄	> 420	5	3367	3223	[62]
Co-ZnIn₂S₄	> 420	8	2824	2769	[63]
0.5%Pt/TiO₂	> 420	2	1840	1639	[64]
1%Ru/TiO₂	simulated sunlight	3	2833	1289	[65]

Fig. 8. Schematic illustration of the synergistic effect between ZnCdS with ZB/WZ phase junctions and VS-ZnCoS (or VZn-ZnCoS) on photogenerated carrier transfer.

Fig. 9. Scavenger tests for photoredox dual reaction of benzyl alcohol oxidation and H2 evolution over VZn-ZnCoS/ZnCdS (A) and VS-ZnCoS/ZnCdS (B) photocatalysts.

Fig. 10. In situ EPR profiles of ZnCdS-based photocatalysts under visible light irradiation for DMPO-Cα radical capture in 2 mL of BA solution (A) and DMPO-?OH radical capture in deionized water (B).

Fig. 11. Proposed mechanistic steps of photoredox dual reaction of benzyl alcohol oxidation and H2 evolution over VS-ZnCoS/ZnCdS photocatalyst: Carbon-centered radical route (A) and Oxygen-centered radical route (B).

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Surface defect engineering of ZnCoS in ZnCdS with twin crystal structure for visible-light-driven H₂ production coupled with benzyl alcohol oxidation

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