Simultaneous benzyl alcohol oxidation and H2 generation over MOF/CdS S-scheme photocatalysts and mechanism study

doi:10.1016/S1872-2067(23)64466-3

Abstract

Abstract:

The conversion from solar energy into storable chemical energy can be achieved through synergistic coupling of photocatalytic H₂ production and organic synthesis, during which photogenerated electrons and holes can be simultaneously utilized. Herein, we combined a zirconium-based metal-organic framework, UiO-66-NH₂, and CdS nanoparticles (NPs) to form a core-shell structure by a chemical bath method. The step-scheme (S-scheme) heterojunction exhibits both substantially enhanced selective oxidation of benzyl alcohol and efficient H₂ generation under light irradiation simultaneously. The electron transfer paths at the S-scheme heterostructure interface were investigated in depth by in situ irradiated X-ray photoelectron spectroscopy. The dynamics of carrier migration at the heterojunction were obtained through femtosecond transient absorption (fs-TA) spectroscopy. Furthermore, the evolution mechanism of benzaldehyde was revealed by in situ diffuse reflectance infrared Fourier transform spectroscopy and electron paramagnetic resonance. This work illustrates the electron transfer mechanism of S-scheme heterojunction by fs-TA spectroscopy and provides new insights into the design of MOF/inorganic composite photocatalysts.

Key words: Step-scheme heterojunction, Photocatalytic hydrogen production, Selective organic oxidation, Ultrafast spectroscopy

Bowen Liu, Jiajie Cai, Jianjun Zhang, Haiyan Tan, Bei Cheng, Jingsan Xu. Simultaneous benzyl alcohol oxidation and H₂ generation over MOF/CdS S-scheme photocatalysts and mechanism study[J]. Chinese Journal of Catalysis, 2023, 51: 204-215.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(23)64466-3

https://www.cjcatal.com/EN/Y2023/V51/I8/204

Figures/Tables 6

Fig. 1. (a) Schematic of synthesis for UCx composite. FESEM (b), TEM (c,d), and HRTEM (e) images of UCx composites. (f) HAADF image and EDS elemental mappings of Zr, O, Cd, and S of UCx composites.

Fig. 2. (a) UV-vis diffuse reflectance spectroscopy and color change digital photographs (inset) of the samples. (b) The band structure of U6N and CdS. EPR signals of DMPO-?O2? (c) and DMPO-?OH (d) of U6N, CdS, and UC0.75 composite.

Fig. 3. (a) XPS survey spectra of CdS and UC0.75. High-resolution Zr 3d (b), Cd 3d (c) and S 2p (d) in situ XPS spectra of U6N, CdS, and UC0.75 are measured under dark and light conditions (λ = 365 nm). (e) Charge-transfer processes in an S-scheme heterojunction.

Fig. 4. 2D transient absorption surface plots of (a) CdS and (b) UC0.75 composite using a 340 nm pump pulse. The fs-TA spectra of CdS (c) and UC0.75 (d) composite signals. (e) Corresponding GSB recovery kinetics of UC0.75 at 510 nm. (f) Mechanisms underlying the photogenerated charge dynamics involved in CdS (left) and UC0.75 composite (right).

Fig. 5. (a) The photocatalytic activities of H2 evolution and BAD production on U6N, CdS, and UCx composites in three hours. (b) The conversion of BA and the selectivity of BAD on the prepared photocatalysts. Hourly photocatalytic performance (c) and photocatalytic cycle test (d) of UC0.75 composite.

Fig. 6. (a) In situ DRIFTS of adsorbed BA aqueous solution on the UC0.75 composite under dark and irradiated conditions. The first 60 minutes are for adsorption, and the next 60 minutes are for irradiation. The spectrum is measured every 10 min. (b) EPR spectra of CdS and UC0.75 composite in CH3CN solution (containing BA) with the addition of DMPO. (c) The mass spectrum of gaseous products of photocatalytic HER on UC0.75 using isotope-labeled D2O and BA as reactants. (d) Two-step single-electron oxidation and reduction mechanism of BA and H2O. (e) Proposed reaction mechanism for photoredox dual reaction for BA conversion and H2 evolution over CdS/U6N S-scheme heterojunction under light irradiation.

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Simultaneous benzyl alcohol oxidation and H₂ generation over MOF/CdS S-scheme photocatalysts and mechanism study

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