Thermo-driven photocatalytic CO reduction and H2 oxidation over ZnO via regulation of reactant gas adsorption electron transfer behavior

doi:10.1016/S1872-2067(20)63760-3

Abstract

Abstract:

Photothermal catalysis is a widely researched field in which the reaction mechanism is usually investigated based on the photochemical behavior of the catalytic material. Considering that the adsorption of reactants is essential for catalytic reactions to occur, in this study, the synergistic effect of photothermal catalysis is innovatively elucidated in terms of the electron transfer behavior of reactant adsorption. For the H₂ + O₂ or CO + H₂ reaction systems over a ZnO catalyst, UV irradiation at 25 °C or heat without UV irradiation did not cause H₂ oxidation or CO reduction; only photothermal conditions (100 or 150 °C + UV light) initiated the two reactions. This result is related to the electron transfer behavior associated with the adsorption of CO or H₂ on ZnO, in which H₂ or CO that lost an electron could be oxidized by O₂ or hydroxyls. However, the electron-accepting CO could be reduced by the electron-donating H₂ into CH₄ under photothermal conditions. Based on the in-situ characterization and theoretical calculation results, it was established that the synergistic effect of the photothermal conditions acted on the (002) crystal surface of ZnO to stimulate the growth of zinc vacancies, which resulted in the formation of defect energy levels, adsorption sites, and an adjusted Fermi level. As a result, the electron transfer behavior between adsorbed CO or H₂ and the crystal surface varied, which further affected the photocatalytic behavior. The results show that the effect of photothermal synergy may not only produce the expected kinetic energy, but more importantly, produce energy that can change the activation mode of the reactant gas. This study provides a new understanding of the CO catalytic oxidation and reduction processes over semiconductor materials.

Key words: Photothermal synergy, Electron transfer behavior, Adsorption kinetic control, In-situ characterization, Fermi level

Zhongming Wang, Hong Wang, Xiaoxiao Wang, Xun Chen, Yan Yu, Wenxin Dai, Xianzhi Fu. Thermo-driven photocatalytic CO reduction and H₂ oxidation over ZnO via regulation of reactant gas adsorption electron transfer behavior[J]. Chinese Journal of Catalysis, 2021, 42(9): 1538-1552.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(20)63760-3

https://www.cjcatal.com/EN/Y2021/V42/I9/1538

Figures/Tables 14

Fig. 1. H2 conversions in the photothermal catalytic H2 oxidation reaction (a) and CH4 yields in the CO reduction reaction (b) over the ZnO catalyst under different photothermal conditions.

Fig. 2. Gas sensitivity response of H2 (a,c) and CO (b,d) adsorption on the surface of ZnO in N2 atmosphere. (a) and (b) were measured at different temperatures under UV irradiation: (1) 25 °C, (2) 50 °C, (3) 100 °C, (4) 150 °C, and (5) 200 °C. (c) and (d) were measured under dark conditions at 150 °C. (e) Schematic diagram of the gas sensing test system.

Fig. 3. In-situ XRD spectra of the ZnO samples at different temperatures. (1) at 25 °C; (2) 50 °C; (3) 100 °C; (4) 150 °C.

Fig. 4. In-situ DRS spectra of the ZnO sample under different photothermal conditions. (a) at 25 °C as a function of UV irradiation time. (1) dark conditions; (2) UV irradiation for 20 min; (3) UV irradiation for 40 min, and (4) UV irradiation for 60 min. (b) Under dark and (c) UV irradiation conditions as a function of temperature. (1) 25 °C; (2) 50 °C; (3) 100 °C; (4) 150 °C.

Fig. 5. In-situ EPR spectrum of the ZnO sample under UV irradiation at 25 °C (1), 50 °C (2), 100 °C (3), and 150 °C (4). The VZns were formed in-situ under the synergistic action of photothermal conditions.

Fig. 6. In-situ UPS profiles of the ZnO sample at 25 °C (1), 50 °C (2), 100 °C (3), 150 °C (4), and 200 °C (5). (b) An enlarged view of the cutoff edge region in (a).

Fig. 7. Diagram indicating the changes in the Fermi level at different temperatures under UV irradiation. The Fermi level change assumes an “S-shaped curve” trend.

Fig. 8. In-situ DRIFT spectra of the ZnO sample after H2 adsorption for 20 min under different conditions. (a): (1) fresh catalyst; (2) at 25 °C under UV irradiation; (3) at 50 °C under UV irradiation; (4) at 100 °C under UV irradiation; (5) at 150 °C under UV irradiation. (b) In-situ DRIFT spectra of the ZnO sample at 150 °C under UV irradiation as a function of H2 adsorption time. (1) for 5 min, (2) for 10 min, (3) for 15 min, and (4) for 20 min.

Fig. 9. H2 chemisorption on the ZnO (100) (a) and (002) (b) surfaces at the different sites: (1) the H2 non-dissociative adsorption at the O site; (2) the H2 non-dissociative adsorption at the Zn site; (3) the H2 non-dissociative adsorption at the VOs or VZns sites; (4) the H2 dissociative adsorption at the VOs or VZns sites. Among them, the surface energies (Esur) of the (100) and (002) surfaces are 0.86 and 3.13 J?m-2, respectively.

Fig. 10. In-situ DRIFT spectra of the ZnO sample under different conditions (a?c). (1) ZnO prior to CO adsorption at 25 °C under UV irradiation; (2) CO adsorption for 20 min at 25 °C under UV irradiation; (3) CO adsorption for 20 min at 50 °C under UV irradiation; (4) CO adsorption for 20 min at 100 °C under UV irradiation; (5) CO adsorption for 20 min at 150 °C under UV irradiation.

Table 1 Assignment of the infrared peaks observed after adsorption of pure CO and CO + H2 on the ZnO surface.

Species	Pure CO (cm^-1)	CO + H₂ (cm^-1)
υ(CO₃^2-)	1662, 1510, 1374, 1310	1376
υ_as(COO)	1606	1597
υ_s(COO)	1547	1339
δ(CH₃,CH₂)	1427, 1458	1475
υ_as(CH₃,CH₂)	3000, 2946	2970
υ_s(CH₃,CH₂)	2904	2900
υ(HCO₃-)	—	1249
υ(C-O)-CH₃O-	1076, 1012	1058

Fig. 11. In-situ DRIFT spectra of the ZnO sample in N2 atmosphere at 25 °C (1), 50 °C (2), 100 °C (3), and 150 °C (4). The surface hydroxyl groups decreased gradually with an increase in the temperature.

Fig. 12 In-situ DRIFT spectra of the ZnO sample at 150 °C under dark and UV irradiation conditions (a?c). (1) CO + H2 adsorption for 10 min in the dark; (2) CO + H2 adsorption for 20 min in the dark; (3) CO + H2 adsorption for 10 min under UV irradiation; (4) CO + H2 adsorption for 15 min under UV irradiation; (5) CO + H2 adsorption for 20 min under UV irradiation.

Fig. 13 Photothermal synergistic effect on the (002) surface of the ZnO sample: (a) provides energy to overcome the energy barrier and enhances the lattice vibration; (b) raises the Fermi level and forms a zinc vacancy adsorption level; (c) and (d) regulates the electron transfer behavior of H2 and CO adsorption, and the further photocatalytic oxidation and reduction reactions.

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Thermo-driven photocatalytic CO reduction and H₂ oxidation over ZnO via regulation of reactant gas adsorption electron transfer behavior

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