通过调节反应物气体吸附电子转移行为实现热驱动ZnO光催化CO还原和H2氧化反应

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

催化学报 ›› 2021, Vol. 42 ›› Issue (9): 1538-1552.DOI: 10.1016/S1872-2067(20)63760-3

通过调节反应物气体吸附电子转移行为实现热驱动ZnO光催化CO还原和H₂氧化反应

王中明^a^,^b, 王洪^a^,^b, 王笑笑^a^,^b, 陈旬^a, 于岩^b, 戴文新^a^,^b^,^*(), 付贤智^a^,^#()

^a福州大学能源与环境光催化国家重点实验室光催化研究所, 福建福州350108
^b福州大学生态材料先进技术重点实验室, 福建福州350108

收稿日期:2020-12-02 接受日期:2020-12-31 出版日期:2021-09-18 发布日期:2021-05-16
通讯作者: 戴文新,付贤智
基金资助:
国家重点研发项目(2018YFE0208500);国家自然科学基金(21872030)

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

Zhongming Wang^a^,^b, Hong Wang^a^,^b, Xiaoxiao Wang^a^,^b, Xun Chen^a, Yan Yu^b, Wenxin Dai^a^,^b^,^*(), Xianzhi Fu^a^,^#()

^aResearch Institute of Photocatalysis, State Key Laboratory of Photocatalysis on Energy and Environment, Fuzhou University, Fuzhou 350108, Fujian, China
^bKey Laboratory of Eco-materials Advanced Technology, Fuzhou University, Fuzhou 350108, Fujian, China

Received:2020-12-02 Accepted:2020-12-31 Online:2021-09-18 Published:2021-05-16
Contact: Wenxin Dai,Xianzhi Fu
About author:^# E-mail: xzfu@fzu.edu.cn
^* Tel/Fax: +86-591-83779083; E-mail: daiwenxin@fzu.edu.cn;
Supported by:
National Key R&D Program of China(2018YFE0208500);National Natural Science Foundation of China(21872030)

摘要/Abstract

摘要：

传统热催化和低温光催化体系在实际应用中都存在技术缺陷. 近些年, 人们通过将光和热耦合, 克服它们各自的局限性, 开创了光热协同催化新领域. 目前已在CO减排、CO甲烷化和VOCs降解等诸多应用领域得到应用. 当然, 随着光热催化的发展, 研究者也一直在思考光热协同的内在作用机理. 目前大多数的机理分析都是从材料本身出发, 通过研究表面反应、光吸收或金属与载体之间的电子转移行为来探讨光热协同效应. 然而, 表面反应只是多相光催化反应的其中一个步骤, 此外还包括反应物的扩散和吸附及产物的脱附和扩散, 其中反应物的吸附过程因其多变的吸附行为可能在整个反应过程中起着重要的作用. 光热协同可能通过作用于气体吸附过程来调节反应的选择性和活性, 但到目前为止, 两者之间的内在联系尚不清楚. 所以, 从反应物气体吸附行为(尤其是吸附电子转移行为)的角度深入研究光热协同效应具有重要意义.
本文在光催化CO还原和H₂氧化体系中引入一定的热条件, 希望通过热驱动效应影响H₂/CO吸附时的电子转移行为, 进而改变反应行为. 为简化实验附加条件, 选用常见的具有合适带隙宽度以及良好光吸收的ZnO作为研究材料, 通过水热法合成了在(100)晶面具有氧空位(V_Os)的ZnO样品, 引入气敏传感系统检测不同光热条件下的H₂/CO气体吸附电子转移行为, 并结合多种原位手段从物质结构和气体吸附两个角度出发, 分析光热条件下气体吸附行为变化的机理. 与我们预测一致, 在紫外光照下随着温度的升高, 光热协同作用于(002)晶面, 原位生长了锌空位(V_Zns), 为H₂分子提供吸附位点. H₂从Vos位点吸附转移到V_Zns上, 并导致H₂(ads)从得电子转变为失电子行为(形成有利于H₂氧化的定向吸附), 从而发生H₂氧化反应. 对于同样吸附在高表面能(002)晶面上的CO分子来说, 光热协同效应通过抬升材料费米能级来改变其电子转移行为, CO(ads)由失电子转变为得电子行为(形成有利于CO还原的定向吸附), 并进一步被失去电子的H₂(ads)还原. 此外, 还发现CO或H₂的光催化氧化反应的发生只依赖于CO或H₂单分子的定向活化(不考虑O₂的吸附和活化), 表明其归属于E-R反应过程. 而CO的光催化还原反应需要同时满足CO和H₂双分子的定向活化, 可能归属于L-H反应过程. 综上, 本文研究结果表明, 光热协同内在作用可能是通过改变ZnO材料结构, 调节反应物吸附动力学中的电子转移行为, 从而引起反应物的定向活化, 进而改变反应选择性.

关键词: 光热协同, 电子转移行为, 吸附动力学控制, 原位表征, 费米能级

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

王中明, 王洪, 王笑笑, 陈旬, 于岩, 戴文新, 付贤智. 通过调节反应物气体吸附电子转移行为实现热驱动ZnO光催化CO还原和H₂氧化反应[J]. 催化学报, 2021, 42(9): 1538-1552.

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

图/表 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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通过调节反应物气体吸附电子转移行为实现热驱动ZnO光催化CO还原和H₂氧化反应

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

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