CoOx促进Mo掺杂BiVO4光电催化H2O2合成及原位降解污染物

doi:10.1016/S1872-2067(24)60175-0

催化学报 ›› 2024, Vol. 67: 176-185.DOI: 10.1016/S1872-2067(24)60175-0

CoO_x促进Mo掺杂BiVO₄光电催化H₂O₂合成及原位降解污染物

田甜^a(), 王婉婷^a, 王怡萍^a, 李可欣^a, 李园园^c, 付文升^a(), 丁勇^b()

^a重庆师范大学化学学院, 绿色催化材料与技术重庆市重点实验室, 重庆 401331
^b兰州大学化学化工学院, 甘肃省先进催化重点实验室, 功能有机分子化学国家重点实验室, 甘肃兰州 730000
^c重庆第二师范学院生物与工程学院, 重庆 400067

收稿日期:2024-08-25 接受日期:2024-10-24 出版日期:2024-12-18 发布日期:2024-11-30
通讯作者: 田甜,付文升,丁勇
基金资助:
国家自然科学基金(52102356);国家自然科学基金(22075119);重庆市巴渝学者青年项目(YS2022029);重庆市基础研究与前沿技术研究计划(cstc2020jcyj-msxmX0939);重庆市自然科学基金科技研究计划(cstc2021ycjh-bgzxm0037);重庆市教委科技研究计划(KJQN202000544);重庆市教委科技研究计划(KJZD-K201900503);重庆市教委科技研究计划(KJQN202400522);重庆师范大学博士启动/人才引进计划(21XLB014);重庆市博士后研究项目特别资助(2023CQBSHTB2004)

Mo-doping and CoO_x loading over BiVO₄ photoanode for enhancing performance of H₂O₂ synthesis and in-situ organic pollutant degradation

Tian Tian^a(), Wanting Wang^a, Yiping Wang^a, Kexin Li^a, Yuanyuan Li^c, Wensheng Fu^a(), Yong Ding^b()

^aChongqing Key Laboratory of Green Catalysis Materials and Technology, College of Chemistry, Chongqing Normal University, Chongqing 401331, China
^bState Key Laboratory of Applied Organic Chemistry, Key Laboratory of Advanced Catalysis of Gansu Province, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000, Gansu, China
^cDepartment of Biological and Chemical Engineering, Chongqing University of Education, Chongqing 400067, China

Received:2024-08-25 Accepted:2024-10-24 Online:2024-12-18 Published:2024-11-30
Contact: Tian Tian, Wensheng Fu, Yong Ding
Supported by:
National Natural Science Foundation of China(52102356);National Natural Science Foundation of China(22075119);Bayu Scholar Program(YS2022029);Chongqing Research Program of Basic Research and Frontier Technology(cstc2020jcyj-msxmX0939);Science and Technology Research Program of Natural Science Foundation of Chongqing, China(cstc2021ycjh-bgzxm0037);Science and Technology Research Program of Chongqing Municipal Education Commission(KJQN202000544);Science and Technology Research Program of Chongqing Municipal Education Commission(KJZD-K201900503);Science and Technology Research Program of Chongqing Municipal Education Commission(KJQN202400522);Doctor Start/Talent Introduction Program of Chongqing Normal University(21XLB014);Special Funding for Postdoctoral Research Projects in Chongqing(2023CQBSHTB2004)

摘要/Abstract

摘要：

光电催化阳极水氧化合成过氧化氢(H₂O₂)耦合阴极制备氢气提高了光电水分解过程的效率和经济性. 然而, 缓慢的水氧化动力学和较慢的载流子传输限制了光电催化H₂O₂的合成. 光阳极氧化水制备H₂O₂需要的电极电势(1.76 V vs. RHE)远高于水氧化的电极电势(1.23 V vs. RHE). BiVO₄光阳极合成方法简单、合成原料便宜, 其价带位置位于2.4 eV (vs.RHE), 是理想的光阳极水氧化H₂O₂材料. 但是, BiVO₄光电极表面反应速率较慢、H₂O₂的选择性较低等缺点制约了其作为光电材料的进一步发展. 因此, 构筑高效的BiVO₄光电复合材料成为解决上述问题的有效途径.

本文采用掺杂和表面负载助催化剂的方法提高了BiVO₄光电极制备H₂O₂的选择性和稳定性. 首先通过Mo的掺杂得到Mo-BiVO₄光电极. 其次, 在Mo-BiVO₄光阳极表面进行了钴氧化物(CoO_x)助催化剂的修饰制得CoO_x/Mo-BiVO₄电极. 在1.76 V_RHE的条件下, BiVO₄的电流密度是2.4 mA cm^‒2. 在相同电位下, Mo-BiVO₄的电流密度上升到2.9 mA cm^‒2, CoO_x/Mo-BiVO₄的电流密度高达4.0 mA cm^‒2. 实验结果表明, CoO_x/Mo-BiVO₄光阳极在1.7 V vs. RHE的电位下H₂O₂的产率为0.39 μmol min^‒1 cm^‒2, 远高于Mo-BiVO₄ (0.18 μmol min^‒1 cm^‒2)和BiVO₄ (0.07 μmol min^‒1 cm^‒2). 在此电压下CoO_x/Mo-BiVO₄对H₂O₂合成的选择选择性为76.9%, 而Mo-BiVO₄和BiVO₄选择性分别为47.5%和32.0%. 这表明Mo的掺杂和CoO_x的负载提高了BiVO₄电极制备H₂O₂的产率和选择性. 开光和黑暗条件下的开路电压差实验结果表明, Mo的掺杂减小了BiVO₄表面能带的弯曲程度, 有利于光电极表面H₂O₂的生成. CoO_x的负载进一步减小了Mo-BiVO₄光电极的能带弯曲程度, 同时抑制了H₂O₂的分解. 通过莫特肖特基曲线得出CoO_x/Mo-BiVO₄具有最大的载流子浓度. 瞬态和稳态荧光结果表明, Mo的掺杂和CoO_x的负载减小了BiVO₄光电极表面载流子的复合. 在1.23 V_RHE条件下测试结果表明, 与BiVO₄和Mo-BiVO₄相比，CoO_x/Mo-BiVO₄具有最好的稳定性. 密度泛函理论计算结果揭示了CoO_x的负载提高了Mo-BiVO₄光阳极生成H₂O₂的效率. 此外, CoO_x_/Mo-BiVO₄光电极原位生成的H₂O₂被用于降解水溶液中的四环素, 结果表明, CoO_x/Mo-BiVO₄在所合成的电极中显示出最佳的降解效果. 通过液质联用探究了CoO_x/Mo-BiVO₄在降解盐酸四环素中的产物, 并且提出了降解盐酸四环素可能的反应机理.

综上所述, 本文揭示了掺杂和负载助催化剂可有效提升BiVO₄电极光电合成H₂O₂的选择性和稳定性, 为高效光电催化合成H₂O₂体系的设计提供新的思路.

关键词: 过氧化氢, BiVO₄光阳极, 助催化剂, 水氧化反应, 四环素降解

Abstract:

The combination of photoelectrochemical water oxidation hydrogen peroxide (H₂O₂) on the anode and hydrogen evolution on the cathode increase the value of the water splitting process. However, the sluggish water oxidation kinetics and slow carrier transport limit the generation of H₂O₂. In this study, to promote H₂O₂ production, the surface of a Mo doped BiVO₄ photoanode was modified with CoO_x co-catalyst. The resulting CoO_x/Mo-BiVO₄ photoanode generates H₂O₂ at a rate of 0.39 μmol min^-1 cm^-2 with a selectivity of 76.9% at 1.7 V_RHE. The experimental results indicate that CoO_x decorated on Mo-BiVO₄ kinetically favors the H₂O₂ production via reduced band bending, while inhibiting H₂O₂ decomposition. According to density functional theory calculations, the loading of CoO_x enhances the efficiency of the Mo-BiVO₄ photoanode in generating H₂O₂. Moreover, the in-situ generated H₂O₂ through CoO_x/Mo-BiVO₄ was applied to the degradation of tetracycline in aqueous solution, finding that CoO_x/Mo-BiVO₄ exhibits the best performance among the catalysts evaluated. This work demonstrates that the CoO_x co-catalyst can effectively facilitate the water oxidation to H₂O₂, opening a way for its application in situ water remediation.

Key words: Hydrogen peroxide, BiVO₄ photoanode, Co-catalyst, Water oxidation reaction, Tetracycline degradation

田甜, 王婉婷, 王怡萍, 李可欣, 李园园, 付文升, 丁勇. CoO_x促进Mo掺杂BiVO₄光电催化H₂O₂合成及原位降解污染物[J]. 催化学报, 2024, 67: 176-185.

Tian Tian, Wanting Wang, Yiping Wang, Kexin Li, Yuanyuan Li, Wensheng Fu, Yong Ding. Mo-doping and CoO_x loading over BiVO₄ photoanode for enhancing performance of H₂O₂ synthesis and in-situ organic pollutant degradation[J]. Chinese Journal of Catalysis, 2024, 67: 176-185.

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图/表 8

Fig. 1. Diagram illustrating the synthesis process of CoOx/Mo-BiVO4.

Fig. 2. SEM image (a), HRTEM image (b), and TEM-EDX elemental mapping images (c-h) of CoOx/Mo-BiVO4.

Fig. 3. XPS survey spectra (a), Bi 4f (b), V 2p (c), and O 1s (d) of the BiVO4-based samples. (e) The percentage of different types oxygen in BiVO4 based photoanodes. (f) Co 2p spectra of CoOx/Mo-BiVO4 photoanode.

Fig. 4. (a) LSV curves of the obtained samples. (b) ABPE curves of different catalysts. (c) H2O2 yield and Faraday efficiency for the H2O2 evolution of BiVO4-based photoanodes. (d) Comparison of PEC H2O2 production rates across different products.

Fig. 5. Nyquist plots at 1.7 VRHE in 1 mol L-1 KHCO3 under AM 1.5G illumination (the inset shows the circuit model) (a), MS curves (b) and schematic (c) of the selective PEC H2O2 production for BiVO4-based photoanodes.

Fig. 6. (a) TRPL decay spectra and (b) EPR spectra of BiVO4-based photoanodes.

Fig. 7. The 2e- pathway for H2O2 generation (black line) and 4e- pathway for O2 production (red line) on BiVO4 (a), Mo-BiVO4 (b), CoOx/Mo-BiVO4 (c). (d) The optimized geometries for BiVO4 and Mo-BiVO4. PDOS for BiVO4 (e) and Mo-BiVO4 (f).

Fig. 8. (a) photoanodic degradation efficiency of TC. (b) The impact of various free radical inhibitors on TC degradation. (c) The proposed degradation pathway for tetracycline.

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CoO_x促进Mo掺杂BiVO₄光电催化H₂O₂合成及原位降解污染物

Mo-doping and CoO_x loading over BiVO₄ photoanode for enhancing performance of H₂O₂ synthesis and in-situ organic pollutant degradation

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