电化学处理构建表面电荷传输通道用于高效光电催化分解水

doi:10.1016/S1872-2067(21)63986-4

催化学报 ›› 2022, Vol. 43 ›› Issue (9): 2342-2353.DOI: 10.1016/S1872-2067(21)63986-4

• 可再生燃料的光催化和光电催化合成专栏 • 上一篇下一篇

电化学处理构建表面电荷传输通道用于高效光电催化分解水

李志伟^a^,^†, 黄辉庭^a^,^†, 罗文俊^a, 胡颖飞^b, 范容莉^a, 朱治^b, 王骏^b, 冯建勇^a^,^*(), 李朝升^a^,^#(), 邹志刚^b

^a南京大学现代工程与应用科学学院, 固体微结构物理国家重点实验室, 人工微结构科学与技术协同创新中心, 江苏南京210093
^b南京大学物理学院, 江苏南京210093

收稿日期:2021-09-17 接受日期:2021-11-19 出版日期:2022-09-18 发布日期:2022-07-20
通讯作者: 冯建勇,李朝升
作者简介:第一联系人：
†共同第一作者.
基金资助:
国家重点研发计划(2018YFA0209303);国家自然科学基金(51902153);国家自然科学基金(U1663228);国家自然科学基金(51972165);江苏省自然科学基金(BK20202003)

Electrochemical creation of surface charge transfer channels on photoanodes for efficient solar water splitting

Zhiwei Li^a^,^†, Huiting Huang^a^,^†, Wenjun Luo^a, Yingfei Hu^b, Rongli Fan^a, Zhi Zhu^b, Jun Wang^b, Jianyong Feng^a^,^*(), Zhaosheng Li^a^,^#(), Zhigang Zou^b

^aCollaborative Innovation Center of Advanced Microstructures, National Laboratory of Solid State Microstructures, College of Engineering and Applied Sciences, Nanjing University, Nanjing, 210093, Jiangsu, China
^bSchool of Physics, Nanjing University, Nanjing 210093, Jiangsu, China

Received:2021-09-17 Accepted:2021-11-19 Online:2022-09-18 Published:2022-07-20
Contact: Jianyong Feng, Zhaosheng Li
About author:First author contact:
†Contributed equally to this work.
Supported by:
National Key Research and Development Program of China(2018YFA0209303);National Natural Science Foundation of China(51902153);National Natural Science Foundation of China(U1663228);National Natural Science Foundation of China(51972165);Natural Science Foundation of Jiangsu Province(BK20202003)

摘要/Abstract

摘要：

理解和调控材料表面性质是研究非均相反应的重点. 对于电化学和光电化学驱动的表面催化反应, 构建表面活性位点并理解其相关的反应机理是众多研究人员关注的重点. 除表面活性位点外, 表面电荷传输通道的存在对于(光)电化学催化反应也同样重要, 因为其决定了传输到(光)电极表面有效电荷的数量. 然而, 目前关于如何构建表面电荷传输通道的研究较少.

本文以经典的钼掺杂钒酸铋光阳极为例, 通过简单的电化学还原处理在其表面原位构建了电荷传输通道, 进而实现了水氧化光电流密度约8.5倍的提升. 通过对比电化学处理前后钼掺杂钒酸铋及氧化钼电极的X射线衍射图谱、拉曼光谱、X射线光电子能谱发现, 电化学处理诱导了电极表面的羟基化反应并且产生了Mo⁵⁺组分. 这表明电化学处理诱导的氢钼青铜相(H_yMoO_x)可能在钼掺杂钒酸铋光阳极表面形成了高效的电荷传输通道. 包括电荷分离和注入效率、开路电压、阻抗谱以及稳态和瞬态荧光光谱等(光)电化学测试结果表明, 这些表面电荷传输通道的存在大幅度提高了钼掺杂钒酸铋光阳极的体相电荷分离和传输效率. 进一步通过构建电化学处理前后钼掺杂钒酸铋和氧化钼电极的能带结构, 本文提出了电化学激活钼掺杂钒酸铋光阳极的内在机理, 即: 钼掺杂钒酸铋电极表面存在氧化钼偏析相, 并严重阻碍了空穴的有效传输, 电化学处理实现了氧化钼空穴阻挡层向H_yMoO_x空穴传导层的转变, 其中H_yMoO_x的缺陷能级构成了光阳极和电解液之间的有效电荷传输通道. 针对该体系, 本课题组曾报道(J. Phys. Chem. C, 2012, 116, 5076-5081)电化学处理消除了充当表面光生载流子复合中心的氧化钼偏析相, 本文则进一步丰富并完善了之前的理解. 此外, 电化学处理构建的H_yMoO_x基表面电荷传输通道对于富氧环境敏感, 在富氧环境中会发生氧化及去质子化反应, 进而逐渐转变成阻碍空穴有效传输的氧化钼层, 使得电化学激活的钼掺杂钒酸铋光电极失去活性. 综上, 本文明确指出构建表面电荷传输通道对实现高效(光)电化学催化反应是不可或缺的, 而进一步理解和优化表面电荷传输通道也将为储能、传感、催化等其它领域的发展提供新机遇.

关键词: 太阳能水分解, 光电化学电池, 电化学处理, 电荷传输通道, 钼掺杂钒酸铋

Abstract:

Electrochemical treatment is a popular and efficient method for improving the photoelectrochemical performance of water-splitting photoelectrodes. In our previous study, the electrochemical activation of Mo-doped BiVO₄ electrodes was ascribed to the removal of MoO_x segregations, which are considered to be surface recombination centers for photoinduced electrons and holes. However, this proposed mechanism cannot explain why activated Mo-doped BiVO₄ electrodes gradually lose their activity when exposed to air. In this study, based on various characterizations, it is suggested that electrochemical treatment not only removes partial MoO_x segregations but also initiates the formation of H_yMoO_x surface defects, which provide charge transfer channels for photogenerated holes. The charge separation of the Mo-doped BiVO₄ electrode was significantly enhanced by these charge transfer channels. This study offers a new insight into the electrochemical activation of Mo-doped BiVO₄ photoanodes, and the new concept of surface charge transfer channels, a long overlooked factor, will be valuable for the development of other (photo)electrocatalytic systems.

Key words: Solar water splitting, Photoelectrochemical cell, Electrochemical treatment, Charge transfer channel, Mo-doped BiVO₄

李志伟, 黄辉庭, 罗文俊, 胡颖飞, 范容莉, 朱治, 王骏, 冯建勇, 李朝升, 邹志刚. 电化学处理构建表面电荷传输通道用于高效光电催化分解水[J]. 催化学报, 2022, 43(9): 2342-2353.

Zhiwei Li, Huiting Huang, Wenjun Luo, Yingfei Hu, Rongli Fan, Zhi Zhu, Jun Wang, Jianyong Feng, Zhaosheng Li, Zhigang Zou. Electrochemical creation of surface charge transfer channels on photoanodes for efficient solar water splitting[J]. Chinese Journal of Catalysis, 2022, 43(9): 2342-2353.

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图/表 8

Fig. 1. (a) Current-voltage curves of the same 5MBVO film successively subjected to electrochemical treatment, air oxidation (day1, day2, day3, day7, and day14), and a repeated electrochemical treatment (day15) in the dark (dotted line) and under AM 1.5G 100 mW cm-2 simulated sunlight (solid lines). (b) Photocurrent densities of the same 5MBVO film successively subjected to electrochemical treatment, air oxidation (day1, day2, day3, day7, and day14), and a repeated electrochemical treatment (day15) at 1.23 VRHE.

Fig. 2. XPS spectra of Bi 4f (a), V 2p (b), O 1s (c), and Mo 3d (d) for the 5MBVO and 5MBVO-CV films. OL, OOH, and OH2O in (c) represent the lattice O2-, surface hydroxyl-like species, and adsorbed H2O molecules, respectively. All spectra have been calibrated by the C 1s peak (284.6 eV).

Fig. 3. (a) XRD patterns of the as-prepared MoOx film and MoOx-CV film. (b) Raman spectra of the MoOx and MoOx-CV films. (c) XPS spectra of Mo 3d for the MoOx and MoOx-CV films exposed to air at different stages (day1, day3, day7, day14, and day35) after the electrochemical treatment. All spectra have been calibrated by the C 1s peak (284.6 eV). (d) Mo5+/(Mo5+ + Mo6+) ratios of the MoOx-CV film exposed to air at different stages (day1, day3, day7, day14, and day35) after the electrochemical treatment, which were calculated according to the peak areas of Mo5+ and Mo6+ in (c).

Fig. 4. ηsep values (a), ηinj values (b), and TRPL spectra (c) of the 5MBVO and 5MBVO-CV films. The TRPL spectra were collected by exciting the electrodes at 360 nm and probing at 500 nm, and the TRPL curves were fit using a double-exponential function. (d) OCP values under AM 1.5 G irradiation (100 mW cm-2). (e) EIS curves (inset: equivalent circuit model) at 1 VRHE under illumination. (f) IPCE values at 1.23 VRHE of the 5MBVO and 5MBVO-CV films. The measurements in (d-f) were conducted in a 0.1 mol L-1 potassium phosphate (KPi) aqueous solution (pH = 7).

Fig. 5. (a) CV curves of bare FTO, the MoOx film, and the MoOx-CV film measured in a K2SO4 electrolyte containing the reversible redox couple ferricyanide/ferrocyanide, [FeIII(CN)6]3-/[FeII(CN)6]4-. (b) Schematic of electrochemical treatment inducing conductivity in the MoOx film.

Fig. 6. TEM images of 5MBVO (a) and 5MBVO-CV (b) particles. HRTEM images of 5MBVO (c) and 5MBVO-CV (d) particles corresponding to the framed areas in TEM images.

Fig. 7. Schematics of the Mo-doped BiVO4/MoOx composite electrode. Detailed energy diagrams for Mo-doped BiVO4, MoOx, and the electrolyte before (a) and after (b) the electrochemical treatment.

Fig. 8. Current-voltage curves of Mo-doped BiVO4 photoelectrodes with various Mo-doping concentrations before (a) and after (b) the electrochemical treatment in the dark (dotted lines) and under AM 1.5G 100 mW cm-2 simulated sunlight (solid lines). (c) Photocurrent densities of Mo-doped BiVO4 photoelectrodes with various Mo-doping concentrations at 1.23 VRHE before and after the electrochemical treatment. Current-voltage curves of the 5MBVO-CV (d), 10MBVO-CV (e), and 20MBVO-CV (f) films (10MBVO and 20MBVO films after the electrochemical treatment are designated as 10MBVO-CV and 20MBVO-CV, respectively) after different numbers of electrochemical treatment cycles (5, 25, 50, 75, and 100 cycles). (g) Current-voltage curves of the 10MBVO-CV film after electrochemical treatment at different threshold reduction potentials (-0.9, -1.0, -1.1, and -1.2 V vs. Ag/AgCl). (h) Photocurrent density of the 10MBVO-CV film at 1.23 VRHE as a function of threshold reduction potential. Photographs of the 10MBVO-CV film undergoing electrochemical treatment at -0.9 (left) and -1.2 (right) V vs. Ag/AgCl threshold reduction potentials are shown in the inset. (i) Schematic showing that electrochemical treatment cannot activate Mo-doped BiVO4 electrodes with high contents/thicknesses of MoOx segregations.

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电化学处理构建表面电荷传输通道用于高效光电催化分解水

Electrochemical creation of surface charge transfer channels on photoanodes for efficient solar water splitting

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