有机/无机杂化FS-COF/WO3 S型异质结电荷载流子动力学及其光催化析氢性能

doi:10.1016/S1872-2067(25)64664-X

催化学报 ›› 2025, Vol. 74: 250-263.DOI: 10.1016/S1872-2067(25)64664-X

有机/无机杂化FS-COF/WO₃ S型异质结电荷载流子动力学及其光催化析氢性能

张云超^a^,^b, 潘劲康^a, 倪响^a^,^b, 莫非奇^a^,^b, 徐远国^c, 董鹏玉^a^,^*()

^a盐城工学院, 江苏省新型环保重点实验室, 江苏盐城 224051
^b盐城工学院材料科学与工程学院, 江苏盐城 224051
^c江苏大学化学化工学院, 江苏镇江 212013

收稿日期:2025-01-08 接受日期:2025-02-25 出版日期:2025-07-18 发布日期:2025-07-20
通讯作者: *电子信箱: dongpy11@gmail.com (董鹏玉).
基金资助:
国家自然科学基金(21403184);江苏省高等学校基础科学(自然科学)研究重大项目(22KJA430008)

Revealing the dynamics of charge carriers in organic/inorganic hybrid FS-COF/WO₃ S-scheme heterojunction for boosted photocatalytic hydrogen evolution

Yunchao Zhang^a^,^b, Jinkang Pan^a, Xiang Ni^a^,^b, Feiqi Mo^a^,^b, Yuanguo Xu^c, Pengyu Dong^a^,^*()

^aKey Laboratory for Advanced Technology in Environmental Protection of Jiangsu Province, Yancheng Institute of Technology, Yancheng 224051, Jiangsu, China
^bKey Laboratory for Ecological-Environment Materials of Jiangsu Province, School of Materials Science and Engineering, Yancheng Institute of Technology, Yancheng 224051, Jiangsu, China
^cSchool of Chemistry and Chemical Engineering, Jiangsu University, Zhenjiang 212013, Jiangsu, China

Received:2025-01-08 Accepted:2025-02-25 Online:2025-07-18 Published:2025-07-20
Contact: *E-mail: dongpy11@gmail.com (P. Dong).
Supported by:
National Natural Science Foundation of China(21403184);Natural Science Foundation of the Jiangsu Higher Education Institutions of China(22KJA430008)

摘要/Abstract

摘要：

光催化技术能将太阳能转化为清洁的化学能, 被认为是解决环境污染和能源短缺问题的可行方法. 近几十年来, 开发高效的析氢光催化剂受到了广泛的关注. 然而, 无机金属氧化物光催化剂由于光学吸收利用效率有限、光生电子-空穴对分离效率低, 且缺乏足够的驱动力满足过电位需求, 限制了其在光催化析氢反应中的实际应用. 因此, 有必要开发具有可见光响应的新型有机化合物析氢光催化剂. 共价有机框架(COFs)是一类有名的可见光驱动型析氢光催化剂, 通过共价键连接有机结构单元而形成的结晶多孔聚合物. 然而, 大多数COFs表面都会发生严重的电荷载流子复合. 为了增强COFs光催化剂中电荷载流子的分离, 可以将COFs与具有适当能带结构的无机金属氧化物半导体结合起来, 形成有机/无机杂化的COFs基异质结光催化剂, 从而提高光催化析氢反应活性.

本文采用溶剂热法在具有强还原能力的砜修饰共价有机框架(FS-COF)上原位生长具有优异氧化能力的无机WO₃纳米颗粒, 设计并构建了独特的有机/无机杂化S型异质结. 研究发现, FS-COF与WO₃具有很好的交错能带排列. 最佳设计的FS-COF/WO₃-20%(即WO₃占FS-COF的质量百分数为20%)在可见光下的最大光催化析氢速率为24.7 mmol g^-1 h^-1, 是纯FS-COF的1.4倍. 并且FS-COF/WO₃-20%样品的光催化析氢速率超过了已报道的很多COFs基异质结. 此外, 由于FS-COF/WO₃的功函数不同, FS-COF/WO₃异质结能够产生有利的内建电场, 因此可以更有效地实现光生电子-空穴对分离, 从而通过一个额外的界面电子转移通道, 加速光生电子从WO₃向FS-COF的转移动力学过程, 该电子转移通道遵从定向S型迁移机制. 此外, 自旋捕获电子顺磁共振谱表明, 在单组分和形成的异质结上的•O₂⁻信号强度的对比验证了光诱导载流子遵从S型迁移机制而非II型迁移机制. 这保证了光激发电子保持在具有强还原能力的FS-COF的最低未占分子轨道上以参与光催化析氢反应, 从而显著提高了H₂的析出速率.

总之, 本文通过原位溶剂热法将还原性FS-COF与氧化性WO₃纳米颗粒杂化, 构建了具有定向内建电场的有机/无机杂化S型异质结. 该异质结具有高效的界面电子传输通道, 大大提升了光催化析氢速率. 该策略不仅为有机/无机杂化光催化剂的构建提供了新思路, 更为设计兼具强氧化还原能力与高效电荷分离特性的S型异质结体系奠定了一定理论基础, 对开发高效太阳能-氢能转换材料具有重要参考.

关键词: S型异质结, 光催化析氢, 共价有机骨架, 载流子动力学, 有机/无机杂化

Abstract:

Designing high-efficiency photocatalysts by the construction of organic/inorganic heterojunctions is considered to be an effective approach for improving photocatalytic hydrogen evolution reaction (HER) activity. This work designed and built unique S-scheme heterojunctions by in-situ growing inorganic WO₃ nanoparticles with excellent oxidation ability on fused-sulfone-modified covalent organic frameworks (FS-COF) with strong reduction ability. It is found that FS-COF and WO₃ have a well-matched staggered band alignment. The best-designed FS-COF/WO₃-20% exhibits a maximum photocatalytic HER rate of 24.7 mmol g^-1 h^-1 under visible light irradiation, which is 1.4 times greater than the pure FS-COF. Moreover, photogenerated electron-hole pairs can be separated and utilized more efficiently thanks to the FS-COF/WO₃ heterojunction's ability to create a favorable internal electric field resulting from the difference in work functions between FS-COF and WO₃, which speeds up the transfer dynamics of photoinduced electrons from WO₃ to FS-COF through an additional interfacial electron-transfer channel obeying the directional S-scheme migration mechanism. Furthermore, the S-scheme migration mechanism of photoinduced charge carriers instead of the type-II mechanism was confirmed by the signal intensity of •O₂⁻ species from spin-trapping electron paramagnetic resonance spectra over the single component and the formed heterojunction. It ensures the photoexcited electrons maintain on the lowest unoccupied molecular orbital of FS-COF with a strong reduction ability to participate in photocatalytic HER, resulting in a significantly boosted H₂ evolution rate. Based on organic/inorganic coupling, this work offers a strategy for creating particular S-scheme heterojunction photocatalysts.

Key words: S-scheme heterojunction, Photocatalytic hydrogen evolution, Covalent organic frameworks, Dynamics of charge carriers, Organic/inorganic hybrid

张云超, 潘劲康, 倪响, 莫非奇, 徐远国, 董鹏玉. 有机/无机杂化FS-COF/WO₃ S型异质结电荷载流子动力学及其光催化析氢性能[J]. 催化学报, 2025, 74: 250-263.

Yunchao Zhang, Jinkang Pan, Xiang Ni, Feiqi Mo, Yuanguo Xu, Pengyu Dong. Revealing the dynamics of charge carriers in organic/inorganic hybrid FS-COF/WO₃ S-scheme heterojunction for boosted photocatalytic hydrogen evolution[J]. Chinese Journal of Catalysis, 2025, 74: 250-263.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64664-X

https://www.cjcatal.com/CN/Y2025/V74/I7/250

图/表 8

Scheme 1. The schematic diagram for the formation of FS-COF/WO3 heterojunction.

Fig. 1. (a) XRD patterns. (b) FTIR spectra. (c) Zeta potentials. N2 adsorption-desorption isotherms tested at -196.15 °C of FS-COF (d), WO3 (e), FS-COF/WO3-20% (f), and pore size distributions (inset).

Fig. 2. (a) XPS survey spectra. The high-resolution C 1s (b), O 1s (c), N 1s (d), S 2p (e), and W 4f (f) XPS spectra.

Fig. 3. SEM images of FS-COF (a), WO3 (b), and FS-COF/WO3-20% (c). TEM images of FS-COF (d) and FS-COF/WO3-20% (e). (f) HRTEM image of FS-COF/WO3-20%. (g) EDS mapping images of FS-COF/WO3-20%.

Fig. 4. (a) Time-dependent H2 generation over prepared samples when exposed to visible light. (b) A bar graph of the photocatalytic H2 production over all as-synthesized samples. (c) The photocatalytic cycling runs over FS-COF/WO3-20%. (d) AQE of FS-COF/WO3-20% at 420, 450, 500, 550, and 600 nm. (e) The water contact angles of prepared samples. (f) UV-Vis DRS spectra and Tauc plots (inset) of samples. (g) Comparison of FS-COF/WO3-20% photocatalytic hydrogen production performance with COF-based heterojunction photocatalytic materials in the literature [20,36,40,43-49].

Fig. 5. (a) EIS Nyquist plots of as-prepared samples. (b) Transient photocurrent response. (c) Mott-Schottky plots of individual components. (d) Energy band-level positions of WO3 and FS-COF.

Fig. 6. (a) Steady-state PL spectra of FS-COF, WO3, and FS-COF/WO3-20% excited by 410 nm. Pseudocolor charts and transient absorption spectra obtained with 340 nm excitation at predetermined delay times: FS-COF (b,d) and FS-COF/WO3-20% (c,e). (f) Decay kinetic curves at 650 nm of FS-COF and FS-COF/WO3-20%.

Fig. 7. The mean electrostatic potentials determined from the surfaces of WO3 (001) (a) and FS-COF (001) (b) at the Z-axis (The corresponding optimized slab structures are displayed in each inset). (c) A constructed geometric model of the FS-COF (001)/WO3 (001) heterojunction interface. (d) Calculated 3D charge density difference distribution of FS-COF (001)/WO3 (001) interface with an isosurface value of 0.0003 e ?-3. The cyan and yellow regions represent electron depletion and accumulation, respectively. (e) DMPO spin-trapping EPR spectra of WO3, FS-COF, and FS-COF/WO3-20%. (f) A diagram showing two possible mechanisms (i.e., Type-II and S-scheme heterojunction) for charge transfer of FS-COF/ WO3-20%. (g) Diagrammatic representation of the charge migration mechanism in the FS-COF/WO3-20% heterostructure both before and after contact under dark and visible light conditions.

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有机/无机杂化FS-COF/WO₃ S型异质结电荷载流子动力学及其光催化析氢性能

Revealing the dynamics of charge carriers in organic/inorganic hybrid FS-COF/WO₃ S-scheme heterojunction for boosted photocatalytic hydrogen evolution

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[2]	李猛, 李炫华, 贾汉·B·哈西米. S型光催化体系电荷转移动力学[J]. 催化学报, 2025, 73(6): 12-15.
[3]	曹腾飞, 徐全龙, 张军, 王升高, 狄廷敏, 邓泉荣. 构建S型g-C₃N₄/BiOBr异质结以增强光催化合成过氧化氢性能[J]. 催化学报, 2025, 72(5): 118-129.
[4]	李瀚, 王往, 许凯强, 程蓓, 许景三, 曹少文. 太阳能驱动S型异质结光催化剂制备过氧化氢[J]. 催化学报, 2025, 72(5): 24-47.
[5]	岳诗雅, 李荣, 魏政荣, 高云, Karen Wilson, 陈绪兴. 构建内建电场可调的全固溶体S型异质结以实现高效光催化活性[J]. 催化学报, 2025, 71(4): 353-362.
[6]	张艳峰, 王珊. Mn_0.5Cd_0.5S/MnWO₄中的S型异质结和超晶格界面用于增强光催化产氢[J]. 催化学报, 2025, 71(4): 1-4.
[7]	吴永辉, 鄢雨晴, 邓奕翔, 黄微雅, 杨凯, 卢康强. 合理构建S型CdS量子点/In₂O₃空心纳米管异质结以增强光催化产氢[J]. 催化学报, 2025, 70(3): 333-340.
[8]	刘晓明, 姜志锋. 含有带内缺陷能级的S型异质结用于人工光合作用[J]. 催化学报, 2025, 70(3): 5-7.
[9]	许明阳, 李真真, 沈荣晨, 张欣, 张治红, 张鹏, 李鑫. 构建卟啉基共价有机框架与Nb₂C MXene的S型异质结并应用于光催化过氧化氢生产[J]. 催化学报, 2025, 70(3): 431-443.
[10]	夏兵全, 刘高雄, 樊坤, 陈润东, 刘欣, 李来全. 基于双氧还原中心的共价三嗪框架构建的1D/2D S型异质结促进过氧化氢光合作用[J]. 催化学报, 2025, 69(2): 315-326.
[11]	项祥林, 程蓓, 朱必成, 姜传佳, 梁桂杰. 高熵合金纳米晶体促进光催化析氢耦合肉桂醇选择性氧化[J]. 催化学报, 2025, 68(1): 326-335.
[12]	李世杰, 游常俊, 杨方, 梁桂杰, 庄春强, 李鑫. 界面Mo-S化学键调控Mn_0.5Cd_0.5S/Bi₂MoO₆ S型异质结增强光催化去除新兴有机污染物[J]. 催化学报, 2025, 68(1): 259-271.
[13]	毛思航, 赫荣安, 宋少青. S型异质结界面超快电子转移促进人工光合成[J]. 催化学报, 2024, 64(9): 1-3.
[14]	刘方璇, 孙彬, 刘子妍, 魏英勤, 高婷婷, 周国伟. 空位工程调控中空结构ZnO/ZnS S型异质结用于高效光催化产氢[J]. 催化学报, 2024, 64(9): 152-165.
[15]	陈春光, 张金锋, 褚海亮, 孙立贤, Graham Dawson, 代凯. 硫族化物基S型异质结光催化剂[J]. 催化学报, 2024, 63(8): 81-108.