非贵金属负载共价有机框架构建异质结高效光催化产氢

doi:10.1016/S1872-2067(25)64904-7

催化学报 ›› 2026, Vol. 81: 172-184.DOI: 10.1016/S1872-2067(25)64904-7

非贵金属负载共价有机框架构建异质结高效光催化产氢

杨博霖, 靳菲, 靳治良()

北方民族大学化学与化学工程学院, 宁夏太阳能化学转化技术重点实验室, 国家民委化工技术基础重点实验室, 宁夏银川 750021

收稿日期:2025-06-23 接受日期:2025-09-04 出版日期:2026-02-18 发布日期:2025-12-26
通讯作者: *电子信箱: zl-jin@nun.edu.cn (靳治良).
作者简介:¹共同第一作者.
基金资助:
宁夏自然科学基金(2023AAC02046)

Efficient photocatalytic hydrogen production by a heterojunction strategy with covalent organic frameworks loaded with non-precious-metal semiconductors

Bolin Yang, Fei Jin, Zhiliang Jin()

School of Chemistry and Chemical Engineering, Ningxia Key Laboratory of Solar Chemical Conversion Technology, Key Laboratory for Chemical Engineering and Technology, State Ethnic Affairs Commission, North Minzu University, Yinchuan 750021, Ningxia, China

Received:2025-06-23 Accepted:2025-09-04 Online:2026-02-18 Published:2025-12-26
Contact: *E-mail: zl-jin@nun.edu.cn (Z. Jin).
About author:¹ Contributed equally to this work.
Supported by:
Natural Science Foundation of the Ningxia Hui Autonomous Region(2023AAC02046)

摘要/Abstract

摘要：

光催化分解水产氢技术是获取绿色清洁能源的途径之一, 开发可持续发展、低成本和高性能的光催化剂是首要任务. 传统的贵金属光催化剂虽表现出优异的催化性能, 但其高昂的价格和稀缺性严重限制了其大规模应用. 非贵金属基催化剂中的过渡金属硫化物具有独特的电子结构和良好的光学性能. 与其他金属硫化物相比, 硫化锰镉由于具有较高的电荷分离效率和合适的能带结构, 成为与COF样品构建异质结的最佳选择. S型异质结具有保留最大的氧化还原能力的优越性, 在异质结设计中被广泛应用. 本研究旨在探索新型的COF催化剂, 通过负载非贵金属构建S型异质结, 以促进光催化产氢效率.

本研究工作采用湿浸渍法合成了TAPT-TFPT-COF/Mn_0.2Cd_0.8S复合光催化剂. COF是由共价键连接形成的有机晶体材料, 具有较高的比表面积和优良的化学稳定性. 非贵金属和柔性单体的加入使其电荷分离途径和光学性质的优化成为可能. 非贵金属硫化物纳米棒和COF的能带结构相互交错, 形成有效的异质结, 光催化产氢实验表明, 复合催化剂比单催化剂Mn_0.2Cd_0.8S的析氢能力提高3倍. 复合催化剂性能的增强归因于异质结的构建以及柔性单体在光照下的光热协同动力学作用, 红外热成像分析光热效应并将光能转化为热能. 通过光电化学实验、原位辐照X射线光电子能谱、表面光电压测试和密度泛函理论计算, 阐明了Mn_0.2Cd_0.8S/COF复合催化剂分解水的产氢机制。首先, Mn_0.2Cd_0.8S和COF由于费米能级的差异产生空间电荷区, 同时伴随Mn_0.2Cd_0.8S能带向上弯曲, COF能带向下弯曲。这种电位差驱动电子向COF迁移, 并在Mn_0.2Cd_0.8S界面形成缺电子区, 产生的内部电场为光生电荷的定向迁移提供驱动力. 在可见光的照射下, Mn_0.2Cd_0.8S和COF半导体被激发后的电子从价带跃迁到导带. Mn_0.2Cd_0.8S价带上的空穴与COF导带上的电子在内部电场、库仑力和能带弯曲的驱动下发生复合. 复合材料相互接触后伴随着动态的界面电荷转移, Mn_0.2Cd_0.8S导带上的电子参与了H⁺的还原, COF价带上的空穴被牺牲试剂消耗. 通过合理的异质结设计策略, 复合催化剂光捕获能力和表面亲水性的增强, 提高了电荷分离效率. Mn_0.2Cd_0.8S与COF的紧密集成优化了光生电子利用效率.

综上所述, 席夫碱缩合反应合成的共价有机框架材料与非贵金属硫化物纳米棒集成复合光催化剂. 各种表征分析表明COF中引入柔性单体促进了复合催化剂中活性位点的暴露, 并加速了光生电子的转移. 有机材料与无机半导体的集成为构建高效光催化产氢系统提供了参考.

关键词: S型异质结, 金属硫化物, 光催化析氢, 共价有机骨架, 电荷转移, 内建电场

Abstract:

Rational energy band engineering and the exposure of catalytically active sites critically enhance the efficiency of the hydrogen evolution reaction. In this study, TAPT-TFPT-COF/Mn_0.2Cd_0.8S composite photocatalysts were prepared by wet impregnation. The energy bands of non-precious-metal sulfide nanorods and a covalent organic framework (COF) were interleaved for effective heterojunction construction, enabling a three-fold enhancement in hydrogen evolution compared to that of the pure Mn_0.2Cd_0.8S catalyst. The enhanced catalyst performance is attributed to the construction of heterojunctions and the synergistic photothermal dynamics of the flexible monomers under illumination, which facilitates localized charge carrier migration. Furthermore, the hydrogen evolution mechanism in the Mn_0.2Cd_0.8S/COF composites was elucidated through photoelectrochemical experiments, in-situ irradiation X-ray photoelectron spectroscopy, surface photovoltage measurements, and density functional theory. The loaded organic semiconductor materials were combined with non-precious-metal semiconductors to construct S-scheme heterojunctions with increased hydrophilicity, and the tight combination of Mn_0.2Cd_0.8S and COF optimized the photogenerated electron utilization efficiency.

Key words: S-scheme heterojunction, Metal sulfide, Photocatalytic hydrogen evolution, Covalent organic frameworks, Charge transfer, Internal electric field

杨博霖, 靳菲, 靳治良. 非贵金属负载共价有机框架构建异质结高效光催化产氢[J]. 催化学报, 2026, 81: 172-184.

Bolin Yang, Fei Jin, Zhiliang Jin. Efficient photocatalytic hydrogen production by a heterojunction strategy with covalent organic frameworks loaded with non-precious-metal semiconductors[J]. Chinese Journal of Catalysis, 2026, 81: 172-184.

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图/表 8

Fig. 1. (a) Schematic of the synthesis of the MCSC-x composite catalyst. (b) XRD patterns of Mn0.2Cd0.8S. (c) Experimental PXRD patterns of COF. (d) XRD patterns of MCSC-x (x = 10, 20, 30).

Fig. 2. Mn 2p (a), Cd 3d (b), S 2p (c), and C 1s (d) XPS spectra of Mn0.2Cd0.8S, COF, and MCSC-20 catalysts. (e) FT-IR spectrum of the TAPT-TFPT-COF catalyst. (f) Zeta potentials of Mn0.2Cd0.8S, COF, and MCSC-20 catalysts. N2 absorption-desorption curves of Mn0.2Cd0.8S (g), COF (h), and MCSC-20 (i) (the insets show the pore-size distribution curves).

Fig. 3. (a) Photocatalytic hydrogen evolution with Mn0.2Cd0.8S, COF, and MCSC-20. (b) Photocatalytic hydrogen evolution with MCSC-x catalysts (variable x represents the range of 10, 20, and 30). (c) Cyclic photocatalytic hydrogen evolution with MCSC-20. (d) TEM images of MCSC-20 after the hydrogen evolution reaction. Infrared thermography of Mn0.2Cd0.8S (g), MCSC-20 (h), and control (blank) (i) catalysts under illumination with light for 180 s.

Fig. 4. SEM images of Mn0.2Cd0.8S (a), COF (b), and MCSC-20 (c). (c-m) TEM images of MCSC-20. (e-j) EDS mapping images of MCSC-20. Water contact angles of Mn0.2Cd0.8S (o), COF (p), and MCSC-20 (q).

Fig. 5. (a) Transient photocurrent response of Mn0.2Cd0.8S, COF, and MCSC-20 catalysts. (b) LSV spectra of Mn0.2Cd0.8S, COF, and MCSC-20. (c) EIS spectra of Mn0.2Cd0.8S, COF, and MCSC-20. (d) Mott-Schottky curves of Mn0.2Cd0.8S and COF. (e) UV-vis DRS of Mn0.2Cd0.8S, COF, and MCSC-20. (f) Bandgaps of Mn0.2Cd0.8S and COF obtained from Tauc plots. (g) PL spectra of Mn0.2Cd0.8S, COF, and MCSC-20. (h) TRPL spectra of Mn0.2Cd0.8S, COF, and MCSC-20. (i) Band structure diagram of Mn0.2Cd0.8S and COF.

Fig. 6. (a,b) Optimized structural models of Mn0.2Cd0.8S and COF. (c) ΔGH* of Mn0.2Cd0.8S and Mn0.2Cd0.8S/COF. (d) ELF of the Mn0.2Cd0.8S/COF heterojunction. Band structure and state density (PDOS) of Mn0.2Cd0.8S (e-g) and COF (i-k). (h,l) Work functions of Mn0.2Cd0.8S and COF.

Fig. 7. LUMO (a) and HOMO (b) of the periodic unit of TAF-COF based on DFT calculations. (c,d) Plane-average difference density plot along the z-axis of the Mn0.2Cd0.8S/COF heterogeneous junction. (e) Diagram of the charge transfer mechanism before and after contact between Mn0.2Cd0.8S and COF.

Fig. 8. In-situ irradiation XPS spectra of Mn 2p (a), Cd 3d (b), S 2p (c), C 1s (d), N 1s (e), and O 1s (f) in Mn0.2Cd0.8S/COF. (g) Photocatalytic reaction mechanism of MCSC-x.

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非贵金属负载共价有机框架构建异质结高效光催化产氢

Efficient photocatalytic hydrogen production by a heterojunction strategy with covalent organic frameworks loaded with non-precious-metal semiconductors

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[1]	刘青桦, 蔡培庆, 李恒帅, 冀学洋, 张大凤, 蒲锡鹏. 可见光驱动的CdS/CuWO₄ S型异质结析氢体系: 界面电荷转移与光热活化的双重协同增强[J]. 催化学报, 2026, 81(2): 299-309.
[2]	胡永盛, 杜史记, 郎集会, 刘恵莲, 李雪飞, 张旗, 鲁铭, 李鑫, 李彬榕, 魏茂彬, 杨丽丽. 构建MXene衍生TiO₂/CoNiO₂双位点S型异质结: 助力C-C偶联以实现高效光催化CO₂转化为C₂H₄[J]. 催化学报, 2026, 81(2): 227-245.
[3]	王聪聪, 权永康, 石穗丽, 王国荣, 靳治良. 自组装3D/2D ZnIn₂S₄/CN-NH₄构建S型异质结用于纯水中高效制备过氧化氢[J]. 催化学报, 2026, 81(2): 259-271.
[4]	戚克振, 程蓓, Mahboobeh Setayeshmehr, Alireza Z. Moshfegh. 通过S型光催化与串联羰基化相结合实现太阳光驱动CO₂到化学品转化[J]. 催化学报, 2026, 81(2): 1-4.
[5]	徐燕东, 景子慧, 苏雯皓, 徐加乐, 王明亮. B-TiO₂@COF S型双功能光催化剂上过氧化氢生产与糠酸合成的协同耦合效应[J]. 催化学报, 2026, 80(1): 135-145.
[6]	王少单, 杨恒, 薛丽君, 张建军, 欧阳述昕, 温丽丽. 金属掺杂ZnIn₂S₄/TpPa-1 S型异质结: 通过调控氢吸附/脱附和内建电场促进双功能光催化[J]. 催化学报, 2026, 80(1): 159-173.
[7]	蒋浩朋, 李金河, 于晓慧, 董慧龙, 王伟康, 刘芹芹. β-酮烯胺共价键桥接的S型异质结实现同步光还原CO₂为CO以及茴香醇选择性氧化为茴香醛[J]. 催化学报, 2026, 80(1): 113-122.
[8]	陈润东, 张宇航, 夏兵全, 周贤龙, 张彦昭, 刘善堂. 双功能Zn_xCd_1-_xS_y/FePS₃阶梯(S)型异质结增强光催化产氢与苯甲醛性能[J]. 催化学报, 2026, 80(1): 123-134.
[9]	张璇, 周林, 闫腾, 张晓虎, 陈浩. S型共价有机框架/Ni-ZIF-8异质结的构筑及其光催化制氢性能[J]. 催化学报, 2026, 80(1): 200-212.
[10]	卞玉琴, 代凯. ZnO/COF通过Zn-N键的界面电荷转移促进光催化生成H₂O₂[J]. 催化学报, 2025, 76(9): 1-5.
[11]	李世杰, 李蕊, 董珂欣, 刘艳萍, 于欣, 李文尧, 刘通, 赵再望, 张明义, 张宾, 陈晓波. 自漂浮Bi₄O₅Br₂/磷掺杂氮化碳/碳纤维布S型异质结光催化剂增强去除新兴有机污染物[J]. 催化学报, 2025, 76(9): 37-49.
[12]	郑相阳, 吴金往, 史海峰. 双空位诱导极化场与内建电场增强的S型异质结用于去除抗生素及六价铬[J]. 催化学报, 2025, 76(9): 50-64.
[13]	艾亚婷, 熊贤强, 朱华跃, 王齐, 翁波, 杨民权. 基于S型Mn_0.5Cd_0.5S/In₂S₃异质结光催化剂的新兴污染物消除系统评估: 降解路径、毒性评价及机理分析[J]. 催化学报, 2025, 75(8): 147-163.
[14]	郑馨龙, 宋一铭, 王崇太, 高奇志, 邵钟鋆, 林佳鑫, 翟佳迪, 李静, 史晓东, 吴道雄, 刘维峰, 黄玮, 陈琦, 田新龙, 刘雨昊. 铜/锌体系多元过渡金属硫化物光催化剂的半导体特性及其光催化制氢的应用与挑战[J]. 催化学报, 2025, 74(7): 22-70.
[15]	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(7): 250-263.