有机-无机S型异质结增强载流子分离用于光催化产氢耦合亚胺合成

doi:10.1016/S1872-2067(26)65073-5

催化学报 ›› 2026, Vol. 87: 185-196.DOI: 10.1016/S1872-2067(26)65073-5

有机-无机S型异质结增强载流子分离用于光催化产氢耦合亚胺合成

吴昊^a^,^b, 曾芯宇^a^,^b, 王往^a^,^b^,^*(), 程蓓^a^,^b, 程敬招^a^,^b, 许景三^c^,^*(), 曹少文^a^,^b^,^*()

^a 武汉理工大学材料复合新技术全国重点实验室, 湖北武汉 430070, 中国
^b 武汉理工大学湖北省先进复合材料技术创新中心, 湖北武汉 430070, 中国
^c 昆士兰科技大学化学与物理学院材料科学中心, 昆士兰布里斯班, 澳大利亚

收稿日期:2025-11-26 接受日期:2025-12-26 出版日期:2026-08-18 发布日期:2026-06-24
通讯作者: ^*电子信箱: doublewang@whut.edu.cn (王往),
jingsan.xu@qut.edu.au (许景三),
swcao@whut.edu.cn (曹少文).
基金资助:
中央高校青年教师科研创新能力支持项目(ZYGXQNJSKYCXNLZCXM-M21);国家自然科学基金(52472245);国家自然科学基金(22278324);国家自然科学基金(22578040);国家自然科学基金(22102121);湖北省自然科学基金(2025AFA013);湖北省自然科学基金(2025AFB482)

The organic-inorganic S-scheme heterojunction with enhanced charge separation simultaneously catalyze the production of hydrogen and imine

Hao Wu^a^,^b, Xinyu Zeng^a^,^b, Wang Wang^a^,^b^,^*(), Bei Cheng^a^,^b, Jingzhao Cheng^a^,^b, Jingsan Xu^c^,^*(), Shaowen Cao^a^,^b^,^*()

^a State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070, Hubei, China
^b Hubei Technology Innovation Center for Advanced Composites, Wuhan University of Technology, Wuhan 430070, Hubei, China
^c School of Chemistry and Physics, Queensland University of Technology, Brisbane QLD 4001, Australia

Received:2025-11-26 Accepted:2025-12-26 Online:2026-08-18 Published:2026-06-24
Supported by:
Scientiﬁc Research Innovation Capability Support Project for Young Faculty(ZYGXQNJSKYCXNLZCXM-M21);National Natural Science Foundation of China(52472245);National Natural Science Foundation of China(22278324);National Natural Science Foundation of China(22578040);National Natural Science Foundation of China(22102121);Natural Science Foundation of Hubei Province(2025AFA013);Natural Science Foundation of Hubei Province(2025AFB482)

摘要/Abstract

摘要：

光催化水裂解制氢已被现代科学视为“圣杯”. 尽管近年来光催化析氢取得了显著进展, 但由于析氧反应的动力学缓慢和载流子的快速复合, 水裂解的总体效率仍然不理想. 为了解决该问题, 一种新兴的双功能光催化剂被开发应用, 将空穴定向用于低成本有机底物的选择性氧化, 不仅有效地规避了析氧反应的限制, 还同时将氧化半反应用于生产高价值化学品. 构建双功能光催化剂要求精细的能带结构设计: 一方面, 光催化剂的带隙过宽会限制光吸收范围; 另一方面, 带隙过窄会导致无法同时满足析氢和有机物氧化耦合的热力学要求. S型异质结光催化剂由一个还原型光催化剂和一个氧化型光催化剂构成, 两者在接触界面上形成内建电场并让无用载流子复合, 保留具有更强氧化还原能力的电子和空穴, 从而提高光催化剂的性能. 因此, 通过巧妙利用S型异质结来构建双功能光催化剂体系以实现高效析氢和亚胺耦合是本研究的主要研究思路.

本研究采用溶剂热-油浴法合成了芘基共轭聚合物(PyDF)/Mn_0.2Cd_0.8S (MCS)有机-无机S型异质结光催化剂, S型异质结的形成显著提高了复合材料的氧化还原能力. 其中, PyDF含量为50 wt%的PMCS_0.5样品表现出最佳性能, 以抗坏血酸为牺牲剂时的析氢速率为16.3 mmol h^-1 g^-1; 在苄胺(BA)氧化析氢耦合体系中, 析氢速率为3.72 mmol h^-1 g^-1, 且4 h内358.8 μmol BA转化为N-苄基苄胺(NBBA)的转化率接近100%. 此外, 通过密度泛函理论计算、原位X射线光电子能谱和原位开尔文探针力显微镜等技术来阐明其S型异质结内的电荷转移机制, 并利用原位红外光谱来监测胺向亚胺的逐步转化过程. 结果表明, 在PMCS_0.5复合材料中, PyDF与MCS复合后, 电子从PyDF转移到MCS, 导致PyDF侧积累正电荷, MCS侧积累负电荷, 从而在界面处引起费米能级弯曲, 并建立起从PyDF到MCS的内建电场. 在光照下, MCS的导带中的光生电子被驱动并与PyDF的最高占据分子轨道中的光生空穴重组. 因此, 电子在PyDF的最低未占有分子轨道中聚集, 而空穴则在MCS的价带中聚集. 这种载流子的空间分离有效地增强了体系的氧化还原能力, 从而提高了其光催化性能. PyDF的LUMO中的光生电子参与H⁺的还原并生成H₂, 而MCS价带中的光生空穴则快速氧化吸附在光催化剂表面的BA分子. 这种氧化引起BA的去质子化, 形成以碳为中心的自由基中间体(C₆H₅CH₂•), 该中间体进一步被另一个空穴氧化成苄胺(C₆H₅CH=NH), 同时伴随着H⁺的释放. 最终, 苄基亚胺中间体与另一个BA分子反应生成NBBA并释放NH₃, 同时产生的质子被PyDF的LUMO中的电子进一步还原, 产生额外的H₂.

综上, 本文为双功能光催化剂的设计提供了一条同时实现能量转换和绿色合成的有前景的方案, 在高效析氢的同时合成了高附加值的NBBA, 并阐明了其反应机制, 为后续双功能光催化体系设计提供了新思路.

关键词: S型异质结, 析氢, 亚胺合成, 双功能光催化体系, 原位光谱

Abstract:

Photocatalytic hydrogen production coupled with value-added chemical synthesis has attracted extensive research interests as a promising route to realize efficient conversion of solar energy to chemical energy. However, the rapid charge recombination hinders the improvement of conversion efficiency. Herein, a pyrene-based conjugated polymer (PyDF)/Mn_0.2Cd_0.8S (MCS) organic-inorganic S-scheme heterojunction photocatalyst (PMCS) was reported. The incorporation of large delocalized π-conjugation system and formation of the S-scheme heterojunction significantly enhanced the charge separation and transfer. As a result, the optimal PMCS_0.5 composite exhibited a hydrogen evolution rate of 16.3 mmol h^-1 g^-1 with ascorbic acid as sacrificial agent. In the coupled system for benzylamine (BA) oxidation and hydrogen production, it delivered a hydrogen evolution rate of 3.72 mmol h^-1 g^-1, with nearly 100% conversion of 358.8 μmol BA to N-benzylidene benzylamine (NBBA) within 4 h. To elucidate the charge transfer mechanism within the S-scheme heterojunction, density functional theory calculations, in-situ X-ray photoelectron spectroscopy, and in-situ irradiated Kelvin probe force microscopy were conducted. In addition, in-situ diffuse reflectance infrared Fourier transform spectroscopy was employed to monitor the stepwise transformation of amines to imines during the photocatalytic process. This work offers a promising approach for bifunctional photocatalyst design toward simultaneous energy conversion and green synthesis.

Key words: S-scheme heterojunction, Hydrogen evolution, Imine synthesis, Bifunctional photocatalytic system, In-situ spectroscopy

吴昊, 曾芯宇, 王往, 程蓓, 程敬招, 许景三, 曹少文. 有机-无机S型异质结增强载流子分离用于光催化产氢耦合亚胺合成[J]. 催化学报, 2026, 87: 185-196.

Hao Wu, Xinyu Zeng, Wang Wang, Bei Cheng, Jingzhao Cheng, Jingsan Xu, Shaowen Cao. The organic-inorganic S-scheme heterojunction with enhanced charge separation simultaneously catalyze the production of hydrogen and imine[J]. Chinese Journal of Catalysis, 2026, 87: 185-196.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65073-5

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图/表 7

Fig. 1. (a) Synthesis diagram of the PMCS composites. XRD patterns of PyDF (b) and MCS and PMCS composites (c).

Fig. 2. TEM (a), HRTEM (b), HAADF-STEM (c) images, and EDX mapping (d) of PMCS0.5.

Fig. 3. (a) UV-Vis DRS spectra of the prepared catalysts. UPS spectra of PyDF (b) and MCS (c). (d) Band structure diagram of PyDF and MCS.

Fig. 4. (a) Comparative analysis of hydrogen production coupling oxidation reactions over all photocatalysts within 4 h under light irradiation. (b) Comparative analysis of BA conversion amount over all photocatalysts within 4 h. (c) BA consumption, NBBA production and BA conversion rate over all photocatalysts within 4 h. (d) Photocatalytic H2 production cycling tests. (e) NBBA production and BA residual in cycling tests. (f) BA conversion rate in six cycles. TRPL spectra (g), photocurrent density curves (h), and EIS Nyquist plots (i) of the prepared catalysts.

Fig. 5. XPS survey spectra (a), and high-resolution XPS spectra of C 1s (b), Cd 3d (c), and Mn 2p (d) of PyDF, MCS and PMCS0.5.

Fig. 6. Surface morphology of PMCS0.5 under dark (a) and light (b). (c) Height map before and after light. KPFM of PMCS0.5 under dark (d) and light (e). (f) CPD changes of PMCS0.5 under dark and light conditions.

Fig. 7. The in-situ DRIFTS of PMCS0.5 under dark (a) and light irradiation for 60 min (b) in N2 atmosphere. (c) Mechanism of photocatalytic hydrogen production coupled with benzylamine oxidation of PyDF/MCS.

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有机-无机S型异质结增强载流子分离用于光催化产氢耦合亚胺合成

The organic-inorganic S-scheme heterojunction with enhanced charge separation simultaneously catalyze the production of hydrogen and imine

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