缺陷工程促进TiO2/Zn0.5Cd0.5S S型异质结电荷转移实现高效光催化析氢

doi:10.1016/S1872-2067(25)64909-6

催化学报 ›› 2026, Vol. 84: 117-129.DOI: 10.1016/S1872-2067(25)64909-6

缺陷工程促进TiO₂/Zn_0.5Cd_0.5S S型异质结电荷转移实现高效光催化析氢

张宝龙^a, 孙彬^a(), 刘兴朋^a, 刘文宇^b, 顾少楠^a, 周国伟^a()

^a 齐鲁工业大学(山东省科学院)化学与化工学院, 山东省高校轻工精细化学品重点实验室, 济南市多尺度功能材料工程实验室, 山东济南 250353
^b 齐鲁工业大学(山东省科学院)机械工程学院, 山东济南 250353

收稿日期:2025-08-23 接受日期:2025-09-22 出版日期:2026-05-18 发布日期:2026-04-16
通讯作者: *电子信箱: binsun@qlu.edu.cn (孙彬),
gwzhou@qlu.edu.cn (周国伟).
基金资助:
国家自然科学基金(52202102);国家自然科学基金(52472215);国家自然科学基金(52202007);齐鲁工业大学(山东省科学院)科教产融合创新试点工程重大创新科研专项项目(2025ZDZX08);山东省重点研发计划(2024TSGC0222);齐鲁工业大学(山东省科学院)学科交叉融合创新引导项目(2025XKJC0103)

Defect-engineered S-scheme charge transfer in TiO₂/Zn_0.5Cd_0.5S heterojunction for high-efficiency photocatalytic hydrogen evolution

Baolong Zhang^a, Bin Sun^a(), Xingpeng Liu^a, Wenyu Liu^b, Shaonan Gu^a, Guowei Zhou^a()

^a Key Laboratory of Fine Chemicals in Universities of Shandong, Jinan Engineering Laboratory for Multi-scale Functional Materials, School of Chemistry and Chemical Engineering, Qilu University of Technology (Shandong Academy of Sciences), Jinan 250353, Shandong, China
^b Faculty of Mechanical Engineering, Qilu University of Technology (Shandong Academy of Sciences), Jinan 250353, Shandong, China

Received:2025-08-23 Accepted:2025-09-22 Online:2026-05-18 Published:2026-04-16
Contact: *E-mail: binsun@qlu.edu.cn (B. Sun),
author.gwzhou@qlu.edu.cn (G. Zhou).
Supported by:
National Natural Science Foundation of China(52202102);National Natural Science Foundation of China(52472215);National Natural Science Foundation of China(52202007);Key Innovation Project of the Science-Education-Industry Integration Pilot Engineering of Qilu University of Technology (Shandong Academy of Sciences)(2025ZDZX08);Key Research & Development Project of Shandong Province(2024TSGC0222);Interdisciplinary Innovation Guidance Program from Qilu University of Technology (Shandong Academy of Sciences)(2025XKJC0103)

摘要/Abstract

摘要：

利用太阳能驱动半导体光催化分解水产氢是应对能源短缺与环境污染的重要途径, TiO₂因其优异的化学稳定性、可调控的形貌且制备成本低廉, 而成为光催化领域的经典材料. 然而, 单一TiO₂固有的宽带隙和光生载流子易复合的本征缺陷, 严重限制了其光催化性能. 同时, 三元硫化物Zn_xCd_1‒_xS虽可见光吸收强、能带结构可调, 却易发生光腐蚀且载流子复合速率快, 稳定性与活性难以兼顾的缺陷. 针对这些问题, 科研工作者一直致力于通过缺陷工程、晶型调控、构建异质结构等策略来提升其光催化性能. 在众多策略中, 利用缺陷工程与S型异质结构建的协同策略, 可拓宽光吸收范围、促进光生载流子空间分离, 同时保留光催化反应所需的强氧化还原能力, 为突破单一光催化剂性能瓶颈、提升光催化分解水产氢效率提供了关键解决方案.

本文采用水热法在氧空位介导的三维分层花状TiO₂上原位生长了Zn_0.5Cd_0.5S纳米颗粒, 构建了具有双电荷转移路径的氧空位TiO₂/Zn_0.5Cd_0.5S S型异质结光催化剂(TiO₂-Ov/Zn_0.5Cd_0.5S). 在模拟太阳光照射下, 最优的TiO₂-Ov/Zn_0.5Cd_0.5S异质结光催化析氢速率可达到15.31 mmol g^-1 h^-1, 分别是TiO₂, TiO₂-Ov, Zn_0.5Cd_0.5S和不含氧空位的TiO₂/Zn_0.5Cd_0.5S的306.2倍、56.7倍、4.7倍和1.9倍, 其性能优于大部分已报道的TiO₂基和三元硫化物基光催化剂. 利用X射线粉末衍射、扫描电子显微镜和电子顺磁共振光谱等表征证实了TiO₂-Ov/Zn_0.5Cd_0.5S异质结中氧空位的存在. 此外, 原位X射线光电子能谱、开尔文探针力显微镜、飞秒瞬态吸收光谱、电子自旋共振光谱和密度泛函理论计算等揭示了S型电荷迁移机理. 同时, 通过对H*吸附吉布斯自由能(ΔG_H^*)的理论计算表明水分子解离产生的H*优先在Zn_0.5Cd_0.5S中的S位点完成吸附、积累与电子转移, 最终结合形成H₂.

综上, 该体系光催化析氢性能的提升可归因于氧空位与S型异质结的协同作用赋予了光催化剂优异的光吸收能力、高效的光生载流子空间分离与转移效率以及强的氧化还原能力. 另外, TiO₂-Ov/Zn_0.5Cd_0.5S异质结中氧空位的引入能够在TiO₂的能带结构中形成新的缺陷能级, 可有效促进TiO₂-Ov中的光生电子与Zn_0.5Cd_0.5S中的光生空穴发生复合, 从而形成了双电荷转移路径. 本研究通过缺陷工程与S型异质结的协同设计, 为构建高效光催化分解水产氢材料提供了可行思路, 对太阳能燃料转化领域具有重要参考价值.

关键词: 缺陷工程, TiO₂/Zn_0.5Cd_0.5S, S型异质结, 双电荷转移路径, 光催化析氢

Abstract:

Photocatalytic water splitting for H₂ evolution represents a viable approach to address energy and environmental challenges, but it still remains a significant challenge by inefficient light absorption, insufficient charge separation, and weak redox potentials. To tackle these problems, a defect-engineered S-scheme photocatalyst is designed and constructed by in-situ growing Zn_0.5Cd_0.5S nanoparticles on flower-like TiO₂ microspheres with oxygen vacancies (TiO₂-Ov) via a hydrothermal method, thus forming defect-engineered TiO₂-Ov/Zn_0.5Cd_0.5S S-scheme heterojunction. Remarkably, the optimal heterojunction achieves a superior H₂ evolution rate of 15.31 mmol g^-1 h^-1, surpassing those of TiO₂, TiO₂-Ov, Zn_0.5Cd_0.5S, and defect-free TiO₂/Zn_0.5Cd_0.5S by factors of 306.2, 56.7, 4.7, and 1.9, respectively. Notably, the presence of oxygen vacancies in TiO₂-Ov enables a broadened light absorption and introduces an intermediate energy level to provide an additional photo-induced charge transfer channel within the S-scheme heterojunction. Combining with defect engineering and S-scheme mechanism, the photocatalytic system significantly exhibits enhanced light-harvesting ability, accelerated the spatial separation and transfer of photo-induced charge, and preserved strong redox power. Simultaneously, the S-scheme charge transfer pathway in the TiO₂-Ov/Zn_0.5Cd_0.5S heterojunction is systematically validated through a combination of in-situ irradiated X-ray photoelectron spectroscopy, kelvin probe force microscopy, femtosecond transient absorption spectra, electron paramagnetic resonance, and density functional theory calculation. This work highlights the synergistic effect of defect engineering and S-scheme heterojunction in boosting photocatalytic H₂ evolution, offering insights for designing high-performance photocatalyst.

Key words: Defect engineering, TiO₂/Zn_0.5Cd_0.5S, S-scheme, Dual charge transfer pathways, Photocatalytic H₂ evolution

张宝龙, 孙彬, 刘兴朋, 刘文宇, 顾少楠, 周国伟. 缺陷工程促进TiO₂/Zn_0.5Cd_0.5S S型异质结电荷转移实现高效光催化析氢[J]. 催化学报, 2026, 84: 117-129.

Baolong Zhang, Bin Sun, Xingpeng Liu, Wenyu Liu, Shaonan Gu, Guowei Zhou. Defect-engineered S-scheme charge transfer in TiO₂/Zn_0.5Cd_0.5S heterojunction for high-efficiency photocatalytic hydrogen evolution[J]. Chinese Journal of Catalysis, 2026, 84: 117-129.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64909-6

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图/表 9

Fig. 1. (a) Schematic diagram of synthesis process of TiO2-Ov/Zn0.5Cd0.5S. (b) XRD patterns of TiO2, TiO2-Ov, Zn0.5Cd0.5S, and TiO2-Ov/Zn0.5Cd0.5S heterojunction with different Zn0.5Cd0.5S content. (c) EPR spectra of TiO2, TiO2-Ov, and TZCS-50wt%.

Fig. 2. FESEM images of TiO2-Ov (a,b), Zn0.5Cd0.5S (c), and TZCS-50wt% (d,e). TEM image (f), HRTEM image (g), fast Fourier transform patterns (h), and elemental mappings (i-n) of Ti, O, Zn, Cd, and S of TZCS-50wt%.

Fig. 3. (a) XPS survey spectra of TiO2-Ov, Zn0.5Cd0.5S, and TZCS-50wt%. High-resolution XPS spectra of Ti 2p (b), O 1s (c), Zn 2p (d), Cd 3d (e), and S 2p (f) of TiO2-Ov, Zn0.5Cd0.5S, and TZCS-50wt% with and without light irradiation.

Fig. 4. UV-vis diffuse reflectance spectra (a) and Tauc plots (b) of TiO2, TiO2-Ov, Zn0.5Cd0.5S, and TiO2-Ov/Zn0.5Cd0.5S heterojunctions. Density of states and energy band structures of TiO2-Ov (c) and Zn0.5Cd0.5S (d). Mott-Schottky plots (e?g) and VB-XPS spectra (h) of TiO2, TiO2-Ov, and Zn0.5Cd0.5S. Corresponding to band structure diagram (i).

Fig. 5. Transient photocurrent spectra (a), EIS Nyquist plots (b), PL spectra (c), and LSV curves (d) of as-prepared samples.

Fig. 6. Photocatalytic H2 evolution (a) and photocatalytic H2 evolution rate (b) of as-obtained samples. Recycling H2 evolution tests (c) of TZCS-50wt%. Comparison of photocatalytic H2 evolution rate (d) of TiO2-Ov/Zn0.5Cd0.5S heterojunction with other reported photocatalysts. Structural model and H-adsorption free energy for Cd and S sites in Zn0.5Cd0.5S via DFT calculation (e).

Fig. 7. KPFM images (a,b) and corresponding to surface potential profiles (c) of TZCS-50wt% with and without light irradiation. Pseudo color plot (d), fs-TA (e), and normalized time profile (f) of TZCS-50wt%.

Fig. 8. EPR spectra of DMPO-?OH (a) and DMPO-?O2- (b) over TiO2-Ov, Zn0.5Cd0.5S, and TZCS-50wt% under light and dark conditions. DFT calculated electrostatic potentials of TiO2-Ov (c) and Zn0.5Cd0.5S (d). The charge density difference from front view (e) and planar-averaged charge density difference (f) of TiO2-Ov/Zn0.5Cd0.5S. Schematic diagram of S-scheme mechanism over TiO2-Ov/Zn0.5Cd0.5S heterojunction: before contact, after contact, and light irradiation (g).

Fig. 9. Proposed photocatalytic H2 mechanism of TiO2-Ov/Zn0.5Cd0.5S S-scheme heterojunction under simulated sunlight irradiation.

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缺陷工程促进TiO₂/Zn_0.5Cd_0.5S S型异质结电荷转移实现高效光催化析氢

Defect-engineered S-scheme charge transfer in TiO₂/Zn_0.5Cd_0.5S heterojunction for high-efficiency photocatalytic hydrogen evolution

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