硫掺杂-氮空位协同增强二维/三维S型异质结光催化合成H2O2

doi:10.1016/S1872-2067(26)64957-1

催化学报 ›› 2026, Vol. 82: 278-291.DOI: 10.1016/S1872-2067(26)64957-1

硫掺杂-氮空位协同增强二维/三维S型异质结光催化合成H₂O₂

陈春园^a^,^c, 王中辽^a^,^d, 马颖^a^,^*(), 翁波^b^,^e^,^*(), 陈士夫^a^,^c, 孟苏刚^a^,^c^,^*()

^a淮北师范大学, 绿色精准合成化学与应用教育部重点实验室, 安徽淮北 235000
^b中国科学院城市环境研究所, 福建厦门 361021
^c淮北师范大学化学与化工学院, 安徽省合成化学与应用重点实验室, 安徽淮北 235000
^d淮北师范大学物理与电子信息学院, 安徽淮北 235000
^e中国科学院大学, 北京 100049

收稿日期:2025-07-01 接受日期:2025-10-23 出版日期:2026-03-18 发布日期:2026-03-05
通讯作者: * 电子信箱: mayingdicp@163.com (马颖),bweng@iue.ac.cn (翁波),sgmeng@chnu.edu.cn (孟苏刚).
基金资助:
国家自然科学基金(52002142);国家自然科学基金(52272297);国家自然科学基金(52402116);安徽省学科/专业带头人资助计划(DTR2025015);绿色和精准合成化学及应用教育部重点实验室自主课题(KLGPSCA202502);安徽省杰出青年科学基金(2022AH020038)

Synergistic effect of S-doping and nitrogen-vacancy engineering on 2D/3D S-scheme photocatalyst for efficient photosynthesis of H₂O₂

Chunyuan Chen^a^,^c, Zhongliao Wang^a^,^d, Ying Ma^a^,^*(), Bo Weng^b^,^e^,^*(), Shifu Chen^a^,^c, Sugang Meng^a^,^c^,^*()

^aKey Laboratory of Green and Precise Synthetic Chemistry and Applications, Ministry of Education, Huaibei Normal University, Huaibei 235000, Anhui, China
^bState Key Laboratory of Advanced Environmental Technology, Institute of Urban Environment, Chinese Academy of Sciences, Xiamen 361021, Fujian, China
^cAnhui Provincial Key Laboratory of Synthetic Chemistry and Applications, School of Chemistry and Chemical Engineering, Huaibei Normal University, Huaibei 235000, Anhui, China
^dSchool of Physics and Electronic Information, Huaibei Normal University, Huaibei 235000, Anhui, China
^eUniversity of Chinese Academy of Sciences, Beijing 100049, China

Received:2025-07-01 Accepted:2025-10-23 Online:2026-03-18 Published:2026-03-05
Contact: * E-mail: mayingdicp@163.com (Y. Ma),bweng@iue.ac.cn (B. Weng),sgmeng@chnu.edu.cn (S. Meng).
Supported by:
National Natural Science Foundation of China(52002142);National Natural Science Foundation of China(52272297);National Natural Science Foundation of China(52402116);Funding Program for Leading scholar of Anhui Province(DTR2025015);Foundation of Key Laboratory of Green and Precise Synthetic Chemistry and Applications(KLGPSCA202502);Foundation of Anhui Province for Distinguished Young Scholars(2022AH020038)

摘要/Abstract

摘要：

过氧化氢(H₂O₂)作为一种重要的绿色氧化剂和潜在清洁能源, 在环境修复、化工合成及能源转换等领域具有广泛应用. 目前, 工业上主要通过高能耗、高污染的蒽醌法生产H₂O₂, 因此开发绿色、可持续的H₂O₂合成路径迫在眉睫. 光催化技术以太阳能为驱动力, 以水和氧气为原料, 有望实现H₂O₂的低碳合成, 但其实际应用仍面临光生载流子复合严重、反应动力学缓慢及依赖牺牲剂等问题. 硫改性石墨相氮化碳(CNS)虽能拓宽可见光吸收范围, 但其价带氧化能力不足, 限制了水氧化路径的效率. 本研究通过构建氮空位调控的CNS/Zn₂In₂S₅ S型异质结, 旨在实现光生电荷的高效分离与利用, 为开发无牺牲剂参与的高效H₂O₂光合成体系提供新策略.

本文创新性地将氮空位工程与S型异质结构建相结合. 通过调控硫脲煅烧时间制备了具有不同氮空位浓度的硫掺杂石墨相氮化碳(富空位Vr-CNS和贫空位Vp-CNS), 并进一步通过水热法在CNS表面原位生长Zn₂In₂S₅(ZIS)纳米花, 形成紧密的界面异质结. 该设计利用硫掺杂拓宽光吸收范围, 氮空位作为电子陷阱促进电荷分离, 同时通过S型异质结的内建电场进一步促进光生电荷分离和实现强氧化还原能力的保留, 克服了单一改性方法的局限性. X射线光电子能谱(XPS)和电子顺磁共振(EPR)证实Vr-CNS中氮空位浓度显著高于Vp-CNS. 紫外-可见漫反射光谱表明, Vr-CNS/ZIS的吸收边红移至550 nm, 可见光捕获能力增强. 结果表明, 硫掺杂可以显著改变g-C₃N₄的电子结构, 导致带隙变窄和吸收边红移. 与单体Vr-CNS, Vp-CNS和ZIS相比, Vr-CNS/ZIS复合催化剂表现出电荷转移与分离效率显著提升, 光电流密度明显增加. 值得注意的是, Vr-CNS的H₂O₂生成速率(143.3 μmol g^-1 h^-1)显著高于g-C₃N₄ (94.6 μmol g^-1 h^-1)与Vp-CNS (100.3 μmol g^-1 h^-1). 自由基捕获实验和EPR检测表明, •O₂⁻是H₂O₂生成的关键活性物种. 氮空位将O₂吸附能垒从0.95降至0.73 eV, 加速了反应决速步的进行. 结果表明, 缺陷工程(硫掺杂结合氮空位)可协同提升光催化生成H₂O₂的性能, 具体作用机制如下: 硫掺杂显著改变g-C₃N₄的电子结构, 导致其禁带宽度变窄, 吸收边发生红移; 氮空位不仅能促进电荷分离、降低电荷转移电阻, 还可通过以下途径加速表面反应: (1)提高界面电荷转移效率; (2)利用富电子的氮空位降低O₂吸附能垒, 加速反应决速步. 光电化学测试、自由基捕获实验、原位XPS, EPR和密度泛函理论计算结果证实, 异质结界面存在由CNS指向ZIS的内建电场, 驱动ZIS的电子与CNS的空穴复合, 从而保留高能电子(CNS导带)和空穴(ZIS价带). 采用电化学分析方法阐明Vr-CNS与ZIS耦合调控生成H₂O₂过程中的动力学行为. Vr-CNS/ZIS的阴极线性扫描伏安曲线对应的塔菲尔斜率(5.8 mV dec^-1)远低于Vr-CNS (24.2 mV dec^-1)和纯ZIS (21.1 mV dec^-1). 这证实了氮空位与S型异质结的协同作用在提高光催化生成H₂O₂效率方面发挥着关键作用. 最终, Vr-CNS/ZIS的H₂O₂生成速率得到显著提升, 达到475.6 μmol g^-1 h^-1, 约为原始g-C₃N₄的5倍.

综上, 本研究为设计“缺陷增强型S型异质结”提供了新策略, 该类异质结可实现高效电荷分离与高性能H₂O₂合成的协同整合. 该工作不仅推动了非牺牲剂体系下H₂O₂绿色合成的进展, 也为多相光催化剂中电荷分离与反应路径的精准调控提供了理论参考.

关键词: 光催化, 过氧化氢, 硫掺杂石墨相氮化碳, 氮空位, S型异质结

Abstract:

The green photocatalytic synthesis of hydrogen peroxide (H₂O₂) has attracted considerable attention as an environmentally friendly approach for H₂O₂ production. However, the rapid recombination of photogenerated charge carriers, reliance on sacrificial agents, and low activity and selectivity of photocatalytic H₂O₂ remain major challenges for the further development of this process. In this study, we synthesized an S-scheme composite photocatalyst composed of N-vacancy-tailored, sulfur-modified graphitic carbon nitride (Vr-CNS) and Zn₂In₂S₅ (ZIS) that enabled solar-driven H₂O₂ synthesis, achieving a rate of 475.6 μmol g^-1 h^-1 in pure water and air without sacrificial agents. This represents a five-fold enhancement over pristine graphitic carbon nitride (g-C₃N₄). S-doping mainly altered the electronic structure of g-C₃N₄, resulting in bandgap narrowing and a redshift of the absorption edge. N vacancies (N_V) not only promoted charge separation and reduced charge transfer resistance, but also accelerated surface reactions. Moreover, N_V lowered the energy barrier due to O₂ adsorption, which is the rate-determining step, thereby accelerating the reaction. The S-scheme Vr-CNS/ZIS heterojunction retained the strong reduction ability of Vr-CNS and robust oxidation capability of ZIS. The presence of N_V strengthened the electronic coupling between Vr-CNS and ZIS after heterojunction contact. The synergistic effect of defect engineering (sulfur doping coupled with nitrogen vacancies) and the S-scheme accelerated the reaction kinetics, promoting the migration and separation of the photogenerated carriers. This study provides an effective strategy for the design of multifunctional photocatalysts by exploiting the synergy between defect engineering and S-scheme heterojunctions.

Key words: Photocatalysis, H₂O₂, S-doped g-C₃N₄, Nitrogen vacancies, S-scheme heterojunctions

陈春园, 王中辽, 马颖, 翁波, 陈士夫, 孟苏刚. 硫掺杂-氮空位协同增强二维/三维S型异质结光催化合成H₂O₂[J]. 催化学报, 2026, 82: 278-291.

Chunyuan Chen, Zhongliao Wang, Ying Ma, Bo Weng, Shifu Chen, Sugang Meng. Synergistic effect of S-doping and nitrogen-vacancy engineering on 2D/3D S-scheme photocatalyst for efficient photosynthesis of H₂O₂[J]. Chinese Journal of Catalysis, 2026, 82: 278-291.

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图/表 7

Fig. 1. SEM images of Vr-CNS (a), ZIS (b), and Vr-CNS/ZIS (c). TEM image (d), magnified TEM image (e), and EDX spectrum (f) of Vr-CNS/ZIS. HRTEM images (g,j-l), corresponding FFT images (h,i), and element mapping (m-r) of Vr-CNS/ZIS.

Fig. 2. XRD patterns (a,b), FTIR spectra (c), and EPR spectra (d) of the synthesized ZIS, Vr-CNS, Vp-CNS, Vp-CNS/ZIS, and Vr-CNS/ZIS samples. N 1s (e) and C 1s (f) high-resolution XPS spectra of Vr-CNS and Vp-CNS.

Fig. 3. High-resolution XPS spectra of C 1s (a), N 1s (b), In 3d (c), and S 2p (d) in Vr-CNS/ZIS. The workfunctions for ZIS (001) (e), monolayer Vr-CNS (001) (f), and Vp-CNS (001) (g). Side views of the induced charge density difference of Vp-CNS/ZIS (h) and Vr-CNS/ZIS (i) plotted using an isosurface of 7.9 × 10-4 e ?-3 (charge accumulation is shown in yellow, and charge depletion is shown in cyan).

Fig. 4. UV-vis DRS spectra (a) and band-gap energies (b) of the as-prepared samples. M-S plots of Vr-CNS (c), ZIS (d), and Vp-CNS (e). (f) Relationships between redox potentials of Vr-CNS, Vp-CNS and ZIS, radicals, and H2O2 production.

Fig. 5. (a) DMPO spin-trapping EPR spectra recorded for ?O2? under light irradiation for ZIS, Vr-CNS, Vp-CNS, Vp-CNS/ZIS, and Vr-CNS/ZIS samples. C 1s (b), N1s (c), S 2p (d), and In 3d (e) in-situ XPS spectra of Vr-CNS/ZIS composite in the dark and under visible light. Photocurrent responses (f), EIS spectra (g), PL spectra (h), and the average lifetime (τave) values (i) of ZIS, Vr-CNS, Vp-CNS, and Vp-CNS/ZIS, and Vr-CNS/ZIS composites.

Fig. 6. (a) Standard absorption curve of H2O2. (b) H2O2 production activities of ZIS, Vr-CNS, Vp-CNS, Vp-CNS/ZIS, and Vr-CNS/ZIS composites under visible light illumination. (c) H2O2 production activities of ZIS and Vr-CNS/ZIS composites with different contents of Vr-CNS. (d) Photocatalytic activity of Vr-CNS/ZIS under different wavelengths of light. (e) Cyclic stability test of ZIS, Vr-CNS, and Vr-CNS/ZIS for photocatalytic H2O2 production. Cathodic LSV curves (f) and corresponding Tafel slopes (g), anodic LSV curves (h), and corresponding Tafel slopes (i) of ZIS, CNS, and Vp-CNS/ZIS and Vr-CNS/ZIS composites.

Fig. 7. (a) Single-variable control experiments of species capture. EPR spectra of TEMPO-e? (b), TEMPO-h+ (c), and DMPO-?OH (d) for the as-prepared ZIS, Vr-CNS, Vp-CNS, Vp-CNS/ZIS, and Vr-CNS/ZIS composites upon visible light irradiation. (e) In-situ DRIFTS spectra of Vr-CNS/ZIS. (f) Free-energy diagrams for the reduction of O2 to H2O2 on Vr-CNS and Vp-CNS. (g) Mechanism of photocatalytic H2O2 production over Vr-CNS/ZIS.

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硫掺杂-氮空位协同增强二维/三维S型异质结光催化合成H₂O₂

Synergistic effect of S-doping and nitrogen-vacancy engineering on 2D/3D S-scheme photocatalyst for efficient photosynthesis of H₂O₂

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