构建噻二唑功能化CTF基S型异质结用于高效光催化合成H2O2

doi:10.1016/S1872-2067(26)65079-6

催化学报 ›› 2026, Vol. 87: 170-184.DOI: 10.1016/S1872-2067(26)65079-6

构建噻二唑功能化CTF基S型异质结用于高效光催化合成H₂O₂

刘高雄^a, 陈润东^a, 夏兵全^a^,^*(), 周贤龙^b, 李来全^c^,^*(), 刘善堂^a^,^*()

^a 武汉工程大学化学与环境工程学院, 湖北武汉 430074
^b 南京林业大学化学工程学院, 江苏南京 210037
^c 上海理工大学能源材料科学研究院, 上海 200093

收稿日期:2025-11-22 接受日期:2026-01-16 出版日期:2026-08-18 发布日期:2026-06-24
通讯作者: ^*电子信箱: xiab@wit.edu.cn (夏兵全),
stliu@wit.edu.cn (刘善堂),
lqli@usst.edu.cn (李来全).
基金资助:
国家自然科学基金(22409151);国家自然科学基金(22402083);国家自然科学基金(22405173);武汉工程大学科学基金(23QD02);国家留学基金管理委员会

Thiadiazole-functionalized covalent triazine frameworks for constructing S-scheme heterojunctions enabling boosted H₂O₂ photosynthesis

Gaoxiong Liu^a, Rundong Chen^a, Bingquan Xia^a^,^*(), Xianlong Zhou^b, Laiquan Li^c^,^*(), Shantang Liu^a^,^*()

^a State Key Laboratory of Green and Efficient Development of Phosphorus Resources, School of Chemistry and Environmental Engineering, Wuhan Institute of Technology, Wuhan 430074, Hubei, China
^b Jiangsu Co-Innovation Centre of Efficient Processing and Utilization of Forest Resources, College of Chemical Engineering, Nanjing Forestry University, Nanjing 210037, Jiangsu, China
^c Institute of Energy Materials Science, University of Shanghai for Science and Technology, Shanghai 200093, China

Received:2025-11-22 Accepted:2026-01-16 Online:2026-08-18 Published:2026-06-24
Supported by:
National Natural Science Foundation of China(22409151);National Natural Science Foundation of China(22402083);National Natural Science Foundation of China(22405173);Science Foundation of Wuhan Institute of Technology(23QD02);China Scholarship Council

摘要/Abstract

摘要：

利用光催化将水和氧气直接合成过氧化氢(H₂O₂)是一种前景广阔的绿色人工光合成途径, 其核心在于开发高效催化剂, 以促进两步单电子氧还原反应. 聚合物氮化碳(g-C₃N₄)存在可见光吸收能力弱、载流子复合快、活性位点不足等问题, 导致其光催化合成H₂O₂效率低下, 而构建S型异质结是增强内建电场和促进电荷分离的常用策略. 目前, 共价三嗪框架(CTFs)基S型异质结中还原组分(如CTFs)的能带调控及其活性位点的关键作用尚不明确. 结构可调的CTFs材料, 可通过引入给电子与受电子单元来构建清晰的给体-受体(D-A)结构, 从而实现能带调控、优化载流子动力学并创建高效活性位点. 将此类CTFs作为S型异质结中的还原型催化剂, 有望协同实现宽光谱吸收、高效电荷分离与定向表面反应.

本研究通过将g-C₃N₄与具有不同给体-受体结构单元的共价三嗪框架(CTFs)进行组装, 构建了有机/有机S型异质结(CNC-TD), 用于高效光催化合成H₂O₂. 研究表明, 引入噻二唑单元的CTF-TD能与g-C₃N₄形成能带匹配的S型异质结, 有效增强了光吸收、电荷分离和氧化还原能力. 优化后的CNC-TD-10在可见光照射下表现出最佳的光催化活性, H₂O₂生成速率为3259 μmol g⁻¹ h⁻¹, 分别是g-C₃N₄和CTF-TD的8倍和78倍, 且循环稳定性良好. X-射线光电子能谱和原位开尔文探针力显微镜分析证明了CTF-TD和g-C₃N₄结合的S型异质结有效地增强了光吸收、氧化还原能力以及载流子的分离和转移. 光电化学测试进一步证明了噻二唑功能化的CNC-TD-10更有利于电荷的转移, 抑制载流子的快速重组. 理论计算与实验结果共同证实, CNC-TD中噻二唑单元上的硫(S)位点促进了Yeager型(侧向)O₂吸附, 富集了活性位点, 并通过连续单电子ORR过程(两步单电子ORR)和单线态氧(¹O₂)途径协同促进H₂O₂的生成.

综上, 本研究通过以苯并噻二唑、苯基及联苯的氰基化合物为前驱体, 设计并合成了一系列具有分子内给体-受体结构的CTFs. 通过调控功能基团, 实现了对材料能带结构和局部微环境的精准优化. 将其与g-C₃N₄复合构建S型异质结后, CTF-TD组分特有的O₂吸附构型促进了两步单电子还原路径, 显著降低了O₂向H₂O₂转化的热力学能垒. 同时, 异质结界面与CTF-TD活性位点的协同作用, 有效促进了电荷分离并富集了反应位点, 从而大幅提升了H₂O₂的生成效率. 本工作为设计具有增强电子结构的有机异质结提供了有效策略, 推动了高效人工光合成H₂O₂的发展.

关键词: 共价三嗪框架, C₃N₄, S型异质结, 噻二唑活性位点, H₂O₂光合成

Abstract:

Photocatalytic hydrogen peroxide (H₂O₂) generation from water and air provides a prospective means for converting solar energy into valuable chemicals, which, however, is limited by the low carrier separation efficiency of traditional single-component semiconductor photocatalysts. Herein, we report a facile strategy for constructing an S-scheme organic heterojunction by integrating graphitic carbon nitride (g-C₃N₄) with covalent triazine frameworks (CTFs). The thiadiazole-modified CTFs are precisely functionalized with benzothiadiazole, phenyl, and biphenyl groups. The hybrid with optimized structure achieves a 3259 μmol g⁻¹ h⁻¹ H₂O₂ generation rate, outperforming pristine CTFs and g-C₃N₄ by 78-fold and 8-fold, respectively. In-situ characterizations confirm the enhanced light absorption, redox capacity, and charge carrier dynamics of the g-C₃N₄/CTF S-scheme heterojunction. The thiadiazole units increase active sites within CTFs and collaborate with g-C₃N₄ to accelerate electron-hole separation and enable high H₂O₂ selectivity. Through theoretical/experimental analyses, the O₂ adsorption configuration on CTFs is revealed to favor a two-step single-electron O₂ reduction route, reducing thermodynamic barriers for O₂-to-H₂O₂ conversion. Providing design strategies for organic heterojunctions with enhanced electronic structures, this study enables efficient artificial H₂O₂ photosynthesis.

Key words: C₃N₄, Covalent triazine frameworks, S-scheme heterojunction, Thiadiazole active sites, Photosynthesis of H₂O₂

刘高雄, 陈润东, 夏兵全, 周贤龙, 李来全, 刘善堂. 构建噻二唑功能化CTF基S型异质结用于高效光催化合成H₂O₂[J]. 催化学报, 2026, 87: 170-184.

Gaoxiong Liu, Rundong Chen, Bingquan Xia, Xianlong Zhou, Laiquan Li, Shantang Liu. Thiadiazole-functionalized covalent triazine frameworks for constructing S-scheme heterojunctions enabling boosted H₂O₂ photosynthesis[J]. Chinese Journal of Catalysis, 2026, 87: 170-184.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65079-6

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图/表 7

Fig. 1. Scheme depicting the H2O2 production via photo-redox reactions on the COF-based heterojunction photocatalyst.

Fig. 2. (a) Illustration of routes for synthesizing CN/CTF samples. (b) XRD patterns of CN/CTF composites. (c) FT‐IR spectra of CN, CTF and CNC-TD-X composites. TEM image (d) and magnified TEM image (e) of CNC-TD-10. HAADF-STEM image of CNC-TD-10 (f) and corresponding elemental distribution for C (g), N (h), and S (i).

Fig. 3. (a) UV-DRS spectra of CN, CTF-TD and the CNC-TD-10 composites. (b) Corresponding Tauc plots derived from the Kubelka-Munk function. Mott-Schottky plots of CN (c) and CTF-TD (d). (e) Proposed diagram illustrating the S-scheme band alignment between CN and CTF-TD. PL spectra (f) and TRPL spectra (g) for CN, CTF-TD and CNC-TD-10. Photocurrent responses (h) and EIS Nyquist plots (i) for CNC-TD-10, CNC-CB-10 and CNC-BP-10.

Fig. 4. XPS spectra and photocatalytic activities (a) S 2p spectra for CTF-TD and CNC-TD-10. C 1s (b) and N 1s (c) spectra for CNC-TD-10 and CN. Surface morphology and corresponding KPFM images of CN (d), CNC-TD-10 (e), and CTF-TD (f). Surface potential scanning curves of CN (g), CNC-TD-10 (h), and CTF-TD (i) under dark and illuminated conditions.

Fig. 5. (a) H2O2 production performance of CTF-based photocatalysts under varying gas atmospheres (λ ≥ 420 nm, 300 W Xe lamp, 100 mW cm−2; 10 mg catalyst, 25 mL ethanol aqueous solution (10 vol%)). (b) Performance comparison of different CTFs (CTF-TD, CTF-CB, and CTF-BP) and corresponding CN/CTF hybrids for photocatalytic H2O2 production. (c) H2O2 production performance over CN, CTF-TD, and CN/CTF-TD- hybrids under 60 min of simulated irradiation. (d) Recycle tests of CNC-TD-10 for H2O2 production.

Fig. 6. (a) EPR spectra of DMPO-•O2− signals for CN, CTF-TD, and CNC-TD-10 measured in MeOH under O2 saturation and light exposure. EPR spectra of TEMP-1O2 signals (b) and DMPO-•OH signals (c) for CN, CTF-TD, and CNC-TD-10 measured in aqueous suspension. In-situ DRIFTS spectra tracking intermediates during H2O2 photosynthesis over CNC-TD-10 (d), CNC-CB-10 (e), and CNC-BP-10 (f). (g) The energies of O2 adsorption at the S and N sites on the CTF backbone in both pristine CTF and the CTF segment within cyanide-modified conjugated triazine frameworks with thiadiazole units (CNC-TD) systems. DFT?calculated Gibbs free energy diagrams for the •O2− (h) and 1O2 (i) transformation pathways during the O2-to-H2O2 conversion over CNC-TD.

Fig. 7. (a) Proposed mechanism of S-scheme charge transfer in CN/CTF-TD (Ef denotes the Fermi level). (b) Schematic diagram of charge transfer and active sites in the S-scheme heterojunction. (c) Schematic illustration of the proposed mechanism for H2O2 synthesis via the ORR pathway on the S-scheme heterojunction.

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构建噻二唑功能化CTF基S型异质结用于高效光催化合成H₂O₂

Thiadiazole-functionalized covalent triazine frameworks for constructing S-scheme heterojunctions enabling boosted H₂O₂ photosynthesis

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