基于双氧还原中心的共价三嗪框架构建的1D/2D S型异质结促进过氧化氢光合作用

doi:10.1016/S1872-2067(24)60210-X

催化学报 ›› 2025, Vol. 69: 315-326.DOI: 10.1016/S1872-2067(24)60210-X

• 论文 • 上一篇

基于双氧还原中心的共价三嗪框架构建的1D/2D S型异质结促进过氧化氢光合作用

夏兵全^a, 刘高雄^a, 樊坤^a, 陈润东^a, 刘欣^c, 李来全^b^,^*()

^a武汉工程大学化学与环境工程学院, 湖北武汉 430074
^b上海理工大学能源材料科学研究院, 上海 200093
^c哈尔滨理工大学电子与电气工程学院, 黑龙江哈尔滨 150080

收稿日期:2024-11-08 接受日期:2024-12-12 出版日期:2025-02-18 发布日期:2025-02-10
通讯作者: *电子信箱: 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(22405173);湖北省自然科学基金(2023AFB181);武汉工程大学科学研究基金(23QD02)

Boosting hydrogen peroxide photosynthesis via a 1D/2D S-scheme heterojunction constructed by a covalent triazine framework with dual O₂ reduction centers

Bingquan Xia^a, Gaoxiong Liu^a, Kun Fan^a, Rundong Chen^a, Xin Liu^c, Laiquan Li^b^,^*()

^aKey Laboratory of Green Chemical Engineering Process of Ministry of Education, School of Chemistry and Environmental Engineering, Wuhan Institute of Technology, Wuhan 430074, Hubei, China
^bInstitute of Energy Materials Science, University of Shanghai for Science and Technology, Shanghai 200093, China
^cKey Laboratory of Engineering Dielectric and Applications (Ministry of Education), School of Electrical and Electronic Engineering, Harbin University of Science and Technology, Harbin 150080, Heilongjiang, China

Received:2024-11-08 Accepted:2024-12-12 Online:2025-02-18 Published:2025-02-10
Contact: *E-mail: lqli@usst.edu.cn (L. Li).
Supported by:
National Natural Science Foundation of China(22409151);National Natural Science Foundation of China(22405173);Natural Science Foundation of Hubei Province(2023AFB181);Science Foundation of Wuhan Institute of Technology(23QD02)

摘要/Abstract

摘要：

过氧化氢(H₂O₂)作为环保型氧化剂, 其国内年需求量约10万吨. 目前主要的生产方法蒽醌法要用昂贵的钯催化剂,同时会产生有毒的副产品, 因此利用太阳能开发一种可持续的H₂O₂生产方法迫在眉睫.具有芳香族三嗪结构的共价三嗪框架(CTFs)具有高电子亲和性和杂原子效应, 有着丰富的活性位点. 然而共价三嗪框架内部载流子快速重组和固有光捕获能力的不足, 使得其光催化性能受到阻碍. 目前常用策略是在结构中引入电子供体, 使其在分子水平上形成供体-受体结构, 通过强大的推拉式分子内电荷转移将载流子和空穴集中在相应的基团附近, 从而改善电荷分离和传输.

受此启发, 本文采用将无供体CTFs与ZnO结合的策略, 以ZnO作为电子供体构筑S型异质结, 利用异质结修饰策略来增加电子供体,充分发挥CTFs中的活性位点进行O₂还原的整体光合H₂O₂生产. 通过构建S型异质结, 解决了分离电荷容易重组的问题, 并改变了电荷转移机制, 提高了光催化效率, 最终促进H₂O₂的生成. 通过物理自组装方法将一维(1D) ZnO纳米棒和二维(2D) CTF组合构筑成了ZnO/CTF S型异质结构的光催化剂, 研究了其对生成H₂O₂的光催化性能. 在模拟可见光照射下, ZC-10的H₂O₂生成速率为12000 μmol g^‒1 h^‒1, 分别是ZnO纳米棒和CTF的10.3倍和164倍. 原位X-射线光电子能谱(XPS)结果表明, 在黑暗条件下ZC-10存在内置静电场, 在光照条件下, ZC-10中ZnO失去电子, 而CTF得到电子, 这与S型异质结的电荷转移机理一致. 原位开尔文探针力显微镜进一步证实了ZC-10在黑暗条件下内置静电场存在, 同时光照之后电荷转移与原位XPS测试结果一致, 再次证明了S型异质结形成. 电子顺磁共振和自由基淬灭实验表明, 超氧自由基是光催化合成过氧化氢的主要活性物种, 同时ZC-10的超氧自由基和羟基自由基的光催化产率明显超过ZnO和CTF, 表明该S型异质结有效地分离了光生电子-空穴对, 从而促进超氧自由基中间体的产生. 原位漫反射傅里叶变换红外光谱和旋转圆盘电极测试结果证实了ZC-10的光催化合成H₂O₂是两步单电子氧还原途径. 另外, 理论计算结果表明, 噻二唑和三嗪基的氮原子作为氧还原反应位点, 两个活性位点吉布斯自由能几乎相同, 可同时作为反应中心.

综上所述, 本文合成1D/2D S型异质结光催化剂, 实现了高效光催化合成过氧化氢, 为构建高效的S型异质结光催化剂提供了新的思路.

关键词: 共价三嗪框架, 光催化合成过氧化氢, S型异质结, 双氧还原中心

Abstract:

Emerging as lamellar materials, covalent triazine frameworks (CTFs) exhibited great potential for photocatalysis, but their photocatalytic performance is always hindered by the prone recombination of photogenerated carriers. To overcome this obstacle, a 1D/2D step-scheme (S-scheme) heterojunction is constructed for photocatalytic synthesis of H₂O₂. The S-scheme heterojunction fabricated with CTF and ZnO effectively enhances light absorption, redox capabilities, and charge carrier separation and transfer. In particular, the CTF is decorated with benzothiadiazole and triazine groups as dual O₂ reduction active centers, boosting photocatalytic H₂O₂ production. The optimal ZC-10 hybrid delivers a maximum H₂O₂ generation rate of 12000 μmol g⁻¹ h⁻¹, 10.3 and 164 times higher than those of zinc oxide nanorods and CTFs, respectively. Moreover, the charge transfer mechanism in the S-scheme heterojunction is well investigated with in situ spectroscopic measurements and theoretical calculations.

Key words: Covalent triazine frameworks, Photocatalytic H₂O₂ production, S-scheme heterojunction, Dual O₂ reduction centers

夏兵全, 刘高雄, 樊坤, 陈润东, 刘欣, 李来全. 基于双氧还原中心的共价三嗪框架构建的1D/2D S型异质结促进过氧化氢光合作用[J]. 催化学报, 2025, 69: 315-326.

Bingquan Xia, Gaoxiong Liu, Kun Fan, Rundong Chen, Xin Liu, Laiquan Li. Boosting hydrogen peroxide photosynthesis via a 1D/2D S-scheme heterojunction constructed by a covalent triazine framework with dual O₂ reduction centers[J]. Chinese Journal of Catalysis, 2025, 69: 315-326.

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图/表 7

Fig. 1. Synthetic process, XRD spectra, and FT-IR spectra. (a) Synthetic procedure of ZnO/CTF samples. XRD patterns (b) and FT-IR spectra (c) of ZnO, CTF, and ZC composites.

Fig. 2. TEM images of the prepared photocatalysts: ZnO nanorods (a), CTF (b) and ZC-10 (c). High-resolution TEM (d), HAADF image (e) and elemental mappings of Zn (f), O (g), C (h), N (i), and S (j) elements in ZC-10.

Fig. 3. Photoelectrochemical characterizations. (a) UV-vis DRS spectra for ZC hybrids, CTF and ZnO; Mott-Schottky plots for ZnO (b) and CTF (c). (d) Proposed energy diagrams for ZnO and CTF.

Fig. 4. XPS spectra and photocatalytic activities. Zn 2p (a) and O 1s (b) spectra for ZnO and ZC-10. N 1s (c) and S 2p (d) spectra for CTF and ZC-10. (e) Performance tests of as-prepared samples for photocatalytic H2O2 production. (f) Comparison of the H2O2 production capability of ZnO, CTF and ZC-X under simulated irradiation for 1 h.

Fig. 5. Side view of the optimized CTF/ZnO: Side view (a) and top view (b) of the charge density difference of CTF/ZnO with an isosurface of 4.2 × 10?3 e ??3. (The charge accumulation is shown as the yellow region, and the charge depletion is shown as the cyan region). (c,d) Under dark and illuminated conditions, the KPFM images of ZC-10. (e,f) Under dark and illuminated conditions, the surface potential scanning curves of ZC-10. PL spectra (g), TRPL spectra (h), and EIS spectra (i) of the samples.

Fig. 6. EPR was utilized to test for ?O2?, ?OH, and 1O2, DRIFTS spectrum, DFT-calculated data, and a schematic diagram of the photocatalytic process. (a) EPR signals of DMPO-?O2? on ZnO, CTF, and ZC-10 in O2-saturated methanol. (b) EPR trapping experiments of TEMP-1O2 in H2O dispersions of ZC-10. (c) EPR signals of DMPO-?OH on ZnO, CTF, and ZC-10 in water. (d) DRIFTs spectrum of ZC-10 in H2O2 photosynthesis. (e) ?O2? and 1O2 conversion pathways for the O2 reduction to H2O2 on the Triazine site and benzothiadiazole site with DFT-calculated Gibbs free energy. (f) Schematic illustration of the photocatalytic production of H2O2 through the ORR pathways.

Fig. 7. Schematic illustration of S-scheme charges transfer mechanism between ZnO and CTF. Ev and Ef respectively stand for vacuum energy level and fermi energy level.

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基于双氧还原中心的共价三嗪框架构建的1D/2D S型异质结促进过氧化氢光合作用

Boosting hydrogen peroxide photosynthesis via a 1D/2D S-scheme heterojunction constructed by a covalent triazine framework with dual O₂ reduction centers

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基于双氧还原中心的共价三嗪框架构建的1D/2D S型异质结促进过氧化氢光合作用

Boosting hydrogen peroxide photosynthesis via a 1D/2D S-scheme heterojunction constructed by a covalent triazine framework with dual O2 reduction centers

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Boosting hydrogen peroxide photosynthesis via a 1D/2D S-scheme heterojunction constructed by a covalent triazine framework with dual O₂ reduction centers