通过碳点从共价三嗪框架中提取光生空穴用于光合作用产过氧化氢

doi:10.1016/S1872-2067(24)60050-1

催化学报 ›› 2024, Vol. 62: 178-189.DOI: 10.1016/S1872-2067(24)60050-1

通过碳点从共价三嗪框架中提取光生空穴用于光合作用产过氧化氢

任卫杰^a^,¹, 李宁^a^,¹, 常青^a, 武杰^b, 杨金龙^a^,^c, 胡胜亮^a^,^*(), 康振辉^d^,^*()

^a中北大学, 煤与煤层气共采全国重点实验室, 山西太原 030051
^b煤与煤层气共采全国重点实验室, 山西晋城 048012
^c清华大学, 新型陶瓷与精细加工国家重点实验室, 北京 100084
^d苏州大学, 功能纳米与软材料研究所, 江苏苏州 215123

收稿日期:2024-02-26 接受日期:2024-05-10 出版日期:2024-07-18 发布日期:2024-07-10
通讯作者: *电子邮箱: hsliang@yeah.net (胡胜亮), zhkang@suda.edu.cn (康振辉).
作者简介:¹共同第一作者.
基金资助:
山西省科技创新团队专项资金(202304051001014);山西省基础研究计划项目(20210302123037);山西省基础研究计划项目(202303021222175);山西省留学基金委科研项目(2022-136);山西省高校科技创新计划项目(2023L176);国家自然科学基金项目(22105181)

Abstracting photogenerated holes from covalent triazine frameworks through carbon dots for overall hydrogen peroxide photosynthesis

Weijie Ren^a^,¹, Ning Li^a^,¹, Qing Chang^a, Jie Wu^b, Jinlong Yang^a^,^c, Shengliang Hu^a^,^*(), Zhenhui Kang^d^,^*()

^aResearch Group of New Energy Materials and Devices, State Key Laboratory of Coal and CBM Co-Mining, North University of China, Taiyuan 030051, Shanxi, China
^bState Key Laboratory of Coal and CBM Co-Mining, Jincheng 048012, Shanxi, China
^cState Key Laboratory of New Ceramics and Fine Processing, Tsinghua University, Beijing 100084, China
^dInstitute of Functional Nano and Soft Materials Laboratory (FUNSOM), Soochow University, Suzhou 215123, Jiangsu, China

Received:2024-02-26 Accepted:2024-05-10 Online:2024-07-18 Published:2024-07-10
Contact: *E-mail: hsliang@yeah.net (S. Hu), zhkang@suda.edu.cn (Z. Kang).
About author:First author contact:
¹ Contributed equally to this work.
Supported by:
special fund for Science and Technology Innovation Teams of Shanxi Province(202304051001014);Fundamental Research Program of Shanxi Province of China(20210302123037);Fundamental Research Program of Shanxi Province of China(202303021222175);Shanxi Scholarship Council of China(2022-136);Science and technology innovation plan of colleges and universities in Shanxi Province(2023L176);National Natural Science Foundation of China(22105181)

摘要/Abstract

摘要：

过氧化氢(H₂O₂)是一种多功能氧化剂, 利用地球上丰富的水和氧合成过氧化氢是解决能源危机和环境修复的一种有前景的方法. 共价三嗪框架(CTFs)因具有独特的稳定结构以及π共轭sp²碳结构上功能基团的高可设计性, 其作为光催化剂而备受关注. 然而, 由于共轭键的可逆性较差, 极大地影响了电荷的分离和转移. 为了提高载流子分离效率, 目前的策略主要为开发高结晶结构或在CTFs骨架中加入具有不同电离势和电子亲和力的供电子和接受电子单元, 但催化性能和太阳能化学转化(SCC)效率仍然低于预期. 碳点(CDs)具有类分子特性, 可以通过表面接触或结合改变材料的微观结构和物理性能, 起到调控光生电荷行为的作用. 因而, 本文把CDs引入到CTFs分子中, 使其充当电荷分离器, 提升光生载流子的利用效率.

本文提出一种可扩展的方法, 使1,4-二氰苯(DCB)、CDs和碱金属盐在溶液中发生选择性吸附反应, 去除溶剂后制备出预混物, 然后再以CF₃SO₃H为催化剂, 在空气氛围内直接加热预混物至250 °C并反应8 h, 获得具有高结晶CTFs与CDs的复合光催化剂(CDs@CTFs). 透射电镜、X射线光电子能谱(XPS)等结果证明了CDs引入到CTFs插层中. 粉末X射线衍射结果表明, 适量的CDs可以提高CTFs的结晶度. 紫外-可见吸收谱表明CDs的引入扩大了可见光的吸收范围. Zeta电位、光致发光光谱等结果表明, 二价和多价阳离子同时与两个或两个以上的CDs相互作用, 导致其溶胶溶液的不稳定性和表面电子态的改变, 影响了光催化剂性能. XPS、红外光谱、热重分析(TGA)等表征结果表明CDs表面羧基的H⁺离子可能被碱金属离子取代, 从而调节表面电荷分布, 促进电荷分离和转移. 电荷牺牲实验、原位漫反射红外傅立叶变换光谱和电子顺磁共振谱测试结果表明, CDs@CTFs可以实现氧还原反应和水氧化反应双通道产H₂O₂. 通过使用已知的电子受体和电子供体来识别CDs和CTFs之间的电荷转移过程, 并结合对空穴传输层器件的暗I-V曲线测试结果, 揭示了CDs具有空穴存储功能. 所制光催化剂的H₂O₂产率为2464 μmol h^‒1 g^‒1, 全光谱光化学转化效率为0.9%, 500 nm的表观量子产率为13%, 超过了目前报道的大多数光催化剂. 结合理论分析结果表明, CDs可以作为空穴提取剂有效地驱动激子解离, 并为水氧化反应提供活性位点; 研究发现碱金属离子在合成过程中与CDs表面的羧酸基团相互作用, 增强对CTFs的空穴提取能力, 加速光催化生成H₂O₂. 此外, 所制光催化剂在自然阳光下可连续工作产H₂O₂, 且光催化性能经过100 d循环使用仍表现出高的稳定性.

综上所述, 本文开发了一种简便且可扩展的方法, 将CDs引入到CTFs中, 以实现高效的光催化产H₂O₂. CDs通过其界面产生的内电场从CTFs中提取光生空穴, 并在CTFs上充当空穴存储层. 此外, 碱金属离子能显著调节内部电场强度, 使CDs@CTFs具有更显著的光催化性能. 本工作揭示了一种新的设计策略来调控有机共轭聚合物中的载流子分离和迁移.

关键词: 共价三嗪框架, 碳点, 过氧化氢光合作用, 光催化过程, 水氧化反应, 光催化剂

Abstract:

Owing to the rapid recombination of photogenerated electron-hole pairs with strong Coulomb interactions, the photocatalytic activity of metal-free conjugated polymers is often unsatisfactory. This article reports a simple method for incorporating carbon dots (CDs) into highly crystalline covalent triazine frameworks (CTFs) by directly heating a pretreated mixture of 1,4-dicyanobenzene, CDs, and alkali metal salts in air. The resultant photocatalyst exhibits a H₂O₂ production rate, solar-to-chemical conversion efficiency, and apparent quantum yield of 2464 μmol h^-1 g^-1, 0.9% at full spectrum, and 13% at 500 nm, respectively, surpassing most reported photocatalysts. The results of this study reveal that CDs can serve as hole extractors to efficiently drive exciton dissociation and can offer active sites for water oxidation reactions. This study is also the first to observe that alkali metal ions can interact with the carboxylic acid groups on the surface of CDs during synthesis to enhance the hole-extraction ability of CTFs, thereby accelerating photocatalytic H₂O₂ production. This study provides insights into the rational design of highly efficient CDs-based photocatalysts.

Key words: Covalent triazine framework, Carbon dot, H₂O₂ photosynthesis, Photocatalytic process, Water oxidation reaction, Photocatalyst

任卫杰, 李宁, 常青, 武杰, 杨金龙, 胡胜亮, 康振辉. 通过碳点从共价三嗪框架中提取光生空穴用于光合作用产过氧化氢[J]. 催化学报, 2024, 62: 178-189.

Weijie Ren, Ning Li, Qing Chang, Jie Wu, Jinlong Yang, Shengliang Hu, Zhenhui Kang. Abstracting photogenerated holes from covalent triazine frameworks through carbon dots for overall hydrogen peroxide photosynthesis[J]. Chinese Journal of Catalysis, 2024, 62: 178-189.

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图/表 8

Fig. 1. Photocatalytic H2O2 production performance. (a,b) Time courses of H2O2 generation over CTFs and CDs@CTFs in different reaction solutions under simulated sunlight irradiation. (c) Comparison of the photocatalytic performances of CTFs and CDs@CTFs before and after introducing 0.1 μmol CsCl. (d) EPR spectra of CDs@CTFs and CDs@CTFs CsCl irradiated for 10 min for O2?? detection. (e) EPR spectra of CDs@CTFs and CDs@CTFs CsCl irradiated for 10 min for ·OH detection. (f) DRIFTS spectra of CDs@CTFs irradiated for various durations.

Fig. 2. Photocatalytic H2O2 production performance. (a) AQY of H2O2 generation over CDs@CTFs CsCl as a function of the incident light wavelength at different wavelengths. (b) Comparison of the H2O2 production performance of the proposed photocatalysts against previously reported photocatalysts. (c) Stability and durability of CDs@CTFs CsCl for H2O2 generation. (d) H2O2 evolution of CDs@CTFs CsCl during 10 h of outdoor sunlight irradiation with careful monitoring of the environmental temperature and solar intensity.

Fig. 3. Characterization of the CTFs and CDs@CTFs. (a) FTIR spectra of the CDs@CTFs, CTFs, and DCB. (b) Powder XRD patterns of the CTFs and CDs@CTFs. (c) HRTEM images and EDS maps of CDs@CTFs CsCl. (d) XPS C 1s spectra of the CTFs and CDs@CTFs. (e) Comparison of the photocatalytic activity of the CTFs against that of the calcined CTFs and CTFs/CDs. (f) UV-vis absorption of the CTFs, CDs@CTFs, and CDs@CTFs CsCl.

Fig. 4. Effect of metal ions on the CDs@CTFs. (a) Zeta potentials of CD solutions containing equal concentrations of different metal ions. (b) PL spectra of CD solutions before and after the addition of different metal ions. (c) Comparison of the photocatalytic activities of CDs@CTFs before and after the addition of different metal ions. (d) Comparison of the photocatalytic performance of CDs@CTFs containing different CsCl contents. (e) Zeta potentials of CD solutions containing different CsCl contents. (f) XRD spectra of CDs@CTFs containing different CsCl contents.

Fig. 5. Interaction of alkali metal ions with CDs. (a) Schematic illustration of the combination of CDs with alkali metal ions. (b) XPS Cs 3d spectra of CsCl and CDs@CTFs CsCl. (c) FTIR spectra of the CDs before and after the addition of CsCl. (d) TGA results of the CTFs, CDs@CTFs, and CDs@CTFs CsCl. (e) FTIR spectra of the CDs@CTFs with and without CsCl. (f) Photocatalytic performance of the CDs@CTFs in different alkali metal ion solutions. (g) Photocatalytic H2O2 production performance of NCDs@CTFs with different CsCl contents.

Fig. 6. Charge separation and transfer analysis. (a) Energy level structures of the CDs and CTFs. (b) PL spectra of the CTFs, CDs@CTFs, and CDs@CTFs CsCl. (c) Transient fluorescence spectroscopy (TFS) spectra of the CTFs, CDs@CTFs, and CDs@CTFs CsCl. (d) Electrochemical impedance spectroscopy (EIS) plots of the CTFs, CDs@CTFs, and CDs@CTFs CsCl. (e) Transient photocurrent response of the CTFs, CDs@CTFs, and CDs@CTFs CsCl.

Fig. 7. Role of CDs in charge transfer. (a,b) PL spectra of the CDs and CDs+CsCl before and after the addition of 2,4-dinitrotoluene and N,N-diethylaniline. (c,d) TFS spectra of the CDs and CDs+CsCl before and after the addition of 2,4-dinitrotoluene and N,N-diethylaniline. (e,f) Schematic illustration of the device structure used and the collected I-V curves of the CTFs and CDs@CTFs in darkness.

Fig. 8. Photogenerated charge separation and transfer mechanism. (a) Schematic diagram illustrating the carrier separation and transfer processes in the CTFs, CDs@CTFs, and CDs@CTFs CsCl. (b,c) Calculated mean charge density distributions of the CDs and CTFs in the z-direction before and after the introduction of Cs+ ions.

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通过碳点从共价三嗪框架中提取光生空穴用于光合作用产过氧化氢

Abstracting photogenerated holes from covalent triazine frameworks through carbon dots for overall hydrogen peroxide photosynthesis

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