高共轭和化学稳定的三维共价有机框架材料用于高效光催化CO2还原

doi:10.1016/S1872-2067(25)64717-6

催化学报 ›› 2025, Vol. 74: 144-154.DOI: 10.1016/S1872-2067(25)64717-6

高共轭和化学稳定的三维共价有机框架材料用于高效光催化CO₂还原

张琳^a^,¹, 张慧^a^,¹, 方敬红^b, 崔嘉琳^a, 刘洁^c, 刘辉^a^,^*(), 孙立水^a, 孙琼^b^,^*(), 董立峰^b^,^*(), 赵英杰^a^,^*()

^a青岛科技大学高性能聚合物及成型技术教育部工程研究中心, 山东青岛 266042
^b青岛科技大学材料科学与工程学院, 山东青岛 266042
^c北京高压科学研究中心, 北京 100193

收稿日期:2024-12-25 接受日期:2025-03-14 出版日期:2025-07-18 发布日期:2025-07-20
通讯作者: *电子信箱: hliu@qust.edu.cn (刘辉),sunqiong@qust.edu.cn (孙琼),donglifeng@qust.edu.cn (董立峰),yz@qust.edu.cn (赵英杰).
作者简介:¹共同第一作者.
基金资助:
国家自然科学基金(22205128);国家自然科学基金(22175101);山东省自然科学基金(ZR2022QB054)

Highly conjugated and chemically stable three-dimensional covalent organic frameworks for efficient photocatalytic CO₂ reduction

Lin Zhang^a^,¹, Hui Zhang^a^,¹, Jinghong Fang^b, Jialin Cui^a, Jie Liu^c, Hui Liu^a^,^*(), Lishui Sun^a, Qiong Sun^b^,^*(), Lifeng Dong^b^,^*(), Yingjie Zhao^a^,^*()

^aEngineering Research Center of High-Performance Polymer and Molding Technology, Ministry of Education, Qingdao University of Science and Technology, Qingdao 266042, Shandong, China
^bCollege of Materials Science and Engineering, Qingdao University of Science and Technology, Qingdao 266042, Shandong, China
^cCenter for High-Pressure Science and Technology Advanced Research, Beijing 100193, China

Received:2024-12-25 Accepted:2025-03-14 Online:2025-07-18 Published:2025-07-20
Contact: *E-mail: hliu@qust.edu.cn (H. Liu), sunqiong@qust.edu.cn (Q. Sun), *donglifeng@qust.edu.cn (L. Dong), yz@qust.edu.cn (Y. Zhao).
About author:¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22205128);National Natural Science Foundation of China(22175101);Shandong Provincial Natural Science Foundation(ZR2022QB054)

摘要/Abstract

摘要：

共价有机框架(COFs)是一类具有高度有序结构的多孔有机材料, 其在光催化领域展现出广阔的应用前景. 近年来, COFs作为高效光催化剂, 可通过可见光驱动CO₂还原, 将CO₂转化为高附加值燃料, 如CO、CH₄和甲醇等, 从而有效减少温室气体排放, 缓解全球气候变暖问题. 然而, 当前CO₂光催化转化技术仍面临诸多挑战, 特别是在无贵金属催化剂或牺牲剂辅助的情况下, 实现高效、选择性的CO₂还原仍然困难. 传统的光催化体系往往依赖贵金属或牺牲剂提供电子, 虽然提高了催化效率, 但成本较高, 且不具备可持续性. 因此, 开发绿色、高效的无金属、无牺牲剂光催化体系, 探索新型COFs结构以增强光吸收能力、促进光生载流子分离, 并提高CO₂还原的催化活性和选择性, 已成为当前研究的重要方向. 该研究不仅有助于推动光催化CO₂还原技术的发展, 同时也为未来实现清洁能源转换提供了可行的解决方案.

本文通过结合两个具有良好光活性的刚性和共轭的正交构筑单元(螺芴和联咔唑), 构建了具有亚胺键连接的高共轭三维 COF, 即3D-COF-1. 通过简单的后合成还原, 获得了化学稳定的仲胺键连接的3D-COF-2, 其保持了优异的结晶性和孔隙率. 值得注意的是, 3D-COF-2由于其高度共轭的结构以及丰富的仲胺基团作为化学吸附位点, 可以更加高效地捕获CO₂. 且在后续的光催化CO₂还原反应中, 3D-COF-2表现出更加优异的性能, 其CO产率在4.5 h内达到了1070 μmol∙g^-1, 是3D-COF-1 (463 μmol∙g^-1)的两倍以上, 且CO选择性接近100%. 而且经过五次循环测试后, 3D-COF-2在光催化性能上保持了优异的稳定性. 此外, 通过瞬态吸收光谱、原位红外的表征以及密度泛函理论计算对3D-COF-1和3D-COF-2的作用机理进行了更深入的研究. 与3D-COF-1相比, 3D-COF-2具有更宽的可见光吸收范围、更高的电子-空穴分离效率、更灵敏的光响应能力、更快速的电子转移能力以及更优化的导带和价带位置及光学带隙. 上述特性显著提升了光生载流子的利用效率, 并有效抑制电子-空穴复合.

综上, 3D COFs由于其独特的结构在光催化领域具有潜在的应用价值, 尤其是在光催化还原CO₂方面展现出了良好的催化活性和稳定性. 本研究不仅拓展了3D COFs在光催化领域的应用范围, 也为后续相关材料的优化设计和性能提升提供了重要的指导意义, 为未来开发高效、环保的无金属光催化CO₂还原材料提供了有价值的理论依据和实验参考.

关键词: 共价有机框架, 三维结构, 光催化CO₂还原, 无金属催化, 化学稳定结构

Abstract:

Covalent organic frameworks (COFs), as efficient photocatalysts, can convert CO₂ and H₂O into value-added fuel, thus improving the deteriorating ecological environment. However, achieving high photocatalytic efficiency and selectivity without relying on noble metals or sacrificial agents remains a significant challenge. Here, a highly conjugated three-dimensional (3D) COF 3D-COF-1 with imine linkage is constructed by the combination of two rigid and conjugated orthogonal building blocks (spirobifluorene and bicarbazole) with good photoactivites. Through a simple post-synthetic reduction, a chemically stable and amine-linked 3D-COF-2 which maintains excellent crystallinity and porosity can be obtained. Notably, the 3D-COF-2 exhibits excellent performance in CO₂ reduction and exceptional selectivity of CO due to the highly conjugated structure and abundant amine groups as chemisorption sites for selectively capturing CO₂. Under the irradiation of visible light and without noble metals and sacrificial agents, 3D-COF-2 produces 1070 μmol g^-1 of carbon monoxide in 4.5 h, and the selectivity is close to 100%.

Key words: Covalent organic frameworks, Three-dimensional structure, Photocatalytic CO₂ reduction, Metal-free catalysis, Chemically stable structure

张琳, 张慧, 方敬红, 崔嘉琳, 刘洁, 刘辉, 孙立水, 孙琼, 董立峰, 赵英杰. 高共轭和化学稳定的三维共价有机框架材料用于高效光催化CO₂还原[J]. 催化学报, 2025, 74: 144-154.

Lin Zhang, Hui Zhang, Jinghong Fang, Jialin Cui, Jie Liu, Hui Liu, Lishui Sun, Qiong Sun, Lifeng Dong, Yingjie Zhao. Highly conjugated and chemically stable three-dimensional covalent organic frameworks for efficient photocatalytic CO₂ reduction[J]. Chinese Journal of Catalysis, 2025, 74: 144-154.

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图/表 6

Fig. 1. (a) The synthesis of 3D-COF-1 and 3D-COF-2. (b) FT-IR spectra of 3D-COF-1, 3D-COF-2, compound A, and compound B and the enlarged portion within the green dashed box of the left image.

Fig. 2. Simulated and experimental powder X-ray diffraction patterns and difference curves of 3D-COF-1 (a) and 3D-COF-2 (b). N2 adsorption?desorption isotherms and pore size distribution profiles of 3D-COF-1 (c) and 3D-COF-2 (d).

Fig. 3. SEM (a, b) and TEM (c,d) images of 3D-COF-1. SEM (e,f) and TEM (g,h) images of 3D-COF-2.

Fig. 4. (a) CO2 adsorption-desorption isotherms at 25 and 0 °C of 3D-COF-1 and 3D-COF-2. (b) Photocatalytic CO yields of 3D-COF-1 and 3D-COF-2. (c) Recycling stability tests of 3D-COF-2.

Fig. 5. (a) Solid-state UV/vis absorption spectra of 3D-COF-1 and 3D-COF-2. (b) Band gaps of 3D-COF-1 and 3D-COF-2. (c) Mott-Schottky plot of 3D-COF-1. (d) Mott-Schottky plot of 3D-COF-2. (e) The band structure diagram of 3D-COF-1 and 3D-COF-2. (f) Transient photocurrent response of 3D-COF-1 and 3D-COF-2. (g) Electrochemical impedance spectroscopy of 3D-COF-1 and 3D-COF-2. (h) EPR spectra of 3D-COF-1 in the dark and under the light. (i) EPR spectra of 3D-COF-2 in the dark and under the light.

Fig. 6. (a) In situ DRIFTS of 3D-COF-2 in the dark (background) and under visible light irradiation for different durations. (b) In situ DRIFTS of 3D-COF-2 for *CO adsorption. (c) In situ DRIFTS of 3D-COF-2 for CO2 adsorption. (d) The possible reaction mechanism for photocatalytic CO2-to-CO reduction on the 3D-COF-2-based metal-free catalyst, along with the corresponding Gibbs free energy change (ΔG) values for each step. (e) Gibbs free energy plots for 3D-COF-2 in the process of CO2 reduction. Calculated ESP on the van der Waals surface of 3D-COF-1 (f) and 3D-COF-2 (g), with blue indicating more negative ESPs and red indicating more positive ESPs. The simulated structures and adsorption energies of CO2 adsorbed in 3D-COF-1 (h) and 3D-COF-2 (i).

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高共轭和化学稳定的三维共价有机框架材料用于高效光催化CO₂还原

Highly conjugated and chemically stable three-dimensional covalent organic frameworks for efficient photocatalytic CO₂ reduction

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