基于共价有机框架非金属位点的光催化CO2还原

doi:10.1016/S1872-2067(24)60027-6

催化学报 ›› 2024, Vol. 60: 201-208.DOI: 10.1016/S1872-2067(24)60027-6

基于共价有机框架非金属位点的光催化CO₂还原

黄浩铭^a, 林清清^a, 牛青^a, 宁江淇^a, 李留义^a^,^*(), 毕进红^b^,^*(), 于岩^a^,^*()

^a福州大学材料科学与工程学院, 生态材料先进技术重点实验室, 福建福州 350108
^b福州大学环境与安全工程学院, 福建福州 350108

收稿日期:2024-02-06 接受日期:2024-03-28 出版日期:2024-05-18 发布日期:2024-05-22
通讯作者: *电子信箱: lyli@fzu.edu.cn (李留义), bijinhong@fzu.edu.cn (毕进红), yuyan@fzu.edu.cn (于岩).
基金资助:
国家重点研发计划(2020YFA0710303);国家自然科学基金(52172188);国家自然科学基金(22272028);国家自然科学基金(52072076)

Metal-free photocatalytic reduction of CO₂ on a covalent organic framework-based heterostructure

Haoming Huang^a, Qingqing Lin^a, Qing Niu^a, Jiangqi Ning^a, Liuyi Li^a^,^*(), Jinhong Bi^b^,^*(), Yan Yu^a^,^*()

^aKey Laboratory of Eco-materials Advanced Technology, College of Materials Science and Engineering, Fuzhou University, Fuzhou 350108, Fujian, China
^bDepartment of Environmental Science and Engineering, Fuzhou University, Fuzhou 350108, Fujian, China

Received:2024-02-06 Accepted:2024-03-28 Online:2024-05-18 Published:2024-05-22
Contact: *E-mail: lyli@fzu.edu.cn (L. Li), bijinhong@fzu.edu.cn (J. Bi), yuyan@fzu.edu.cn (Y. Yu).
Supported by:
National Key Research and Development Program of China(2020YFA0710303);National Natural Science Foundation of China(52172188);National Natural Science Foundation of China(22272028);National Natural Science Foundation of China(52072076)

摘要/Abstract

摘要：

光催化CO₂还原制备碳基化学品, 是解决能源危机的理想途径之一. 以往的研究主要聚焦于金属位点催化, 尽管金属催化剂具有显著的应用潜力, 但其高昂的成本和金属中心易失活的问题, 限制了其广泛应用. 因此, 模拟植物光合作用, 探寻基于非金属位点的光催化剂, 为CO₂还原提供了新的解决思路. 共价有机框架材料(COFs)作为一种新型有机晶态多孔材料, 因其高度有序的结构和π共轭体系, 通常表现出半导体特性. 在COF中引入氮官能团, 能有效增强对CO₂的吸附和活化能力, 有望在COFs上实现非金属光催化CO₂还原.

本文利用COF异质结材料研究了非金属位点催化CO₂还原过程. 采用原位合成方法制备出ZnIn₂S₄@TAz-COF异质结材料. 红外光谱、Raman光谱和X-射线衍射等方法证明了异质结材料的成功合成. 扫描电镜和透射电镜观察显示, ZnIn₂S₄纳米片与COF形成了异质互融界面, 这对后续研究电子转移路径和光催化增强机制至关重要. 通过紫外-可见光漫反射光谱、紫外光电子能谱和Mott-Schottky表征, 分析了复合前后样品在能带结构上发生的变化和单独组分的功函数. 由此推断, 当两者复合后, 在费米能级差的驱动下, TAz-COF表面的电子流向ZnIn₂S₄, 在界面处形成内建电场, 这与差分电荷计算结果相一致. 进一步的原位光照X射线光电子能谱研究证实, ZnIn₂S₄@TAz-COF异质结两相之间存在电荷转移, 在界面处形成由TAz-COF指向ZnIn₂S₄的内建电场. 这驱动了ZnIn₂S₄导带上的光生电子与TAz-COF价带上的光生空穴定向迁移和复合, 而TAz-COF导带上还原能力较强的光生电子和ZnIn₂S₄价带上氧化能力较强的光生空穴被空间分离并参与光催化反应. 在以水为电子供体的光催化还原CO₂反应中, 该异质结材料表现出较好的还原CO₂到CO活性和良好的稳定性, 其转化效率可与部分金属催化的CO₂还原体系相当. 密度泛函理论计算和原位光谱分析结果表明, 吖嗪基团是CO₂分子的吸附和活化位点, 吖嗪中的氮原子与CO₂中的碳原子的强相互作用确保了CO₂向COOH*中间体的转化, 最终通过光生电子和质子的协助在COF表面转化为CO.

综上所述, 本文制备了ZnIn₂S₄@TAz-COF异质结光催化材料. 在可见光照射下, 该材料界面处形成的内建电场有效驱动了光生电子和空穴的定向迁移, 使得COF导带上具有较强还原能力的光生电子与ZnIn₂S₄价带上具有较强氧化能力的光生空穴实现了高效的空间分离. 在没有金属助催化剂和空穴牺牲剂的条件下, ZnIn₂S₄@TAz-COF复合光催化剂表现出较好的光催化CO₂还原活性. 本工作不仅为深入理解非金属位点催化CO₂还原机理提供了新视角, 也为设计和构建高效CO₂还原光催化材料提供了参考.

关键词: 共价有机框架, 光催化, 二氧化碳还原, 异质结构, 非金属位点

Abstract:

Photocatalytic reduction of CO₂ with H₂O is thought as an environment friendly approach for sustainable development. It is highly desirable but remains challenging to develop photocatalyst with metal-free site for CO₂ reduction. Here, we fabricated a heterostructure by integrating azine-based COF with ZnIn₂S₄, where the azine unit in COF acts as metal-free sites for CO₂ adsorption and reduction. The as-formed interfused heterointerface in the heterostructure ensures the effective electron transfer from ZnIn₂S₄ across the interface to the COF, resulting in a spatial separation of redox sites for CO₂ reduction and water oxidation. The hybrid catalyst exhibits remarkably enhanced photocatalytic activity for CO₂ reduction to CO, which is 8 and 6 times than the COF and ZnIn₂S₄, respectively, and is even comparable with some metal-catalyzed CO₂ reduction systems. This study provides a new paradigm to mimic natural photosynthesis by using metal-free site for CO₂ reduction.

Key words: Covalent organic framework, Photocatalysis, CO₂ reduction, Heterostructure, Metal-free site

黄浩铭, 林清清, 牛青, 宁江淇, 李留义, 毕进红, 于岩. 基于共价有机框架非金属位点的光催化CO₂还原[J]. 催化学报, 2024, 60: 201-208.

Haoming Huang, Qingqing Lin, Qing Niu, Jiangqi Ning, Liuyi Li, Jinhong Bi, Yan Yu. Metal-free photocatalytic reduction of CO₂ on a covalent organic framework-based heterostructure[J]. Chinese Journal of Catalysis, 2024, 60: 201-208.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60027-6

https://www.cjcatal.com/CN/Y2024/V60/I5/201

图/表 6

Fig. 1. Schematic illustration of COF-based heterostructure for photocatalytic CO2 reduction with H2O.

Fig. 2. (a) Schematic synthesis of ZnIn2S4@TAz-COF. SEM (b), TEM (c), HRTEM (d) and EDX mapping (e) images of ZnIn2S4@TAz-COF. (f) PXRD patterns of ZnIn2S4@TAz-COF, ZnIn2S4 and TAz-COF.

Fig. 3. (a) UV-vis DRS spectra. (b) Schematic diagram of the band structure alignment for ZnIn2S4 and TAz-COF. Photocurrent response (c), EIS (d), steady-state solid PL (e), and time-resolved PL (f) spectra for TAz-COF, ZnIn2S4, and ZnIn2S4@TAz-COF.

Fig. 4. (a) XPS spectra for N 1s in TAz-COF and ZnIn2S4@TAz-COF under darkness and in light. (b) XPS spectra for Zn 2p in ZnIn2S4 and the ZnIn2S4@TAz-COF under darkness and in light. (c) EPR of TAz-COF, ZnIn2S4, and ZnIn2S4@TAz-COF under light irradiation. (d) Top and side views of the averaged charge density difference for ZnIn2S4@TAz-COF. Red and green regions represent electron accumulation and depletion, respectively. C (dark gray), N (blue), H (light gray), Zn (pink), In (violet) and S (yellow).

Fig. 5. (a) Photocatalytic CO2 conversion rates of TAz-COF, ZnIn2S4 and ZnIn2S4@TAz-COF with different mass ratios (x = 5, 10, 15, 20, 30). (b) Evolution rates of CO, CH4 and O2 over ZnIn2S4@TAz-COF. (c) GC-MS spectra of 13CO and 18O2 by using ZnIn2S4@TAz-COF as photocatalyst with 13CO2 and H218O. (d) Stability test of ZnIn2S4@TAz-COF in four repeats with each run lasting 4 h.

Fig. 6. (a) In-situ FTIR experiment over ZnIn2S4@TAz-COF under light irradiation. (b) CO2 binding energy on triazine and azine units. (c) Gibbs free energy diagrams of photocatalytic reduction of CO2 on azine units of TAz-COF and ZnIn2S4@TAz-COF. Where the asterisk (*) indicated the adsorption state on the photocatalyst surface. (d) Proposed mechanism of photocatalytic reduction of CO2 by ZnIn2S4@TAz-COF.

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基于共价有机框架非金属位点的光催化CO₂还原

Metal-free photocatalytic reduction of CO₂ on a covalent organic framework-based heterostructure

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