嵌入铂单原子的苯并咪唑基共价有机框架实现高效可见光析氢

doi:10.1016/S1872-2067(23)64422-5

催化学报 ›› 2023, Vol. 48: 137-149.DOI: 10.1016/S1872-2067(23)64422-5

嵌入铂单原子的苯并咪唑基共价有机框架实现高效可见光析氢

马方沛^a, 汤庆平^a, 席识博^b, 李国庆^a, 陈涛^a, 凌星辰^a, 吕忆农^c, 刘云鹏^d, 赵小龙^a, 周瑜^a^,^*(), 王军^a^,^*()

^a南京工业大学化工学院, 材料化学工程国家重点实验室, 江苏南京211816, 中国
^b新加坡科技研究局化学与工程科学研究院, 新加坡, 中国
^c南京工业大学材料科学与工程学院, 材料化学工程国家重点实验室, 江苏南京211816, 中国
^d中国科学院高能物理研究所, 北京100049, 中国

收稿日期:2022-11-24 接受日期:2023-03-06 出版日期:2023-05-18 发布日期:2023-04-20
通讯作者: * 电子信箱: njutzhouyu@njtech.edu.cn (周瑜), junwang@njtech.edu.cn (王军).
基金资助:
国家自然科学基金(22072065);国家自然科学基金(22178162);国家自然科学基金(22222806);国家自然科学基金(U1662107);国家自然科学基金(21136005);江苏省杰出青年基金(BK20220053);江苏省“六大人才高峰”项目(JNHB-035);材料化学工程国家重点实验室开放基金(KL20-07);江苏省研究生研究与实践创新计划(KYCX20_1018);江苏省高等学校优势学科建设项目

Benzimidazole-based covalent organic framework embedding single-atom Pt sites for visible-light-driven photocatalytic hydrogen evolution

Fangpei Ma^a, Qingping Tang^a, Shibo Xi^b, Guoqing Li^a, Tao Chen^a, Xingchen Ling^a, Yinong Lyu^c, Yunpeng Liu^d, Xiaolong Zhao^a, Yu Zhou^a^,^*(), Jun Wang^a^,^*()

^aState Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemical Engineering, Nanjing Tech University, Nanjing 211816, Jiangsu, China
^bInstitute of Chemical and Engineering Sciences, Jurong Island, Singapore 627833, Singapore
^cState Key Laboratory of Materials-Oriented Chemical Engineering, College of Materials Science and Engineering, Nanjing Tech University, Nanjing 211816, Jiangsu, China
^dInstitute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049, China

Received:2022-11-24 Accepted:2023-03-06 Online:2023-05-18 Published:2023-04-20
Contact: * E-mail: njutzhouyu@njtech.edu.cn (Y. Zhou), junwang@njtech.edu.cn (J. Wang).
Supported by:
National Natural Science Foundation of China(22072065);National Natural Science Foundation of China(22178162);National Natural Science Foundation of China(22222806);National Natural Science Foundation of China(U1662107);National Natural Science Foundation of China(21136005);Distinguished Youth Foundation of Jiangsu Province(BK20220053);Six Talent Peaks Project in Jiangsu Province(JNHB-035);State Key Laboratory of Materials-Oriented Chemical Engineering-Open Fund(KL20-07);Postgraduate Research & Practice Innovation Program of Jiangsu Province(KYCX20_1018);Project of Priority Academic Program Development of Jiangsu Higher Education Institutions (PAPD)

摘要/Abstract

摘要：

氢气(H₂)是一种清洁的无碳燃料, 具有很高的能量密度, 是化石能源的潜在替代品之一. 半导体光催化水分解反应可将取之不竭的太阳能转化为氢气中的化学能, 从而提供一条有前途的、经济和环境友好的产氢路线. 光催化析氢反应(HER)涉及光捕集、激发、电荷分离和传输, 以及表面质子还原过程. 光激发态通常在几皮秒内发生, 通过辐射或非辐射复合弛豫返回到基态, 然而, 光生电子迁移到表面并触发两电子的质子还原是一个慢过程, 时间通常在几毫秒或以上. 整个过程中转换效率因光生电子极易复合而大大降低. 因此, 如何延长光生电子寿命, 促进电子及时传递到表面析氢位点, 提高催化位点的析氢速率, 是设计水分解高效光催化剂的关键, 也是该领域的难题. 有机半导体催化剂可以从地球丰度高的轻元素制备, 具有成本低、毒性小和结构多样等特点. 其中一个典型代表是共价有机框架(COFs), 其具有大的比表面积及丰富可调的骨架组成和孔道结构, 在分子水平上的可设计性具有独特优势. 苯并咪唑化合物具有较大极性和灵活可调的π共轭结构, 被广泛用作光电器件的共轭辅助分子. 以苯并咪唑基单体直接合成的COF种类罕见, 且未见相关COF用于光催化反应的报道.
本文通过选用不对称的苯并咪唑单体(2-(4-氨基苯基)-5-氨基苯并咪唑)与三醛基间苯三酚直接通过席夫碱化学反应缩合, 制备了苯并咪唑基COF. 该COF材料有效促进了光吸收和电荷分离/传递, 以及高活性Pt单原子析氢位点的形成, 在可见光驱动的析氢反应中表现出较好的析氢速率和转换频率. 采用微波辅助的溶剂热策略快速合成了苯并咪唑基COF (PABZ-Tp), 通过X射线衍射、傅立叶变换红外吸收光谱、¹³C固态核磁共振等研究其结构. 光学和光电化学表征结果表明, PABZ-Tp在可见光范围内展现出较好的光吸收, 具有较低的激子解离能(17.8 meV), 有效促进了长寿命自由光电子的形成. 骨架中带负电荷的苯并咪唑基团不但是Pt单原子形成和稳定的主要因素, 还有助于构建良好的电子迁移通道, 从而有效促进了光生电子快速传递到表面Pt单原子位点, 使得该催化剂在可见光驱动的析氢反应中表现出较高的催化效率, 析氢速率高达115 mmol g^-1 h^-1, 转换频率为4475.1 h^-1. 理论计算结合瞬态吸收光谱等实验结果表明, 苯并咪唑COF框架是产生高活性的关键, 对于光吸收、电荷分离传递以及高效析氢位点的构筑均起了重要作用. 综上, 本文构筑了一种高效的COF基有机光催化剂用于可见光析氢过程, 展示了使用不对称咪唑基单体构筑功能化COF材料的广阔前景.

关键词: 共价有机框架, 光催化, 析氢, 单原子催化, 可持续能源

Abstract:

Visible-light-driven photocatalytic hydrogen evolution reaction (HER) over a semiconductor provides an effective avenue to produce renewable clean energy and alleviate energy and environmental crises. However, the HER efficiency is still limited by the sluggish electron transfer process. Herein, a highly active covalent organic framework (COF) was constructed from the unusual benzimidazole monomer in a microwave-assisted solvothermal pathway. With single-atom Pt sites as cocatalyst, the catalyst exhibited an HER rate up to 115 mmol g^-1 h^-1 and a high turnover frequency of 4475.1 h^-1 under visible-light irradiation. The above performance relied on the combination of benzimidazole moieties and COF framework, which, on the one hand, stabilized photogenerated electrons to prolong the electron lifetime, and on the other hand provided a strong host-guest interaction that resulted in the creation of single-atom Pt sites and the acceleration of the electron-transfer to the active sites for proton reduction. This work demonstrates the perspective of electron stabilization and interfacial charge transfer avenue construction in the HER process, which can be reached by a molecular-level design of COF-based organic semiconductors by using structural and functional diverse asymmetric building blocks.

Key words: Covalent organic framework, Photocatalysis, Hydrogen evolution reaction, Single-atom catalysis, Renewable energy

马方沛, 汤庆平, 席识博, 李国庆, 陈涛, 凌星辰, 吕忆农, 刘云鹏, 赵小龙, 周瑜, 王军. 嵌入铂单原子的苯并咪唑基共价有机框架实现高效可见光析氢[J]. 催化学报, 2023, 48: 137-149.

Fangpei Ma, Qingping Tang, Shibo Xi, Guoqing Li, Tao Chen, Xingchen Ling, Yinong Lyu, Yunpeng Liu, Xiaolong Zhao, Yu Zhou, Jun Wang. Benzimidazole-based covalent organic framework embedding single-atom Pt sites for visible-light-driven photocatalytic hydrogen evolution[J]. Chinese Journal of Catalysis, 2023, 48: 137-149.

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图/表 4

Fig. 1. (a) Schematic illustration of the molecular structure for PABZ-Tp with the synthetic procedure. (b) Lattice structure at the top and side view (yellow: carbon; white: hydrogen; blue: nitrogen; red: oxygen; red: sulfur). (c) Experimentally observed (red) and Pawley refined (black) PXRD patterns with their refinement difference (gray), the reflections and the simulated one (blue) for ideal AA-stacking mode. (d) Solid-state 13C CP-MAS NMR spectrum of PABZ-Tp. (e) N2 sorption isotherms and the corresponding pore size distribution profiles of PABZ-Tp; HR-TEM (f) and Fourier transform (FFT) (g) images. HAADF-STEM (h) and the corresponding elemental mapping (i-k) images for C, N, and O atoms. Scale bars: f: 5 nm; g: 1 nm; h-k: 100 nm.

Fig. 2. UV-vis diffuse reflection absorption spectra (a), energy band gap (b) determined from the Kubelka-Munk-transformed reflectance spectra, transient photocurrent responses (c), electrochemical impedance spectra (d), steady-state Photoluminescence spectra (e), and time-resolved fluorescence decay spectra (f) of PABZ-Tp, PABZ-Tp-A, and Tp-BD.

Fig. 3. (a) Time-resolved HER activity of PABZ-Tp, PABZ-Tp-A, and Tp-BD. (b) TOF comparisons of PABZ-Tp (red pentastar) and other representative photocatalysts (entries 1-21 in Table S14; the circle is COF-based photocatalyst, the square is TiO2-based photocatalyst, the pentagon is MOF-based photocatalyst, and the diamond is amorphous polymer photocatalyst). (c) Cycling HER behavior of PABZ-Tp. (d) Wavelength-dependent AQE of PABZ-Tp. (e) The photocatalytic H2 evolution rate of PABZ-Tp, PABZ-Tp-A, and Tp-BD in the absence of Pt additive. (f) HR-TEM, AC HAADF-STEM images of Pt/PABZ-Tp, and corresponding electron lattice diffraction diagram; Pt L3-edge X-ray absorption near-edge structure (g) and corresponding k3-weighted Fourier transform spectra (h) at R space of Pt/PABZ-Tp, PtO2, and Pt foil.

Fig. 4. (a) TPV curves of PABZ-Tp and Tp-BD. (b) The radical anion pathway (solid arrow) and radical cationic pathway (dotted arrows) after photoexcitation of PABZ-Tp and Tp-BD, with the difference of the adiabatic stabilization energy of the radical cation and anion state relative to the neutral state for the optimized representative fragment of PABZ-Tp and Tp-BD. Charge distribution and dipole moment of the radical anion state for the optimized representative fragment of PABZ-Tp (c) and Tp-BD (d). C gray, H white, O red, N blue.

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嵌入铂单原子的苯并咪唑基共价有机框架实现高效可见光析氢

Benzimidazole-based covalent organic framework embedding single-atom Pt sites for visible-light-driven photocatalytic hydrogen evolution

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