采用共价有机骨架(COF)和g-C3N4纳米片构筑2D/2D S型异质结并用于高效光催化析氢

doi:10.1016/S1872-2067(22)64094-4

催化学报 ›› 2022, Vol. 43 ›› Issue (10): 2592-2605.DOI: 10.1016/S1872-2067(22)64094-4

采用共价有机骨架(COF)和g-C₃N₄纳米片构筑2D/2D S型异质结并用于高效光催化析氢

董鹏玉^a^,^†, 张艾彩珺^b^,^†, 程婷^c, 潘劲康^b, 宋骏^a, 张磊^a, 关荣锋^a, 奚新国^c^,^*(), 张金龙^d^,^#()

^a盐城工学院, 江苏省新型环保重点实验室, 江苏盐城 224051
^b盐城工学院化学化工学院, 江苏盐城 224051
^c盐城工学院材料科学与工程学院, 江苏省生态环境材料重点实验室, 江苏盐城 224051
^d华东理工大学化学与分子工程学院, 上海多介质环境催化与资源化工程技术研究中心, 上海 200237

收稿日期:2022-01-17 接受日期:2022-03-08 出版日期:2022-10-18 发布日期:2022-09-30
通讯作者: 奚新国,张金龙
作者简介:^†共同第一作者.
基金资助:
国家自然科学基金(51772258);国家自然科学基金(21403184);国家自然科学基金(21972040);国家自然科学基金(21878257);江苏省“青蓝工程”项目;江苏省研究生科研与实践创新项目(KYCX21_3147);上海市教委创新计划项目(2021-01-07-00-02-E00106);江苏省高等学校优秀科技创新团队;江苏省自然科学基金(BK20191024);上海市科学技术委员会(20DZ2250400)

2D/2D S-scheme heterojunction with a covalent organic framework and g-C₃N₄ nanosheets for highly efficient photocatalytic H₂ evolution

Pengyu Dong^a^,^†, Aicaijun Zhang^b^,^†, Ting Cheng^c, Jinkang Pan^b, Jun Song^a, Lei Zhang^a, Rongfeng Guan^a, Xinguo Xi^c^,^*(), Jinlong Zhang^d^,^#()

^aKey Laboratory for Advanced Technology in Environmental Protection of Jiangsu Province, Yancheng Institute of Technology, Yancheng 224051, Jiangsu, China
^bSchool of Chemistry and Chemical Engineering, Yancheng Institute of Technology, Yancheng 224051, Jiangsu, China
^cKey Laboratory for Ecological-Environment Materials of Jiangsu Province, School of Materials Science and Engineering, Yancheng Institute of Technology, Yancheng 224051, Jiangsu, China
^dKey Laboratory for Advanced Materials and Institute of Fine Chemicals, School of Chemistry & Molecular Engineering, Shanghai Engineering Research Center for Multi-media Environmental Catalysis and Resource Utilization, East China University of Science and Technology, Shanghai 200237, China

Received:2022-01-17 Accepted:2022-03-08 Online:2022-10-18 Published:2022-09-30
Contact: Xinguo Xi, Jinlong Zhang
About author:^†Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(51772258);National Natural Science Foundation of China(21403184);National Natural Science Foundation of China(21972040);National Natural Science Foundation of China(21878257);Qinglan Project of Jiangsu Province;Scientific Research and Practical Innovation Project for Graduate Students in Jiangsu Province(KYCX21_3147);Innovation Program of Shanghai Municipal Education Commission(2021-01-07-00-02-E00106);Outstanding Scientific and Technological Innovation Team of Universities of Jiangsu Province;Natural Science Foundation of Jiangsu Province(BK20191024);Science and Technology Commission of Shanghai Municipality(20DZ2250400)

摘要/Abstract

摘要：

作为一种清洁能源, 氢能因具有洁净、高热值、高效率和环境友好等特点, 而被认为是解决能源危机和环境问题的最理想的替代能源之一. 近年来, 利用太阳能光催化分解水析氢受到了人们的广泛关注, 开发高效的光催化剂成为研究重点. 构建具有良好界面接触、更快光生电荷转移效率以及高氧化还原能力的S型异质结被认为是提高光催化析氢性能的最有效途径之一.

本文制备了具有较高化学稳定性的β-酮烯胺基TpPa-1-COF纳米片, 并通过在乙二醇中超声剥离得到的g-C₃N₄纳米片(g-C₃N₄ NS), 再将它们各自的纳米片分散液混合后经过油浴加热回流处理, 由于TpPa-1-COF纳米片与g-C₃N₄纳米片两相之间的π-π共轭相互作用, 制得了一种独特的二维/二维(2D/2D) S型异质结TpPa-1-COF NS/g-C₃N₄ NS(TPCNNS)光催化剂. 为了比较, 通过物理混合的方法制备了TpPa-1-COF NS与g-C₃N₄ NS的混合物(TPCNNS-pm), 并制备了块体β-酮烯胺基TpPa-1-COF/块体g-C₃N₄复合材料(TPCN). 实验发现, 具有S型异质结的TpPa-1-COF NS与g-C₃N₄ NS之间表现出紧密的界面接触, 形成了π-π共轭异质界面. 稳态光致发光光谱(PL)、瞬态PL衰减谱、光电流-时间响应图和电化学阻抗谱结果表明, 相比于TPCNNS-pm和TPCN, TPCNNS样品表现出明显增强的光生载流子分离和转移效率, 这主要是由于2D/2D结构导致的π-π共轭异质界面极大地促进了光生电荷分离. 密度泛函理论计算表明, TpPa-1-COF和g-C₃N₄具有不同的功函数, 较大的功函数差值产生了较大的费米能级能量差, 这导致界面处的能带发生了向上/向下弯曲; 差分电荷密度分析表明, 基态条件下在π-π共轭异质界面区域中g-C₃N₄的界面电荷自发向TpPa-1-COF转移导致了内建电场的形成. 这种强的内建电场可以有效地驱动电荷定向迁移, 对于电荷的分离和利用具有很大帮助. 由于内建电场显著促进了载流子的分离和迁移, 导致在可见光照射下, 具有最佳复合比例的TPCNNS-2(TpPa-1-COF:g-C₃N₄ NS质量比为2:1)样品的光催化析氢速率(1153 μmol g^-1 h^-1)比纯TpPa-1-COF NS和g-C₃N₄ NS分别提高了2.8和5.6倍, 而且表现出良好的光催化稳定性. 另外, 通过DMPO自由基捕获实验证实了在可见光照射下TpPa-1-COF NS不能产生超氧阴离子自由基(^•O₂^-), 而TPCNNS-2样品却表现出明显的^•O₂^-信号, 进一步从实验上验证了2D/2D TpPa-1-COF NS/g-C₃N₄ NS异质结光生电荷的分离和迁移遵循S型机制. 总之, 本文为开发具有高效析氢性能的π-π共轭2D/2D COF基S型光催化异质结材料提供了新思路.

关键词: 共价有机框架材料, g-C₃N₄, π-π共轭, 2D/2D材料, S型异质结, 光催化析氢

Abstract:

The fabrication of S-scheme heterojunctions with fast charge transfer and good interface contacts, such as intermolecular π-π interactions, is a promising approach to improve photocatalytic performance. A unique two-dimensional/two-dimensional (2D/2D) S-scheme heterojunction containing TpPa-1-COF/g-C₃N₄ nanosheets (denoted as TPCNNS) was developed. The established maximum interfacial interaction between TpPa-1-COF NS and g-C₃N₄ NS may result in a π-π conjugated heterointerface. Furthermore, the difference in the work functions of TpPa-1-COF and g-C₃N₄ results in a large Fermi level gap, leading to upward/downward band edge bending. The spontaneous interfacial charge transfer from g-C₃N₄ to TpPa-1-COF at the π-π conjugated interface area results in the presence of a built-in electric field, according to the charge density difference analysis based on density functional theory calculations. Such an enhanced built-in electric field can efficiently drive directional charge migration via the S-scheme mechanism, which enhances charge separation and utilization. Thus, an approximately 2.8 and 5.6 times increase in the photocatalytic hydrogen evolution rate was recorded in TPCNNS-2 (1153 μmol g^-1 h^-1) compared to pristine TpPa-1-COF and g-C₃N₄ NS, respectively, under visible light irradiation. Overall, this work opens new avenues in the fabrication of 2D/2D π-π conjugated S-scheme heterojunction photocatalysts with highly efficient hydrogen evolution performance.

Key words: Covalent organic framework, g-C₃N₄, π-π, Conjugated, 2D/2D material, S-Scheme heterojunction, Photocatalytic hydrogen evolution

董鹏玉, 张艾彩珺, 程婷, 潘劲康, 宋骏, 张磊, 关荣锋, 奚新国, 张金龙. 采用共价有机骨架(COF)和g-C₃N₄纳米片构筑2D/2D S型异质结并用于高效光催化析氢[J]. 催化学报, 2022, 43(10): 2592-2605.

Pengyu Dong, Aicaijun Zhang, Ting Cheng, Jinkang Pan, Jun Song, Lei Zhang, Rongfeng Guan, Xinguo Xi, Jinlong Zhang. 2D/2D S-scheme heterojunction with a covalent organic framework and g-C₃N₄ nanosheets for highly efficient photocatalytic H₂ evolution[J]. Chinese Journal of Catalysis, 2022, 43(10): 2592-2605.

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图/表 9

Scheme 1. Preparation of TpPa-1-COF/g-C3N4 NS (TPCNNS) hybrid heterojunction.

Fig. 1. (a) PXRD patterns; (b) FT-IR spectra. (c) Raman spectra (excited at 532 nm). (d) N2 adsorption isotherms tested at 77 K (inset: pore size distributions). C 1s (e) and N 1s (f) high-resolution XPS spectra.

Fig. 2. SEM images of g-C3N4 NS (a), TpPa-1-COF NS (b), and TPCNNS-2 (c). TEM images of g-C3N4 NS (d), TpPa-1-COF NS (e), and TPCNNS-2 (f). (g?j) TEM-EDS mapping images (scale bar: 500 nm) of TPCNNS-2.

Fig. 3. AFM image (a) and corresponding height profiles (b) of TPCNNS-2.

Fig. 4. (a) Photocatalytic H2 evolution of as-prepared samples deposited with Pt co-catalyst (3 wt%) under visible light irradiation in 8 h. (b) Comparison of photocatalytic H2 evolution rate bar chart of all samples with error bar. (c) Cycle tests of photocatalytic H2 evolution over TPCNNS-2 and TpPa-1-COF NS. (d) AQE values at various wavelengths and the corresponding diffuse reflectance absorption spectrum of TPCNNS-2. XRD patterns (e) and FTIR spectra (f) of TPCNNS-2, before and after photocatalysis.

Fig. 5. (a) Steady-state PL spectra (excited at 280 nm). (b) Transient PL decay profiles of the light emission at 430 nm (excitation wavelength: 280 nm). (c) Photocurrent responses (I-t). (d) EIS Nyquist plots of various samples (inset shows the equivalent circuit model and the fitted results).

Fig. 6. (a) UV-vis diffuse reflectance absorption spectra; (b) Corresponding Tauc plots; (c) UPS spectra; (d) Schematic energy levels diagram of TpPa-1-COF NS and g-C3N4 NS.

Fig. 7. Electrostatic potential of TpPa-1-COF (001) surface (a) and g-C3N4 (001) surface (b) along the Z-axis direction (the insets show the corresponding optimized slab structures). The construction for simulating the interfaces of TpPa-1-COF (001)/g-C3N4 (001) heterojunction before geometry optimization (c,d) and after geometry optimization (e,f) from the top side and cross views with brown, grey, red, and light-pink representing N, C, O, and H, respectively. The calculated charge density differences in the TpPa-1-COF (001)/g-C3N4 (001) heterojunction from the top (g) and side views (h). The cyan region represents charge depletion, and the yellow region denotes charge accumulation. The isosurface value is 0.025 e Å-3 (i) Planar-averaged electron density difference of the TpPa-1-COF (001)/g-C3N4 (001) heterostructure.

Fig. 8. (a) DMPO spin-trapping EPR spectra of TpPa-1-COF NS, g-C3N4 NS, and TPCNNS. (b) Schematic illustration of two potential mechanisms (i.e., the systems of type II and S-scheme heterojunction) for charge-transfer of TPCNNS. (c) Schematic explanation of the charge migration mechanism in S-scheme TPCNNS heterostructure before contact, after contact in darkness, and irradiated with visible light.

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采用共价有机骨架(COF)和g-C₃N₄纳米片构筑2D/2D S型异质结并用于高效光催化析氢

2D/2D S-scheme heterojunction with a covalent organic framework and g-C₃N₄ nanosheets for highly efficient photocatalytic H₂ evolution

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[1]	赵彬彬, 钟威, 陈峰, 王苹, 别传彪, 余火根. 高晶化g-C₃N₄光催化剂: 合成、结构调控和光催化产氢[J]. 催化学报, 2023, 52(9): 127-143.
[2]	蔡铭洁, 刘艳萍, 董珂欣, 陈晓波, 李世杰. 漂浮型Bi₂WO₆/C₃N₄/碳布S型异质结光催化材料用于高效净化水体环境[J]. 催化学报, 2023, 52(9): 239-251.
[3]	孙丽娟, 于晓慧, 唐丽永, 王伟康, 刘芹芹. 构建K₃PW₁₂O₄₀/CdS核壳S型异质结实现同步太阳能光催化分解水和选择性苯甲醇氧化反应[J]. 催化学报, 2023, 52(9): 164-175.
[4]	刘鑫, 王茂弟, 任亦起, 刘嘉立, 戴慧聪, 杨启华. 构建模块化催化体系用于氢转移反应: 氢键的促进作用[J]. 催化学报, 2023, 52(9): 207-216.
[5]	宋明明, 宋相海, 刘鑫, 周伟强, 霍鹏伟. ZnIn₂S₄/MOF-808微球结构S型异质结光催化剂的制备及其光还原CO₂性能研究[J]. 催化学报, 2023, 51(8): 180-192.
[6]	李世杰, 王春春, 董珂欣, 张鹏, 陈晓波, 李鑫. 新型MIL-101(Fe)/BiOBr S型异质催化剂用于高效光催化降解抗生素和还原六价铬: 光催化性能分析和光催化机理研究[J]. 催化学报, 2023, 51(8): 101-112.
[7]	孙利娟, 王伟康, 路平, 刘芹芹, 王乐乐, 唐华. 纳米高熵合金实现光催化剂肖特基势垒的调控用于光催化制氢与苯甲醇氧化耦合反应[J]. 催化学报, 2023, 51(8): 90-100.
[8]	余治晗, 关晨, 岳晓阳, 向全军. 碳环渗入的结晶氮化碳S型同质结及其光催化析氢[J]. 催化学报, 2023, 50(7): 361-371.
[9]	牛青, 米林华, 陈玮, 李秋军, 钟升红, 于岩, 李留义. 基于共价有机框架的单位点光(电)催化材料的研究进展[J]. 催化学报, 2023, 50(7): 45-82.
[10]	何厚伟, 王中辽, 代凯, 李素文, 张金锋. LSPR效应增强碳包覆In₂O₃/W₁₈O₄₉ S型异质结用于高效CO₂光还原[J]. 催化学报, 2023, 48(5): 267-278.
[11]	李宁, 高雪云, 苏俊珲, 高旸钦, 戈磊. 类金属WO₂/g-C₃N₄复合光催化剂的构造及其优异的光催化性能[J]. 催化学报, 2023, 47(4): 161-170.
[12]	Eun Hyup Kim, Min Hee Lee, Jeehye Kim, Eun Cheol Ra, Ju Hyeong Lee, Jae Sung Lee. 无碱CO₂加氢高效制甲酸Pd/g-C₃N₄催化剂的单原子和纳米簇的协同作用[J]. 催化学报, 2023, 47(4): 214-221.
[13]	李钱, 唐麒君, 熊珮瑶, 陈东之, 陈建孟, 吴忠标, 王海强. 钯化学态对g-C₃N₄光催化还原CO₂的影响: 单原子态在促进CH₄生成中的独特作用[J]. 催化学报, 2023, 46(3): 177-190.
[14]	李瀚, 陶善仁, 万思杰, 邱国根, 龙庆, 余家国, 曹少文. ZnCdS纳米球和二苯并噻吩修饰的g-C₃N₄构成的S型异质结用于增强光催化产氢[J]. 催化学报, 2023, 46(3): 167-176.
[15]	张志洁, 王雪盛, 唐慧玲, 李德本, 徐家跃. 调控Cs₃Bi₂Br₉@V_O-In₂O₃ S型异质结的费米能级和内建电场促进光生电荷分离和二氧化碳还原[J]. 催化学报, 2023, 55(12): 227-240.