绝缘聚合物调控光氧化还原催化的起源研究

doi:10.1016/S1872-2067(24)60070-7

催化学报 ›› 2024, Vol. 63: 109-123.DOI: 10.1016/S1872-2067(24)60070-7

绝缘聚合物调控光氧化还原催化的起源研究

莫乔铃^,¹, 熊锐^,¹, 董俊豪, 萨百晟^*(), 郑晶莹, 陈青, 吴悦, 肖方兴^*()

福州大学材料科学与工程学院, 福建福州 350108

收稿日期:2024-03-08 接受日期:2024-06-05 出版日期:2024-08-18 发布日期:2024-08-19
通讯作者: *电子邮箱: bssa@fzu.edu.cn (萨百晟),fxxiao@fzu.edu.cn (肖方兴).
作者简介:
¹共同第一作者.
基金资助:
国家自然科学基金(21703038);国家自然科学基金(22072025);国家自然科学基金(21905050);福建省闽江学者资助计划;中国福建光电信息科学与技术创新实验室(2021ZR147)

Identification of origin of insulating polymer maneuvered photoredox catalysis

Qiao-Ling Mo^,¹, Rui Xiong^,¹, Jun-Hao Dong, Bai-Sheng Sa^*(), Jing-Ying Zheng, Qing Chen, Yue Wu, Fang-Xing Xiao^*()

College of Materials Science and Engineering, Fuzhou University, Fuzhou 350108, Fujian, China

Received:2024-03-08 Accepted:2024-06-05 Online:2024-08-18 Published:2024-08-19
Contact: *E-mail: bssa@fzu.edu.cn (B.-S. Sa), fxxiao@fzu.edu.cn (F.-X. Xiao).
About author:
¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(21703038);National Natural Science Foundation of China(22072025);National Natural Science Foundation of China(21905050);Award Program for Minjiang Scholar Professorship;Fujian Science & Technology Innovation Laboratory for Optoelectronic Information of China(2021ZR147)

摘要/Abstract

摘要：

固态非共轭聚合物由于缺乏沿分子链框架的离域π电子, 长期以来被视为不具备转移能力的绝缘聚合物. 因此, 利用这类固态绝缘聚合物作为载体介质来刺激电荷转移或光氧化还原催化, 在传统观念中被认为是不可行的. 在异相光催化中, 为了提升催化效率, 常采用煅烧法去除非共轭绝缘聚合物, 以暴露更多的活性位点, 增强界面接触, 从而减少界面电荷传输阻力并加速电荷转移. 然而, 由于聚合物的结构多样性和易获取性, 深入探索非共轭绝缘聚合物在光催化中的电荷传输机制具有重要意义.

本文采用静电自组装策略, 在常温下, 将表面带负电荷的ZnIn₂S₄ (ZIS)纳米片分散在带正电荷的固态绝缘支化聚乙烯亚胺(bPEI)的溶液中, 通过两者间的静电作用力, 制得具有高活性的、Zn空位调控的bPEI/ZIS光催化剂. X射线粉末衍射、拉曼光谱和紫外-可见漫反射光谱结果表明, bPEI的包覆并未改变ZIS的晶体结构和光学性质. 高分辨透射电镜、原子力显微镜、X射线光电子能谱、傅里叶变换红外光谱和热重分析等结果证明了bPEI的成功包覆及显著的电子相互作用. 采用瞬态吸收光谱、光致发光光谱、时间分辨光致发光光谱、光电流强度曲线和电化学阻抗曲线等光电化学测试, 研究了催化剂的电荷传输路径和分离效率. 电子顺磁共振谱和同步辐射吸收谱结果表明, 采用15 mg mL^‒1的bPEI溶液包裹的ZIS(简称15bPEI/ZIS)中的Zn空位浓度显著高于ZIS, 有利于延长载流子寿命. 结合理论计算结果, 推断bPEI的包裹可以优化Zn空位浓度, 促进H₂O和4-硝基苯胺的吸附. 研究了析氧反应(OER)每步所需的自由能, 结果表明, bPEI的存在有利于光生电子的转移. 光催化还原硝基化合物性能评价结果表明, 与ZIS相比, 15bPEI/ZIS表现出更好的光催化活性和稳定性. 在可见光下还原4-硝基苯胺体系中, 15bPEI/ZIS的转化率可达91.58%, 显著优于纯ZIS的16.33%. 通过在体系中混合ZIS和bPEI制得15bPEI+ZIS, 发现其光催化活性不如15bPEI/ZIS. 同时, 在惰性气氛下煅烧15bPEI/ZIS制得15bPEI/ZIS-200 °C, 相较于15bPEI/ZIS, 15bPEI/ZIS-200 °C的光催化性能没有显著提升, 证明15bPEI/ZIS样品中ZIS和bPEI间界面结合紧密, 存在强电子相互作用, 有利于提升界面电荷传输效率. 此外, 在ZIS表面包裹多种含胺基的有机分子和聚合物催化剂, 以及在ZIS和bPEI层间生长/刻蚀构建不同绝缘SiO₂厚度的催化剂, 通过光催化实验证实胺基官能团参与了界面电荷传输过程, 并在光催化反应中抑制电荷复合并提供大量活性位点.

综上, 本文从异相光催化的角度揭示了固态非共轭绝缘聚合物的电荷传输能力, 并探讨了绝缘聚合物中单体片段对光催化性能的贡献作用. 这种由绝缘聚合物包覆引起的协同缺陷工程、丰富的表面活性位点和加速的电荷流动动力学, 共同显著提升了光催化活性. 这一发现为利用固态绝缘聚合物操控电荷转移以实现太阳能转换提供新思路.

关键词: 绝缘聚合物, 电荷转移, 光氧化还原催化, 聚电解质, 自组装

Abstract:

Solid non-conjugated polymers have long been regarded as insulators due to deficiency of delocalized π electrons along the molecular chain framework. Up to date, origin of insulating polymer regulated charge transfer has not yet been uncovered. In this work, we unleash the root origin of charge transport capability of insulating polymer in photocatalysis. We ascertain that insulating polymer plays crucial roles in fine tuning of electronic structure of transition metal chalcogenides (TMCs), which mainly include altering surface electron density of TMCs for accelerating charge transport kinetics, triggering the generation of defect over TMCs for prolonging carrier lifetime, and acting as hole-trapping mediator for retarding charge recombination. These synergistic roles contribute to the charge transfer of insulating polymer. Our work opens a new vista of utilizing solid insulating polymers for maneuvering charge transfer toward solar energy conversion.

Key words: Insulating polymer, Charge transfer, Photoredox catalysis, Polyelectrolyte, Self-assembly

莫乔铃, 熊锐, 董俊豪, 萨百晟, 郑晶莹, 陈青, 吴悦, 肖方兴. 绝缘聚合物调控光氧化还原催化的起源研究[J]. 催化学报, 2024, 63: 109-123.

Qiao-Ling Mo, Rui Xiong, Jun-Hao Dong, Bai-Sheng Sa, Jing-Ying Zheng, Qing Chen, Yue Wu, Fang-Xing Xiao. Identification of origin of insulating polymer maneuvered photoredox catalysis[J]. Chinese Journal of Catalysis, 2024, 63: 109-123.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60070-7

https://www.cjcatal.com/CN/Y2024/V63/I8/109

图/表 4

Fig. 1. (a) Schematic illustration of electrostatic self-assembly of bPEI/ZIS nanocomposites. (b) XRD patterns of ZIS and 15bPEI/ZIS. (c) DRS results of ZIS and 15bPEI/ZIS with corresponding transformed plots calculated by the Kubelka-Munk function vs. photon energy (inset). High-resolution Zn 2p (d), In 3d (e), S 2p (f) and N 1s (g) spectra of ZIS and 15bPEI/ZIS. AFM analysis with height profiles in the inset (h), TEM (i) and HRTEM (j) images of 15bPEI/ZIS with SAED pattern in the inset. (k) TEM-EDS mapping result of 15bPEI/ZIS nanocomposite for Zn, In, S, N, and C elements.

Fig. 2. (a) Photoactivities of ZIS and 15bPEI/ZIS toward anaerobic photocatalytic reduction of a series of aromatic nitro compounds including 2-NA, 3-NA, 4-NA, 2-NP, 3-NP, 4-NP, NB, 4-nitrotoluene, 4-nitroanisole and 4-nitroacetophenone with adding ammonium formate as hole scavenger under visible light irradiation (λ > 420 nm). (b) Photoactivities of ZIS, 15PAH/ZIS, 15LPEI/ZIS and ZIS@amine-containing organic molecules (Ethylenediamine, N,N-Dimethylenediamine, N,N,N,N-Tetramethylenediamine and Triethylamine) toward photoreduction of 4-NA under the same conditions with corresponding molecular structures clearly displayed. (c) Photoactivities of CIS and 15bPEI/CIS (25 min), In2S3 and 15bPEI/In2S3 (25 min), and CdS and 15bPEI/CdS (10 min) toward photoreduction of 4-NA. (d) Photoactivities of ZIS, ZIS@xSiO2, and ZIS@xSiO2-15bPEI (x = 1, 2, 3 mL TEOS) with different SiO2 coating thickness, ZIS@3SiO2-Exh (x = 1, 2, 4 h), ZIS@3SiO2-Exh-15bPEI with different etching time, and the optimal 15bPEI/ZIS toward photoreduction of 4-NA. HRTEM images of SiO2-coated ZIS without etching and with etching for different time including ZIS@3SiO2 (e), ZIS@3SiO2-E1h (f), ZIS@3SiO2-E2h (g), and ZIS@3SiO2-E4h (h) with corresponding schematic models displayed in the insets. (i) High angle annular dark-field (HAADF) TEM images of ZIS@3SiO2-E4h nanocomposite with elemental mapping results.

Fig. 3. Characterizations of photoexcited charge separation efficiency. Ultrafast TA kinetics at a probe wavelength of 600 nm for 15bPEI/ZIS (a) and ZIS (b). The TA signal (i.e., differential absorbance, ΔA) is given in mOD, where OD stands for the optical density. (c) Time-resolved transient PL decay curves of ZIS and 15bPEI/ZIS under an excitation wavelength of 540 nm. (d) Room-temperature PL spectra of ZIS and 15bPEI/ZIS. Transient photocurrent responses (e) and anodic transient dynamics (f) of ZIS and 15bPEI/ZIS under visible light irradiation (λ > 420 nm, inset: on-off I-t results). (g) Open-circuit-potential decay curves of ZIS and 15bPEI/ZIS. (h) Nyquist plots of EIS results for ZIS and 15bPEI/ZIS under visible light irradiation (λ > 420 nm). (i) Schematic illustration of the PEC water dissociation mechanism.

Fig. 4. Plot of charge density difference (violet: charge depletion, skyblue: charge accumulation) for the most energy favorable model of H2O (a) and 4-NA (b) molecular absorbed on the ZIS@bPEI monolayer surface. (c) EPR spectra of ZIS and 15bPEI/ZIS. (d) Zn K-edge XANES spectra of Zn foil, ZIS and 15bPEI/ZIS. (e) k3-weighted Fourier transform (FT) χ(k) function of the EXAFS spectra for Zn foil, ZIS and 15bPEI/ZIS. (f) CV curves of bPEI with different concentrations (15, 30, 60 mg mL?1) in CH2Cl2 with 0.1 mol L?1 tetrabutylammonium tetrafluoroborate for scanning profile of ?1.5?1.5 V. (g) Schematic illustration of the photocatalytic mechanism of bPEI/ZIS nanocomposite.

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绝缘聚合物调控光氧化还原催化的起源研究

Identification of origin of insulating polymer maneuvered photoredox catalysis

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