入射光切换调控空心等离子激元TiO2/AuCu@COF核壳光催化剂的CO2还原产物选择性

doi:10.1016/S1872-2067(26)65075-9

催化学报 ›› 2026, Vol. 87: 87-99.DOI: 10.1016/S1872-2067(26)65075-9

入射光切换调控空心等离子激元TiO₂/AuCu@COF核壳光催化剂的CO₂还原产物选择性

袁欣^a^,¹, 吴林艺^a^,¹, 曹凤莹^a, 徐乐楚^a, 王鹏^b, 石胡琳^a, 仲淑贤^b^,^*(), 刘炼^a, 莫伟豪^c^,^*(), 赵雷洪^a, 柏嵩^a^,^*()

^a 浙江师范大学化学与材料科学学院, 先进催化材料教育部重点实验室, 全省先进催化与吸附材料重点实验室, 浙江金华 321004
^b 浙江师范大学地理与环境科学学院, 全省流域环境数智监测与修复重点实验室, 浙江金华 321004
^c 攀枝花学院生物与化学工程学院, 四川攀枝花 617000

收稿日期:2025-11-27 接受日期:2026-02-01 出版日期:2026-08-18 发布日期:2026-06-24
通讯作者: ^*电子信箱: shuxian@zjnu.edu.cn (仲淑贤),
whaomo@163.com (莫伟豪),
songbai@zjnu.edu.cn (柏嵩).
作者简介:¹共同第一作者.
基金资助:
国家自然科学基金(22572174);浙江省自然科学基金(LMS25B030006);浙江省自然科学基金(LY20B030003);浙江省“尖兵” “领雁”研发公关计划(2023C03148);金华市科技计划项目(2024-4-011);浙江省大学生创新创业训练计划项目(S202510345033)

Light-switchable product selectivity in CO₂ photoreduction over hollow plasmonic TiO₂/AuCu@COF core-shell architectures

Xin Yuan^a^,¹, Linyi Wu^a^,¹, Fengying Cao^a, Lechu Xu^a, Peng Wang^b, Hulin Shi^a, Shuxian Zhong^b^,^*(), Lian Liu^a, Weihao Mo^c^,^*(), Leihong Zhao^a, Song Bai^a^,^*()

^a Key Laboratory of the Ministry of Education for Advanced Catalysis Materials, Zhejiang Key Laboratory of Advanced Catalysis and Adsorption Materials, Zhejiang Normal University, Jinhua 321004, Zhejiang, China
^b Zhejiang Key Laboratory of Digital Intelligence Monitoring and Restoration of Watershed Environment, College of Geography and Environmental Sciences, Zhejiang Normal University, Jinhua 321004, Zhejiang, China
^c School of Biological and Chemical Engineering, Panzhihua University, Panzhihua 617000, Sichuan, China

Received:2025-11-27 Accepted:2026-02-01 Online:2026-08-18 Published:2026-06-24
About author:¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22572174);Zhejiang Provincial Natural Science Foundation of China(LMS25B030006);Zhejiang Provincial Natural Science Foundation of China(LY20B030003);Key Research and Development Program of Zhejiang Province(2023C03148);Foundation of Science and Technology Bureau of Jinhua(2024-4-011);College Students’ Innovation and Entrepreneurship Training Program of Zhejiang Province(S202510345033)

摘要/Abstract

摘要：

太阳光驱动CO₂和H₂O转化为高价值化学品和燃料, 是实现碳循环闭环、缓解全球能源与环境危机的重要途径. 然而, 较差的产物选择性严重限制了该技术的实际应用. CO₂光还原包含多步质子耦合电子转移过程, 经由不同反应路径可生成多样的C₁和C₂₊产物. 尽管提升目标产物选择性已成为研究热点, 但现有策略仍主要依赖于光催化剂自身的精确调控. 相比之下, 基于入射光波长切换的产物选择性调控策略, 可有效规避繁琐的催化剂优化过程, 在最大化光能转换效率的同时, 实现无需催化剂更换或改性的产物灵活切换, 为按需调控CO₂还原产物开辟了简便高效的新途径. 因此, 构建入射光波长响应型CO₂还原催化体系意义重大.

本文制备了一种具有空心核壳结构的等离子激元TiO₂/AuCu@TB-COF(TACT)异质结, 通过改变入射光波长实现了纯水体系中CO₂光还原产物选择性的精准调控. 该催化剂以紫外光响应的TiO₂空心球为内核, 以增强入射光的多重反射和散射; 同时吸收紫外光和可见光的多孔TB-COF(TAPT-BTCA-COF, 其中TAPT = 4,4',4''-(1,3,5-三嗪-2,4,6-三基)三苯胺, BTCA = 1,3,5-均苯三甲醛)为外壳, 以促进反应物和产物的高效传质. 此外, 将具有可见光吸收特性的等离子激元AuCu纳米粒子嵌入TiO₂核与TB-COF壳之间以促进界面电荷转移过程. 原位光照X-射线光电子能谱技术结合光电化学测试表明, 在紫外光照射下, TiO₂核和TB-COF壳产生的光生电子均迁移至位于两者中间的AuCu进行CO₂还原反应, 有效促进了载流子的空间分离, 使得更多电子和空穴参与CO₂还原和H₂O氧化过程. 此外, 原位傅里叶变换红外光谱和密度泛函理论计算表明, TiO₂核提供了高效的H₂O氧化位点, 加速了O₂析出和质子释放, 而AuCu能够稳定*CO中间体使其经历连续加氢过程而非直接脱附. 得益于充足的电子和质子供应以及更有利的CO₂甲烷化路径, TACT实现了343.9 μmol g_cat^-1 h^-1的CH₄产率和98.7%的CH₄选择性. 相反, 在可见光照射下, 尽管AuCu具有电磁近场增强效应并能将热电子注入到TB-COF中, 但光生电子和空穴均集中在COF壳层上, 分别进行CO₂还原和H₂O氧化反应, 从而降低了载流子分离效率. 此外, TB-COF表面较缓慢的H₂O氧化析氧动力学延缓了质子释放速率, 而且*CO中间体在TB-COF表面更易发生脱附而非连续加氢. 由于有限的电子和质子供应, 加之*CO更易发生脱附, TACT选择性地将CO₂还原为CO, 其产率和选择性分别为132.7 μmol g_cat^-1 h^-1和86.6%.

综上, 本文通过切换TACT异质结催化剂的入射光波长, 成功实现了CO₂光还原产物选择性的调控. 该工作揭示了依赖于入射光波长的载流子传输路径、质子供应速率及中间体吸附-脱附行为对产物选择性的协同调控机制, 为开发智能化人工光合成体系提供了新策略.

关键词: 光控催化剂, CO₂还原, H₂O氧化, 电子与质子差异化供给, *CO中间体不同反应路径

Abstract:

The development of photo-switchable CO₂ reduction catalysts capable of selectively generating two distinct target products under different light irradiation holds significant potential for achieving multifunctional catalysis and enhancing economic viability in industrial applications, yet remains a formidable challenge. Herein, we demonstrate a hollow core-shell plasmonic TiO₂/AuCu@TB-COF (TACT) photocatalyst that achieves 343.9 μmol g_cat^-1 h^-1 activity and 98.7% selectivity toward CH₄ under ultraviolet (UV) light, but switches to 132.7 μmol g_cat^-1 h^-1 activity with 86.6% selectivity for CO under visible light in pure water without altering any other reaction conditions. Comprehensive mechanistic studies reveal that UV and visible light selectively excite different components, inducing distinct interfacial charge transfer routes. This not only endows TACT with higher charge separation efficiency under UV light versus visible light, but also directs photocarriers to different active sites for redox reactions depending on the irradiation wavelength. Specifically, H₂O oxidation occurring on the TiO₂ core under UV light more favorably promotes O₂ evolution and proton liberation compared to oxidation on the TB-COF shell under visible light. For CO₂ reduction, UV light drives consecutive hydrogenation of *CO intermediates on the AuCu sites, whereas visible light preferentially induces *CO desorption from the TB-COF surface. The contrasting electron and proton supply, combined with the divergent fates of *CO intermediates, collectively govern the wavelength-dependent CO₂ reduction pathways.

Key words: Photo-switchable catalyst, CO₂ reduction, H₂O oxidation, Differential electron and proton supply, Divergent *CO intermediate fate

袁欣, 吴林艺, 曹凤莹, 徐乐楚, 王鹏, 石胡琳, 仲淑贤, 刘炼, 莫伟豪, 赵雷洪, 柏嵩. 入射光切换调控空心等离子激元TiO₂/AuCu@COF核壳光催化剂的CO₂还原产物选择性[J]. 催化学报, 2026, 87: 87-99.

Xin Yuan, Linyi Wu, Fengying Cao, Lechu Xu, Peng Wang, Hulin Shi, Shuxian Zhong, Lian Liu, Weihao Mo, Leihong Zhao, Song Bai. Light-switchable product selectivity in CO₂ photoreduction over hollow plasmonic TiO₂/AuCu@COF core-shell architectures[J]. Chinese Journal of Catalysis, 2026, 87: 87-99.

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图/表 6

Fig. 1. Synthesis and electronic microscopy characterizations of TACT. (a) Schematic illustrating the synthesis of TACT. TEM (b,c) and HRTEM (d) images of TAC. TEM (e,f), HRTEM (g), and STEM-EDS mapping (h) images of TACT.

Fig. 2. Spectroscopic characterizations of TACT and reference samples. (a) XRD patterns. (b) UV-vis DRS. (c) N2 sorption isotherms. (d) CO2 adsorption isotherms. High-resolution XPS spectra of Ti 2p (e), Au 4f (f), Cu 2p (g), and N 1s (h).

Fig. 3. Photocatalytic performance of TACT and reference samples. CO and CH4 evolution rates and selectivities under UV (a) and visible light (b) irradiation. (c) CO and CH4 yields of TACT under alternating UV and visible light illumination. (d) O2 evolution rates under UV and visible light irradiation. (e) Mass spectra of generated 13CH4 (top) and 13CO (bottom). (f) Recycling tests over TACT under UV and visible light irradiation, respectively.

Fig. 4. Light-dependent charge kinetics and mechanisms in TACT. Steady-state (a) and time-resolved (b) PL spectra of TACT and reference samples. (c) Photocurrent responses under UV and visible light irradiation. (d) Schematic illustrating the heterojunction formation and charge transfer mechanisms in TACT under UV and visible light irradiation. Charge density differences of TiO2/AuCu (e), AuCu/TB-COF (f), and TiO2/TB-COF (g) heterointerfaces (electron accumulation and depletion are represented by the yellow and blue regions, respectively; the isosurface is 0.002 electron per Å3).

Fig. 5. Light-dependent surface reactivities of TACT. EPR spectra of TEMPO-e- signals (a), TEMPO-h+ signals (b), DMPO-CO2•- signals (c), and DMPO-H signals (d) under UV and visible light irradiation. (e) In-situ DRIFTS spectra of TACT in CO2 photoreduction under UV (top) and visible (bottom) light irradiation.

Fig. 6. DFT calculations and light-dependent photocatalytic mechanisms in TACT. (a) CO2 adsorption energies on AuCu and TB-COF as well as H2O adsorption energies on TiO2 and TB-COF. (b) Gibbs free energy diagrams for H2O-to-O2 oxidation on TiO2 and TB-COF surfaces. (c) Gibbs free energy diagrams for CO2 reduction to CO and CH4 on AuCu and TB-COF surfaces. (d) Schematic illustrating the photocatalytic reaction mechanisms in TACT under UV and visible light irradiation.

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入射光切换调控空心等离子激元TiO₂/AuCu@COF核壳光催化剂的CO₂还原产物选择性

Light-switchable product selectivity in CO₂ photoreduction over hollow plasmonic TiO₂/AuCu@COF core-shell architectures

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