钴配位共价有机框架用于染料敏化光电化学水分解

doi:10.1016/S1872-2067(26)65196-0

催化学报 ›› 2027, Vol. 92: 248-261.DOI: 10.1016/S1872-2067(26)65196-0

钴配位共价有机框架用于染料敏化光电化学水分解

梁子展^a^,¹, 王晓林^a^,¹, 洪智林^a, 李鑫奥^a, 彭新邦^a, 谭礼林^b^,^*(), 肖利民^c, 周业成^a^,^*(), 刘军民^a^,^*()

^a 中山大学材料科学与工程学院, 广东省低碳化学与节能重点实验室, 广东广州 510275
^b 汕头市绿色精密制造高值化学品工程技术研究中心, 化学与精细化工广东省实验室, 广东汕头 515031
^c 北京航空航天大学计算机科学与工程学院, 北京 100191

收稿日期:2026-02-26 接受日期:2026-04-02 出版日期:2027-01-02 发布日期:2026-10-30
通讯作者: *电子信箱: tanll@ccelab.com.cn (谭礼林),
zhouych29@mail.sysu.edu.cn (周业成),
liujunm@mail.sysu.edu.cn (刘军民).
作者简介:第一联系人：
1共同第一作者.
基金资助:
国家自然科学基金(22275214);国家自然科学基金(21975291);广东省自然科学基金(2024A1515012076);广东省自然科学基金(2022A1515011949);广东特支计划青年拔尖人才项目(2024TQ08C327)

Cobalt-coordinated covalent organic framework as a versatile water oxidation catalyst in dye-sensitized photoelectrochemical cells for solar water splitting

Zizhan Liang^a^,¹, Xiaolin Wang^a^,¹, Zhilin Hong^a, Xinao Li^a, Xinbang Peng^a, Lilin Tan^b^,^*(), Limin Xiao^c, Yecheng Zhou^a^,^*(), Junmin Liu^a^,^*()

^a The Key Laboratory of Low-Carbon Chemistry & Energy Conservation of Guangdong Province, School of Materials Science and Engineering, Sun Yat-sen University, Guangzhou 510275, Guangdong, China
^b Shantou Engineering Technology Research Center for Green and Precise Manufacturing of High-value Chemicals, Chemistry and Chemical Engineering Guangdong Laboratory, Shantou 515031, Guangdong, China
^c School of Computer Science and Engineering, Beihang University, Beijing 100191, China

Received:2026-02-26 Accepted:2026-04-02 Online:2027-01-02 Published:2026-10-30
Contact: *E-mail: tanll@ccelab.com.cn (L.-L. Tan),
zhouych29@mail.sysu.edu.cn (Y. Zhou),
liujunm@mail.sysu.edu.cn (J.-M. Liu).
About author:First author contact:
¹ Contributed equally to this work.
Supported by:
National Natural Science Foundation Project of China(22275214);National Natural Science Foundation Project of China(21975291);Natural Science Foundation Project of Guangdong Province(2024A1515012076);Natural Science Foundation Project of Guangdong Province(2022A1515011949);Tip-top Scientific and Technical Innovative Youth Talents of Guangdong Special Support Program(2024TQ08C327)

摘要/Abstract

摘要：

太阳能驱动的光催化水分解是实现可再生能源转化的重要途径, 其中染料敏化光电化学电池(DSPEC)因结构可调、成本可控而备受关注. 然而, DSPEC的实际应用受限于高效、稳定的水氧化催化剂(WOC)的缺乏. 共价有机框架(COFs)是一类具有高比表面积、可预先设计结构和周期性孔道的晶态多孔聚合物, 在催化领域展现出巨大潜力, 但将其作为WOC集成到DSPEC中的研究目前仍未见报道. 本研究合成了一种高结晶度的钴配位共价有机框架(TFPP-Co-COF), 并将其成功应用于DSPEC光阳极, 实现了高效、稳定的光驱动水氧化. 该工作不仅为DSPEC提供了一种新型高性能WOC, 也为COFs在太阳能燃料生产中的进一步应用开辟了新方向.

本文利用COFs的晶态结构与可功能化特性, 通过钴原子与卟啉环的配位引入催化活性中心, 构建具有高结晶度、大比表面积和均匀钴位点的TFPP-Co-COF. 同时, 制备无定形对照物(TFPP-Co-polymer)和无金属对照物(TFPP-COF), 系统对比晶态结构、钴位点以及界面电子转移对光阳极性能的影响. 通过溶剂热法合成TFPP-Co-COF, 傅里叶变换红外光谱证实亚胺键的形成及钴-氮配位; 粉末X-射线衍射显示其在3.3°处有尖锐衍射峰, Pawley精修验证高结晶性; 氮气吸附测试表明比表面积为730.3 m²/g, 平均孔径2.56 nm; 扫描电镜和透射电镜观察到清晰的晶格条纹(晶面间距2.60 nm), 像差校正透射电镜显示钴原子均匀分布(间距约2.5 nm). 将TFPP-Co-COF与N719光敏剂共负载于TiO₂/FTO光阳极. 光电化学测试表明: 在0 V vs. Ag/AgCl偏压下, 光阳极初始光电流密度达800 μA/cm², 200 s后仍保持700 μA/cm²; 在无偏压(0 V vs. NHE)条件下, 光电流密度为450 μA/cm², 25 min后保持400 μA/cm². 电化学阻抗谱显示TFPP-Co-COF具有最高的复合电阻和最低的电荷转移电阻. 发生器-收集器装置测得有偏压下析氧法拉第效率为88.8%, 无偏压下为71.6%. 此外, TFPP-Co-COF与纯有机染料C4BTP和DT1也表现出良好兼容性, 进一步证明其普适性. 在机理研究方面, 固体荧光光谱表明N719与TFPP-Co-COF混合后荧光显著猝灭, 证实从COF到光敏剂的高效电子转移; 荧光滴定得猝灭常数为-7.14 μL^-1, 远高于TFPP-COF的-5.67 μL^-1, 表明钴位点增强电子给体能力; X-射线光电子能谱显示光照后Co 2p峰正移0.20 eV, 直接证明钴作为电子给体. 密度泛函理论计算表明,水氧化通过钴位点的亲核水进攻路径进行, 最大吉布斯自由能垒在染料存在下从1.59降至0 eV, 而金属-free路径能垒更高.

综上, 本研究将晶态钴配位COF作为高效水氧化催化剂应用于DSPEC, 其优异性能源于高结晶度、高比表面积、均匀分散的钴活性位点及高效电子转移, 展示了COFs在太阳能水分解中的巨大潜力, 为太阳能驱动水分解提供了新的催化剂设计思路.

关键词: 染料敏化光电化学电池, 共价有机框架, 光敏剂, 水氧化催化剂, 太阳能水分解

Abstract:

The development of efficient water oxidation catalysts is crucial for advancing dye-sensitized photoelectrochemical cells toward practical solar-driven water splitting. Herein, we synthesize a cobalt-coordinated covalent organic framework, TFPP-Co-COF, and integrate it with photosensitizers to construct high-performance photoanodes. The optimized electrode achieves an initial photocurrent density of 800 μA/cm² at 0 V vs. Ag/AgCl, maintaining 700 μA/cm² after 200 s with a Faradaic efficiency of 88.8%. Even under unbiased conditions (0 V vs. NHE), it delivers 450 μA/cm² (71.6% FE) and retains 400 μA/cm² over 25 min. Mechanistic studies confirm efficient electron transfer from TFPP-Co-COF to the photosensitizer. Theoretical calculations further reveal that water oxidation proceeds through a water nucleophilic attack pathway at cobalt sites, exhibiting a lower energy barrier than metal-free alternatives. The superior performance over amorphous analogs originates from enhanced crystallinity, high surface area, and abundant cobalt active sites that collectively promote charge separation and catalytic activity. TFPP-Co-COF also demonstrates excellent compatibility with pure organic dyes C4BTP and DT1, highlighting its versatility. This work pioneers COF application in DSPECs, providing a promising pathway for efficient solar fuel production.

Key words: Dye-sensitized photoelectrochemical cells, Covalent organic frameworks, Photosensitizers, Water oxidation catalysts, Solar water splitting

梁子展, 王晓林, 洪智林, 李鑫奥, 彭新邦, 谭礼林, 肖利民, 周业成, 刘军民. 钴配位共价有机框架用于染料敏化光电化学水分解[J]. 催化学报, 2027, 92: 248-261.

Zizhan Liang, Xiaolin Wang, Zhilin Hong, Xinao Li, Xinbang Peng, Lilin Tan, Limin Xiao, Yecheng Zhou, Junmin Liu. Cobalt-coordinated covalent organic framework as a versatile water oxidation catalyst in dye-sensitized photoelectrochemical cells for solar water splitting[J]. Chinese Journal of Catalysis, 2027, 92: 248-261.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65196-0

https://www.cjcatal.com/CN/Y2027/V92/I1/248

图/表 6

Scheme 1. Schematic diagram of DSPEC device based on OPPs (middle) and chemical structures of dyes (left) and WOCs (right).

Fig. 1. (a) The synthetic route of TFPP-Co-COF under solvothermal conditions. (b) FT-IR spectra of TFPP-Co-COF, TFPP-Co-polymer and TFPP-COF. (c) Experimental, Pawley-refined, and simulated PXRD patterns of TFPP-Co-COF (Rp: unweighted-profile factor; Rwp: weighted-profile factor). (d) Solid-state UV-vis spectra of TFPP-Co-COF, TFPP-Co-polymer and TFPP-COF. (e) Mott-Schottky plot of TFPP-Co-COF. (f) Energy level diagrams of N719, OPPs and the oxygen evolution oxidation potential of water. (g) The nitrogen adsorption isotherm measured at 77 K and (h) the pore size distribution curves of TFPP-Co-COF.

Fig. 2. (a,b) SEM images of TFPP-Co-COF at different magnifications. STEM (c) and AC-TEM (d) images of TFPP-Co-COF. (e) SEM image of FTO|TiO2|N719+TFPP-Co-COF. (f) Profile analysis of electrode structure (Blue area represents FTO glass, yellow area represents TiO2 attached with dye molecules and purple area represents OPPs).

Fig. 3. (a) Schematic diagram of preparation process of sensitized electrode. (b) LSV curves of the N719-sensitized electrodes corresponding to different OPPs under positive scan direction. (c) I-t curves of photoanodes corresponding to the different OPPs with a bias of 0 V vs. Ag/AgCl. (d) DPV curves of FTO|TiO2|N719+TFPP-Co-COF, FTO|TiO2|N719 and FTO|TiO2|TFPP-Co-COF. EIS Nyquist plots of photoanodes in the dark with a bias of -0.6 V vs. Ag/AgCl (R1: series resistance; R2: recombination resistance; CPE: constant phase element) (e) and under irradiation with a bias of 0.2 V vs. Ag/AgCl (R1: series resistance; R2: charge-transfer resistance; CPE: constant phase element) (f). (g) I-t curves of photoanodes corresponding to the different OPPs with a bias of 0 V vs. NHE. (h) Long-term illumination test of electrodes corresponding to different OPPs under illumination without bias voltage in a dual-electrode system. Faradaic efficiency test results of FTO|TiO2|N719+TFPP-Co-COF in three-electrode system at 0 V vs. Ag/AgCl (i) and in dual-electrode system without bias voltage (j).

Fig. 4. (a) Energy level diagram of various dyes matching with TFPP-Co-COF. (b) Open circuit voltage-time curves of electrodes sensitized by different dyes. I-t curves of photoanodes sensitized by different dyes with a bias of 0 V vs. Ag/AgCl (c) and with a bias of 0 V vs. NHE (d). (e) Long-term illumination test of electrodes sensitized by different dyes under illumination without bias voltage in a dual-electrode system. (f) IPCE curves of different dye-sensitized electrodes loaded with TFPP-Co-COF.

Fig. 5. (a) Solid-state FL spectra of N719, TFPP-Co-COF and their complexes. (b) Fluorescence intensity-titration volume curves of fluorescence quenching experiment of OPPs. (c) Mechanism of water oxidation catalyzed by Co active site on TFPP-Co-COF. (d) XPS spectra of Co on TFPP-Co-COF before and after illumination. (e) Gibbs free energy diagrams for oxygen evolution at Co active sites of TFPP-Co-COF. (f) Gibbs free energy diagrams for direct oxygen evolution at C1 active sites of TFPP-COF.

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钴配位共价有机框架用于染料敏化光电化学水分解

Cobalt-coordinated covalent organic framework as a versatile water oxidation catalyst in dye-sensitized photoelectrochemical cells for solar water splitting

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