碳纳米角负载单分子分散酞菁钴限制质子转移增强酸性CO2电还原制CO

doi:10.1016/S1872-2067(26)65157-1

催化学报 ›› 2026, Vol. 89: 390-401.DOI: 10.1016/S1872-2067(26)65157-1

碳纳米角负载单分子分散酞菁钴限制质子转移增强酸性CO₂电还原制CO

王春春^a^,¹, 葛洋^a^,¹, 宋鑫东^a, 丁奕祺^b, 邢卓^a^,^*(), 余颖^a^,^*()

^a华中师范大学物理科学与技术学院,纳米科学与技术研究所,湖北武汉 430079
^b武汉大学动力与机械学院,湖北武汉 430072

收稿日期:2026-01-09 接受日期:2026-02-22 出版日期:2026-10-18 发布日期:2026-09-01
通讯作者: *电子信箱: xingzhuo@ccnu.edu.cn (邢卓),
yuying01@ccnu.edu.cn (余颖).
作者简介:
¹共同第一作者.
基金资助:
国家自然科学基金(12275199);国家自然科学基金(52472205);中央高校基本科研业务费(CCNU26ZH014)

Restricting proton transfer via carbon nanohorn-supported monomolecular cobalt phthalocyanine enhances CO₂-to-CO electrocatalysis in acidic media

Chunchun Wang^a^,¹, Yang Ge^a^,¹, Xindong Song^a, Yiqi Ding^b, Zhuo Xing^a^,^*(), Ying Yu^a^,^*()

^aInstitute of Nanoscience and Nanotechnology, College of Physical Science and Technology, Central China Normal University, Wuhan 430079, Hubei, China
^bSchool of Power and Mechanical Engineering, Wuhan University, Wuhan 430072, Hubei, China

Received:2026-01-09 Accepted:2026-02-22 Online:2026-10-18 Published:2026-09-01
Contact: *E-mail:xingzhuo@ccnu.edu.cn(Z. Xing),yuying01@ccnu.edu.cn(Y. Yu).
About author:
¹ Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(12275199);National Natural Science Foundation of China(52472205);self-determined research funds of CCNU from the colleges’ basic research and operation of MOE(CCNU26ZH014)

摘要/Abstract

摘要：

利用可再生电能驱动电催化二氧化碳还原反应(CO₂RR)为制备一氧化碳(CO)提供了一条温和且具有广阔前景的绿色技术路线. CO是合成各类基本有机化工品及中间体的关键原料, 为推动该技术应用, 大量研究致力于在酸性介质中进行CO₂RR. 因为酸性环境不仅有利于实现高CO₂利用率, 还能在工程上规避中性或碱性介质中常见的碳酸盐沉淀问题. 然而, 酸性介质的电化学条件更为严苛, 催化剂常因金属原子溶解或金属-载体间化学键断裂而失活. 因此, 为满足实际应用需求, 设计能在强酸环境中同时实现高活性和法拉第效率(FE)并保持优异稳定性的电催化剂至关重要.

本文通过将酞菁钴(CoPc)以单分子形式分散于富含拓扑缺陷的碳纳米角(CNHs)载体上, 利用CNHs独特的锥形尖端结构和大丽花状聚集体形貌, 构建了缺电子的Co中心及质子受限的微环境. X-射线光电子能谱和X-射线吸收精细结构谱证实CoPc与CNHs之间存在强相互作用, 诱导Co-N键的拉伸, 同时Co中心呈现缺电子态, 有利于CO₂活化. 电化学性能评估表明, 在pH为1的酸性电解液中, 最佳负载量的CoPc/CNHs-3催化剂在-1.2至-1.5 V电位区间内CO法拉第效率(FE_CO)均超过95%, 在-1.5 V时FE_CO达到96.8%, 且CO的分电流密度(j_CO)高达171.1 mA cm^-2, 转化频率(TOF)达到19472 h^-1. 即使在pH为0.5的强酸性条件下, CoPc/CNHs-3仍保持95.9%的FE_CO和259.1 mA cm^-2的j_CO, 并在38 h稳定性测试中保持>85%的FE_CO. 相比之下, 传统碳纳米管负载的CoPc在相同酸性条件下因难以抑制的析氢反应(HER)而性能急剧下降. 在旋转圆盘电极上的Koutecký-Levich分析定量揭示了CNHs载体对质子传质的双重限制作用: 一方面, CNHs表面丰富的五元环拓扑缺陷增加了质子沿碳骨架扩散的阻力, 抑制了表面氢溢流; 另一方面, CNHs的大丽花状聚集体结构重构了电极/电解质界面的双电层, 富集了外亥姆霍兹层的K⁺离子, 阻碍了水合氢离子从体相向活性位点的轴向扩散, 导致质子表观扩散系数降低37.5% (相较于纯CNHs)和75.0% (相较于CoPc/CNTs). 原位电化学阻抗谱显示, CoPc/CNHs-3在低频区具有独特的电化学响应, 表明其界面传质和吸附过程得到优化. 原位衰减全反射表面增强红外吸收光谱进一步揭示, 在CoPc/CNHs-3表面, CO₃^2-物种的强吸收峰反映了质子受限环境下可持续的质子耦合电子转移过程; *COOH中间体的增强吸附表明CO₂质子化步骤得到增强; 而*CO桥式吸附物种的显著富集则证实了CO生成路径的优势. 这些结果共同证明, CNHs载体通过构建质子受限微环境, 有效抑制了竞争性HER, 促进了关键中间体的稳定和转化, 从而在强酸性条件下实现了优异的CO₂RR性能.

综上, 本研究通过碳载体工程调控质子传质行为, 为在强酸性介质中实现高效CO₂电还原提供了新的设计思路. 这种通过载体结构设计构建质子受限微环境的策略, 不仅适用于CoPc分子催化剂, 也为其他分子催化剂体系在严苛反应条件下的应用提供了重要参考, 这将有助于开发更高效稳定的酸性CO₂电还原体系, 推动其实际应用.

关键词: 酞菁钴, 碳纳米角, 酸性二氧化碳电催化, 氢溢流, 受限质子传质

Abstract:

Electrocatalytic reduction of CO₂ to CO in acidic media is a compelling approach toward closing carbon cycle, as it can increase CO₂ utilization while circumvent carbonate precipitation. Nonetheless, a cardinal challenge remains the inherent competition from hydrogen evolution reaction (HER), driven by high proton availability at catalyst surface, which severely suppresses CO₂ reduction selectivity and activity. Herein, we engineer a catalyst comprising monomolecularly dispersed cobalt phthalocyanine on carbon nanohorns (CNHs) with abundant topological defects, which orchestrates efficient CO₂ electroreduction in acidic media via restricting proton transfer. This design constructs an electron-deficient Co center and surrounded with a proton-deficient microenvironment, achieving CO electrogeneration with 95.9% Faradaic efficiency (FE) and 259.1 mA cm^-2 partial current density at pH = 0.5 while maintaining > 85% FE across 38 h durability at pH 1. Mechanistic investigations reveal that the CNHs support simultaneously restricts both key proton-supply pathways: the defect-rich structure suppresses surface hydrogen spillover along the carbon framework, while the dahlia-like architecture of CNHs aggregate hinder axial hydronium diffusion from the bulk electrolyte. The resulting reduction in proton availability around Co centers, combined with limited hydronium access from the bulk, stabilizes crucial *COOH and *CO intermediates and accelerates CO₂ reduction kinetics. By showcasing how carbon-support engineering can modulate proton-transfer pathways, this work offers a viable and generalizable strategy toward high-performance CO₂ electrolysis in strongly acidic media, advancing the design of robust molecular catalysts for practical application.

Key words: Cobalt phthalocyanine, Carbon nanohorns, Acidic CO₂ electrocatalysis, Hydrogen spillover, Restricted proton transfer

王春春, 葛洋, 宋鑫东, 丁奕祺, 邢卓, 余颖. 碳纳米角负载单分子分散酞菁钴限制质子转移增强酸性CO₂电还原制CO[J]. 催化学报, 2026, 89: 390-401.

Chunchun Wang, Yang Ge, Xindong Song, Yiqi Ding, Zhuo Xing, Ying Yu. Restricting proton transfer via carbon nanohorn-supported monomolecular cobalt phthalocyanine enhances CO₂-to-CO electrocatalysis in acidic media[J]. Chinese Journal of Catalysis, 2026, 89: 390-401.

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https://www.cjcatal.com/CN/Y2026/V89/I10/390

图/表 5

Fig. 1. Synthesis and structural characterization of monomolecularly dispersed CoPc on CNHs. (a) Schematic illustration showing CoPc molecules immobilized on CNHs. (b) Raman spectra. (c) TEM image and structure diagram (inset) of CoPc/CNHs-3 catalyst. (d) HRTEM images of CoPc/CNHs-3 catalyst. (e) The AC-TEM image of CNHs fragment. (f) FFT filtered image of the selected area (red box), with pentagonal and hexagonal carbocycles marked in white and red, respectively. (g) HAADF-STEM image from 4D-STEM of CoPc/CNHs-3 catalyst with many single Co atoms (bright dots) distributed. Average Co atomic density is roughly 1.38 ± 1.13?atom nm-2. (h) EDX mapping of CoPc/CNHs-3 catalyst.

Fig. 2. Electronic structure and coordination environment characterization. High-resolution XPS spectra of Co 2p (a), N 1s (b), and C 1s (c) for CoPc/CNHs-3, CoPc, and CNHs catalysts. Co K-edge XANES spectra (d) and EXAFS spectra (e) of CoPc/CNHs-3, CoPc and Co foil references. (f) Fitted Fourier-transformed EXAFS spectra in R space for CoPc/CNHs-3 and CoPc. Wavelet-transformed EXAFS spectra of CoPc/CNHs-3 (g), CoPc (h), and Co foil (i).

Fig. 3. Electrocatalytic CO2RR performance in acid electrolyte. (a) FEs and jCO of CoPc/CNHs with different Co contents. FEs and total current densities over CoPc/CNHs-3 in 1 mol L-1 KCl (pH = 1) (b) and 1 mol L-1 KCl (pH = 0.5) (d) catholyte. (c) TOF of CO production for CoPc/CNHs-3 and CoPc in 1 mol L-1 KCl (pH = 1) catholyte. The TOF is calculated based on the total number of Co atoms in the catalyst as determined by ICP-OES. (e) FEs of products and total current densities over CoPc/CNTs in 1 mol L-1 KCl (pH = 0.5) catholyte. (f) FEs and jCO of CoPc/CNHs-3 and CoPc/CNTs with electrolyte pH from 7 to 0.5. (g) CO2RR durability of CoPc/CNHs-3 at -1.4 V vs. RHE and the corresponding FECO and FEH2 evolution with time in 1 M KCl (pH = 1) catholyte. (h) Comparison of CO product performance in this study with values reported for other catalysts. The error bars represent the standard deviation of three independent measurements.

Fig. 4. Effect of restricted proton transfer and reaction kinetics measurements of CO2RR. (a) CVs of CoPc/CNHs-3 and CoPc/CNTs electrodes in Ar-saturated 0.5 mol L-1 H2SO4 with a scan rate of 100 mV s-1. LSV curves of CoPc/CNHs-3 (b) and CoPc/CNTs (d) on RDE in Ar-saturated 0.1 mol L-1 K2SO4 (pH = 2.5) with different rotation rates. Linear fitting plots based on Koutecky-Levich equation for CoPc/CNHs-3 (c) and CoPc/CNTs (e) catalysts. Potential-dependent in-situ Nyquist plots of CoPc/CNHs-3 (f) and CoPc/CNTs (g) catalysts. Potential-dependent in-situ Bode phase plots of CoPc/CNHs-3 (h) and CoPc/CNTs (i) catalysts.

Fig. 5. In-situ spectroscopic investigation for intermediates detection. In-situ ATR-SEIRAS spectra on CoPc/CNHs-3 (a), CoPc/CNTs (b), and CoPc (c) at different potentials. Band intensity of key intermediates CO32- (d), *COOH (e), and *CO (f) formed on surface of CoPc/CNHs-3, CoPc/CNTs, CoPc, and CNHs catalysts.

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碳纳米角负载单分子分散酞菁钴限制质子转移增强酸性CO₂电还原制CO

Restricting proton transfer via carbon nanohorn-supported monomolecular cobalt phthalocyanine enhances CO₂-to-CO electrocatalysis in acidic media

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