原子级Mn掺入Co3O4用于纯水和稀释CO2条件下CO2选择性光还原

doi:10.1016/S1872-2067(25)64861-3

催化学报 ›› 2026, Vol. 81: 216-226.DOI: 10.1016/S1872-2067(25)64861-3

原子级Mn掺入Co₃O₄用于纯水和稀释CO₂条件下CO₂选择性光还原

周港华^a^,^b, 刘杰^a, 张龙云^a, 毕传周^a, 徐航敏^a, 姜为易^a, 朱兴旺^a(), 宁欣^a(), 许晖^c(), 王小治^a^,^d()

^a 扬州大学碳中和技术研究院, 环境科学与工程学院, 机械工程学院, 江苏扬州 225009, 中国
^b 南洋理工大学材料科学与工程学院, 新加坡, 新加坡
^c 江苏大学能源研究院环境与安全工程学院, 江苏镇江 212013, 中国
^d 江苏省固体有机废弃物资源化协同创新中心, 江苏南京 210095, 中国

收稿日期:2025-07-03 接受日期:2025-09-01 出版日期:2026-02-18 发布日期:2025-12-26
通讯作者: *电子信箱: zxw@yzu.edu.cn (朱兴旺),ningxin@yzu.edu.cn (宁欣),xh@ujs.edu.cn (许晖),xzwang@yzu.edu.cn (王小治).
基金资助:
国家自然科学基金(22308300);江苏省自然科学基金(BK20220598);江苏省政府留学奖学金

Atomic-level Mn incorporation into Co₃O₄ for selective CO₂ photoreduction in pure water under dilute CO₂ atmosphere

Ganghua Zhou^a^,^b, Jie Liu^a, Longyun Zhang^a, Chuanzhou Bi^a, Hangmin Xu^a, Weiyi Jiang^a, Xingwang Zhu^a(), Xin Ning^a(), Hui Xu^c(), Xiaozhi Wang^a^,^d()

^a School of Mechanical Engineering, College of Environmental Science and Engineering, Institute of Technology for Carbon Neutralization, Yangzhou University, Yangzhou 225009, Jiangsu, China
^b School of Materials Science and Engineering, Nanyang Technological University, 50 Nanyang Avenue, Singapore 639798, Singapore
^c School of the Environment and Safety Engineering, Institute for Energy Research, Jiangsu University, Zhenjiang 212013, Jiangsu, China
^d Jiangsu Collaborative Innovation Center for Solid Organic Waste Resource Utilization, Nanjing 210095, Jiangsu, China

Received:2025-07-03 Accepted:2025-09-01 Online:2026-02-18 Published:2025-12-26
Contact: *E-mail: zxw@yzu.edu.cn (X. Zhu),ningxin@yzu.edu.cn (X. Ning),xh@ujs.edu.cn (H. Xu),xzwang@yzu.edu.cn (X. Wang).
Supported by:
National Natural Science Foundation of China(22308300);Natural Science Foundation of Jiangsu Province(BK20220598);and the Jiangsu Government Scholarship for Overseas Studies

摘要/Abstract

摘要：

利用太阳能光催化技术驱动CO₂还原可实现太阳能到化学能的转化. 然而, 光催化技术的实际应用受到光催化剂及反应物分子自身局限性的制约, 包括高的光生载流子复合率、CO₂分子C=O键高的键解离能以及CO₂还原产物低的选择性等. 此外, 大多数已报道的光催化CO₂还原反应体系依赖高纯度CO₂原料气和额外添加剂的使用, 导致整体运行成本上升. 因此, 开发高性能的CO₂转化光催化剂并探讨其在绿色反应体系下(如纯水、稀释CO₂氛围)的选择性转化尤为重要.

本文以原位合成的Mn掺杂ZIF-67为前驱体, 采用“浸渍-热解”策略制备了Mn掺杂Co₃O₄(MMC)光催化剂. 基于MOF牺牲模板法有助于Mn在Co₃O₄晶格中的均匀掺入, 同时保持分级多孔结构, 从而增强催化活性位点的暴露并精细调控催化剂的电子性质. 首先评估了传统牺牲剂体系中的光催化CO₂还原反应(PCRR)性能. 在含三乙醇胺作为牺牲剂的PCRR体系中, 2 at%Mn掺杂的MOF衍生Co₃O4 (2MMC)催化剂10 h的CO生成速率(182.7 μmol g^-1 h^-1)是原始MOF衍生Co₃O₄ (MC)催化剂的12.8倍. 这一性能相较先前报道的PCRR工作具有竞争力. 当使用稀释CO₂作为原料气时, 2MMC的CO生成速率仍呈上升趋势, 并且未检测到CH₄. 这可能是由于稀释CO₂氛围中传质效率低, 抑制了关键反应中间体通过质子耦合电子转移(PCET)途径形成. 稳定性测试显示2MMC的CO产量在20 h光照下持续增加, 意味着其具有优异的耐久性. 在纯水、高浓度CO₂条件下, 2MMC的CO生成速率是MC催化剂的2.68倍, 同时CO选择性从85.6%升至97.6%. 而在稀释CO₂条件下, 2MMC的CO产率仍为MC的1.37倍. 此外, 2MMC在纯水反应体系中同样展现出良好的催化活性和耐久性. 基于密度泛函理论计算的态密度分析结果表明, 相较于原始MC, 更多的电子态穿过2MMC催化剂的费米能级, 表明客体Mn原子引入增强了MC的导电性, 这有利于加速界面电荷传输. 此外, 2MMC的d能带中心下移相比较MC, 表明2MMC催化剂表面与CO中间体的相互作用减弱, 这有利于产物CO从Mn活性位点脱附, 从而提升整体CO₂到CO转化效率及产物选择性. 原位辐照X-射线光电子能谱(XPS)结果表明, XPS Mn 2p峰在光照下向低结合能方向移动, 表明光生载流子更易在2MMC的Mn位点积累. 原位傅里叶变换红外光谱结果表明, 在光照下2MMC催化剂上观察到一系列对应于PCRR中间体的特征振动峰, 且随着光照延长而逐渐增强, 表面吸附中间体的逐步积累. 这反映了光生电子与吸附CO₂分子及质子在光照下发生强相互作用. 吉布斯自由能计算结果显示表明, 2MMC催化剂通过优化*CO₂与*CO中间体的形成能垒增强光催化CO₂转化和CO的选择性生成.

综上, 本文基于MOF牺牲模板制备了客体原子掺杂金属氧化物催化剂, 从原子水平揭示了金属氧化物电子结构调控PCRR机制, 为实现可持续的太阳能驱动碳资源利用提供了有前景的策略. 更多绿色可持续的PCRR反应体系值得在后续的研究中进一步被探讨.

关键词: 光催化, CO₂转化, 选择性还原, 金属氧化物, 一氧化碳

Abstract:

The photocatalytic carbon dioxide reduction represents a promising route for solar-to-chemical energy conversion, enabling the sustainable production of carbon-neutral fuels. Achieving high selectivity toward specific products remains a major challenge due to the complex multi-electron transfer pathways and competing reaction intermediates. Herein, the Mn-doped Co₃O₄ (MMC) photocatalysts are synthesized based on an “impregnation-pyrolysis” strategy using in situ synthesized Mn-doped ZIF-67 as a precursor. The MOF-templated approach enables uniform Mn incorporation into the Co₃O₄ lattice while preserving a hierarchical porous architecture, thereby enhancing active-site accessibility and modulating the electronic environment of catalyst. The introduction of guest Mn effectively suppresses the competing hydrogen evolution reaction. As a result, the optimized 2MMC catalyst shows a 12.8-fold increase in CO production over undoped Co₃O₄ and enables selective CO₂ conversion in pure water with diluted CO₂. Photoelectrochemical characterizations reveal that guest Mn doping accelerates charge separation dynamics. In-situ irradiated X-ray photoelectron spectroscopy, in-situ Fourier transformed infrared spectra, and theoretical calculations unveil a Mn-mediated pathway that selectively promotes the formation of *CO₂ and *CO intermediates. This work provides new atomic-level insights into the selective photocatalytic conversion of CO₂ under green and sustainable conditions.

Key words: Photocatalysis, CO₂ conversion, Selective reduction, Metal oxides, Carbon monoxide

周港华, 刘杰, 张龙云, 毕传周, 徐航敏, 姜为易, 朱兴旺, 宁欣, 许晖, 王小治. 原子级Mn掺入Co₃O₄用于纯水和稀释CO₂条件下CO₂选择性光还原[J]. 催化学报, 2026, 81: 216-226.

Ganghua Zhou, Jie Liu, Longyun Zhang, Chuanzhou Bi, Hangmin Xu, Weiyi Jiang, Xingwang Zhu, Xin Ning, Hui Xu, Xiaozhi Wang. Atomic-level Mn incorporation into Co₃O₄ for selective CO₂ photoreduction in pure water under dilute CO₂ atmosphere[J]. Chinese Journal of Catalysis, 2026, 81: 216-226.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64861-3

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图/表 6

Fig. 1. Synthesis, morphology, and structural characterization of prepared catalysts. (a) Illustration of synthesized MMC catalyst. SEM (b), HR-TEM (c) images, and SAED (d) of 2MMC. (e) HRTEM image of 2MMC. (f) Intensity profiles along the blue and red lines in (e). HAADF (g) and EDX elements mapping (h?j) of 2MMC. Calculated work function of MC (k) and 2MMC (l). (m) Differential charge density and Bader charge analyses based on DFT calculations.

Fig. 2. Surface composition and chemical states. (a) XRD patterns of the as-prepared catalysts. (b) Enlarged view of the dominant (311) crystal plane diffraction peak. (c) Raman spectra of the as-prepared catalysts. High-resolution XPS spectra of prepared catalysts: Co 2p (d), O 1s (e), and Mn 2p (f).

Fig. 3. PCRR performance evaluation. (a) The PCRR activity of MC and 2MMC catalysts in TEOA-containing systems using high-concentration and low-concentration CO2 as the feed gas. (b) The PCRR durability of the 2MMC catalyst in a TEOA-containing system using high- and low-concentration CO2 as the feed gas. (c) The PCRR activity of MC and 2MMC catalysts in a pure-water system using high-concentration and low-concentration CO2 as the feed gas. (d) The PCRR durability of the 2MMC catalyst in a pure-water system using high- and low-concentration CO2 as the feed gas.

Fig. 4. Evaluation of charge separation dynamics. EIS (a), transient photocurrent response (b), PL spectra (c), and TRPL spectra (d) of the as-prepared catalysts. Tafel curves of MC (e) and 2MMC (f) catalysts.

Fig. 5. Investigation of the surface properties of the catalyst. (a) N2 adsorption-desorption isotherms of MC and 2MMC. Pore size distribution plots of MC (b) and 2MMC (c). CO2 adsorption isotherms (d), Zeta potential (e), and CO2-TPD (f) of MC and 2MMC. (g) CA of as-prepared samples.

Fig. 6. Mechanism exploration. DOS for MC (a) and 2MMC (b). In-situ XPS Mn 2p spectrum (c) and in-situ FT-IR spectrum (d) of 2MMC. (e) Calculated Gibbs free energy of MC and 2MMC. (f) Proposed PCRR pathway.

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原子级Mn掺入Co₃O₄用于纯水和稀释CO₂条件下CO₂选择性光还原

Atomic-level Mn incorporation into Co₃O₄ for selective CO₂ photoreduction in pure water under dilute CO₂ atmosphere

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