构建MXene衍生TiO2/CoNiO2双位点S型异质结: 助力C-C偶联以实现高效光催化CO2转化为C2H4

doi:10.1016/S1872-2067(25)64866-2

催化学报 ›› 2026, Vol. 81: 227-245.DOI: 10.1016/S1872-2067(25)64866-2

构建MXene衍生TiO₂/CoNiO₂双位点S型异质结: 助力C-C偶联以实现高效光催化CO₂转化为C₂H₄

胡永盛^a, 杜史记^a^,^c, 郎集会^a^,^b, 刘恵莲^a^,^b, 李雪飞^a^,^b, 张旗^a^,^b, 鲁铭^a^,^c, 李鑫^a^,^b^,^c(), 李彬榕^d(), 魏茂彬^a^,^b(), 杨丽丽^a^,^b()

^a 吉林师范大学物理学院, 功能材料物理与化学教育部重点实验室, 吉林长春 130103
^b 吉林师范大学国家级物理实验教学示范中心, 吉林四平 136000
^c 吉林师范大学功能材料物理与化学教育部重点实验室, MAX/MXene材料联合实验室, 吉林长春 130103
^d 城市生活污水资源化利用技术国家地方联合工程实验室, 苏州科技大学环境科学与工程学院, 江苏苏州 215009

收稿日期:2025-07-20 接受日期:2025-09-18 出版日期:2026-02-18 发布日期:2025-12-26
通讯作者: *电子信箱: xlwl@jlnu.edu.cn (李鑫),libr@usts.edu.cn (李彬榕),jlsdzccw@126.com (魏茂彬),llyang1980@126.com (杨丽丽).
基金资助:
国家自然科学基金(22378158);国家自然科学基金(22306142);吉林省科学技术发展项目(YDZJ202301ZYTS246);吉林省科学技术发展项目(20230508040RC);吉林省科学技术发展项目(20240601047RC);吉林省中青年科技创新团队培养计划(20250601083RC);吉林省发展和改革委员会工业技术与发展计划(2023C44-4);吉林省教育厅科学技术处项目(JJKH20250941KJ);江苏省自然科学基金(BK20230656)

Rational construction of MXene-derived TiO₂/CoNiO₂ dual-site S-scheme heterojunction for boosting C-C coupling toward efficient photocatalytic CO₂-to-C₂H₄ conversion

Yongsheng Hu^a, Shiji Du^a^,^c, Jihui Lang^a^,^b, Huilian Liu^a^,^b, Xuefei Li^a^,^b, Qi Zhang^a^,^b, Ming Lu^a^,^c, Xin Li^a^,^b^,^c(), Binrong Li^d(), Maobin Wei^a^,^b(), Lili Yang^a^,^b()

^a Key Laboratory of Functional Materials Physics and Chemistry of Ministry of Education, Jilin Normal University, Changchun 130103, Jilin, China
^b National Demonstration Center for Experimental Physics Education, Jilin Normal University, Siping 136000, Jilin, China
^c The Joint Laboratory of MAX/MXene Materials, Key Laboratory of Functional Materials Physics and Chemistry of the Ministry of Education, Jilin Normal University, Changchun 130103, Jilin, China
^d National and Local Joint Engineering Laboratory of Municipal Sewage Resource Utilization Technology, School of Environmental Science and Engineering, Suzhou University of Science and Technology, Suzhou 215009, Jiangsu, China

Received:2025-07-20 Accepted:2025-09-18 Online:2026-02-18 Published:2025-12-26
Contact: *E-mail: xlwl@jlnu.edu.cn (X. Li),libr@usts.edu.cn (B. Li),jlsdzccw@126.com (M. Wei),llyang1980@126.com (L. Yang).
Supported by:
program for the National Natural Science Foundation of China(22378158);program for the National Natural Science Foundation of China(22306142);development of Science and Technology of Jilin province(YDZJ202301ZYTS246);development of Science and Technology of Jilin province(20230508040RC);development of Science and Technology of Jilin province(20240601047RC);Cultivation Programme for Young and Middle-aged Innovative Teams in Science and Technology of Jilin Province(20250601083RC);program for the Industrial Technology and Development of Jilin Province Development and Reform Commission(2023C44-4);program for the Science and Technology of Education Department of Jilin Province(JJKH20250941KJ);Jiangsu Provincial Natural Science Foundation(BK20230656)

摘要/Abstract

摘要：

乙烯(C₂H₄)作为重要的化工原料之一, 其传统生产方法主要依赖石油烃类裂解, 消耗不可再生能源的同时, 还伴随大量碳排放. 而光催化CO₂还原(CO₂RR)转化C₂H₄技术, 既能实现温室气体CO₂的资源化利用, 又能够在温和条件下实现C₂H₄的制备. 该技术仍面临两大挑战: 其一是由于*C1中间体间存在过高的C-C偶联能垒, 导致产物多以C1产物形式解吸, 从而限制了C2+产物的生成; 其二是电子(e^-)和质子(H⁺)供应动力学缓慢. C₂H₄的光催化生成是一个多步过程, 涉及复杂的质子耦合电子转移(PCET)过程. 因此, 快速的e^-和H⁺产生与供给是实现高效CO₂RR的关键因素之一. 然而, 过快的载流子复合与较高的界面传输能垒直接影响着催化剂的CO₂RR速率.

针对上述分析, 本研究设计了一种由MXene衍生TiO₂ (MT)和CoNiO₂ (CNO)构成的TiO₂/CoNiO₂ (MTC) S型异质结体系. 该设计的核心思想在于: 利用CNO本征的Co-Ni邻位异核双原子位点来降低C-C偶联的能垒, 同时构建S型异质结以克服CNO自身光生载流子复合率高、H₂O氧化能力弱的不足, 从而进一步提升C-C偶联速率. 结果表明, Co-Ni双位点与S型异质结之间的协同作用有效促进了CO₂向C₂H₄的高选择性还原. 实验发现, MTC-2(理论质量比为10:1)样品表现出最优的CO₂光还原制C₂H₄性能: 在紫外-可见光光照条件下, 其C₂H₄产率达到25.2 μmol/(g·h), 相较于纯CoNiO₂催化剂提升约23倍. 同时, MTC-2对C₂H₄的选择性高达59.4%, 该样品展现出优异的催化活性与产物选择性. 结合光电化学测试、原位X射线光电子能谱、原位开尔文探针显微镜、飞秒瞬态吸收光谱以及差分电荷密度计算, 验证了MTC-2复合物界面间S型异质结的成功构建. 通过原位傅里叶变换红外光谱和吉布斯自由能计算, 确定了*COCOH转化*CCO是CO₂RR转化C₂H₄的限速步骤, 从理论层面阐明了Co-Ni双位点结构与S型异质结协同促进C-C偶联动力学过程的增强机制.

综上, 本研究通过Co-Ni双位点配合S型异质结的协同策略, 成功优化了CO₂RR转化C₂H₄过程中C-C偶联能垒高与电子、质子供给效率低的关键问题, 不仅提供了一种高性能MTC-2催化剂的制备方法, 更通过系统的表征与理论计算, 揭示了Co-Ni双位点与S型异质结协同增强C-C偶联效率的作用规律, 为设计具有高活性、高选择性的CO₂光还原制C₂H₄催化体系提供了新的实验参考与理论依据.

关键词: 光还原二氧化碳, 镍酸钴, Ti₃C₂ MXene, S型异质结

Abstract:

The CO₂ photoreduction reaction (CO₂RR) into C₂H₄represents a highly promising technology for converting greenhouse gases into value-added chemicals. However, this technology faces challenges such as a high energy barrier in the C-C coupling process and a slow electron supply efficiency. In this study, we constructed Ti₃C₂ MXene-derived TiO₂/CoNiO₂ S-scheme heterojunction (MTC-X) by a simple in-situ growth process. The Co-Ni dual-site provided the structural foundation for C-C coupling, effectively reducing the energy barrier of the *CO-*COH intermediate coupling step. Meanwhile, the S-scheme heterojunction ensured the rapid supply of electrons and protons during the CO₂RR, thereby enabling the efficient conversion of CO₂ to C₂H₄. Notably, the MTC-2 sample exhibited the C₂H₄ production rate of 25.2 μmol·g^-1·h^-1, which was 23 times higher than that of the pure CoNiO₂. In summary, by combining in-situ X-ray photoelectron spectroscopy, in-situ Kelvin probe force microscopy, femtosecond transient absorption spectroscopy and difference charge density calculation, confirmed the formation of the TiO₂/CoNiO₂ S-scheme heterojunction. Further, by photoelectrochemical tests, in-situ Fourier transform infrared spectroscopy, Gibbs free-energy calculations, elucidated the mechanism by which the Co-Ni dual-site structure and S-scheme heterojunction synergistically enhance the C-C coupling kinetic process. This provides new experimental reference and theoretical basis for the selective conversion of CO₂ to C₂H₄.

Key words: CO₂ photoreduction, CoNiO₂, Ti₃C₂ MXene, S-scheme heterojunction

胡永盛, 杜史记, 郎集会, 刘恵莲, 李雪飞, 张旗, 鲁铭, 李鑫, 李彬榕, 魏茂彬, 杨丽丽. 构建MXene衍生TiO₂/CoNiO₂双位点S型异质结: 助力C-C偶联以实现高效光催化CO₂转化为C₂H₄[J]. 催化学报, 2026, 81: 227-245.

Yongsheng Hu, Shiji Du, Jihui Lang, Huilian Liu, Xuefei Li, Qi Zhang, Ming Lu, Xin Li, Binrong Li, Maobin Wei, Lili Yang. Rational construction of MXene-derived TiO₂/CoNiO₂ dual-site S-scheme heterojunction for boosting C-C coupling toward efficient photocatalytic CO₂-to-C₂H₄ conversion[J]. Chinese Journal of Catalysis, 2026, 81: 227-245.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64866-2

https://www.cjcatal.com/CN/Y2026/V81/I2/227

图/表 10

Scheme 1. The synthesized steps of MTC-X S-scheme heterojunction.

Fig. 1. (a) XRD images of MT, MTC-2 and CNO. (b) Survey XPS spectra of MT CNO and MTC-2. XPS spectra of MT, CNO and MTC-2 of Co 2p (c), Ni 2p (d). XPS spectra of MT and MTC-2 of O 1s (e) and Ti 2p (f).

Fig. 2. (a) Normalized Co K-edge XANES spectra. (b) Normalized Ni K-edge XANES spectra. (c) FT-EXAFS spectra of Co K-edge and Ni K-edge. WT-EXAFS of Co K-edge for Co foil (d), MTC-2 (e), and Co3O4 references (f). WT-EXAFS of Ni K-edge for Ni foil (g), MTC-2 (h), and NiO references (i).

Fig. 3. SEM (a), TEM (b), HRTEM (c) images of MT and lattice spacing analysis of MT (c1). SEM (d), TEM (e), HRTEM (f) images of CNO and lattice spacing analysis of CNO (f1). SEM (g), TEM (h), HRTEM (i) images of MTC-2 and lattice spacing analysis of MTC-2 (i1-i2). (j1-j4) Elemental mapping images of (j) MTC-2.

Fig. 4. (a) CO, CH4, C2H4 and C2H6 yield with prepared samples. (b) Cyclic CO2 photoreduction results of C2H6. (c) Electron utilization efficiency. (d) C2H6 selectivity of the prepared sample. (e) Mass spectrometric analysis of the products from conventional CO2 reduction. (f) Product analysis of CO2 photoreduction using isotope-labeled 13CO2. (g) Comparison of C2H4 production performance with other reported CO2RR catalysts.

Fig. 5. In-situ FTIR of CNO (a) and MTC (b). (c) Gibbs free energy pathway of DFT calculation for CO2RR to *CO and *COH of MTC-2 and CNO. (d) Gibbs free energy pathway of DFT calculation for CO2RR to C2H4 of MTC-2 and CNO. (e) Reaction pathway and chemical structures of intermediates during CO2RR to *CO and *COH. (f) Reaction pathway and chemical structures of intermediates during CO2RR to C2H4.

Fig. 6. (a) UV-vis DRS spectra of CNO, MTC-2 and MT. (b) Transient photocurrent response curve. (c) Electrochemical impedance spectroscopy. (d) PL spectra. (e) TR-PL spectra and attenuation constant (τ). (f) TPV relaxation curves of CNO, MTC-2 and MT. (g) Attenuation constants (τ) of CNO, MTC-2 and MT. (h) Maximum charge extraction time (tmax) of CNO, MTC-2 and MT. (i) Charge extraction efficiency of CNO, MTC-2 and MT.

Fig. 7. In-situ XPS analysis of MTC-2 under reaction conditions: Co 2p (a), Ni 2p (b), Ti 2p (c), and O 1s (d). (e,f) Mechanism diagram of KPFM measurement. AFM images of CNO (g), MT (h) and MTC-2 (i). (j,k) VCPD of CNO and MT in dark along the marked line of (g,h). (l) VCPD of MTC-2 in the different light times along the marked line of (i).

Fig. 8. (a) TA spectra signals of CNO. (b) 2D mapping TA spectra of CNO. (c) TA spectra signals of MTC-2. (d) 2D mapping TA spectra of MTC-2. (e) Normalized decay kinetic curves of CNO. (f)Normalized decay kinetic curves of MTC-2. Schematics for the decay pathways of photogenerated electrons in CNO (g) and MTC-2 (h) composite.

Fig. 9. (a) UPS spectra of CNO and MT. (b) The band gaps of MT and CNO. Work function of MT (c) and CNO (d). (e)Three-dimensional charge density difference distribution (the yellow and cyan regions represent electron accumulation and depletion). (f) Plane-averaged charge density difference along the Z direction. (g) Schematic illustration of heterojunction formation dynamics and interfacial charge transfer mechanism.

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构建MXene衍生TiO₂/CoNiO₂双位点S型异质结: 助力C-C偶联以实现高效光催化CO₂转化为C₂H₄

Rational construction of MXene-derived TiO₂/CoNiO₂ dual-site S-scheme heterojunction for boosting C-C coupling toward efficient photocatalytic CO₂-to-C₂H₄ conversion

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