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

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

Chinese Journal of Catalysis ›› 2026, Vol. 81: 227-245.DOI: 10.1016/S1872-2067(25)64866-2

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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)

Abstract

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·h), 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

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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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(25)64866-2

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Figures/Tables 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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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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