缺陷介导的Zn-CuInS2双位点协同催化: 轨道调控实现高效光催化CO2转化制乙烯

doi:10.1016/S1872-2067(26)65022-X

催化学报 ›› 2026, Vol. 85: 153-167.DOI: 10.1016/S1872-2067(26)65022-X

缺陷介导的Zn-CuInS₂双位点协同催化: 轨道调控实现高效光催化CO₂转化制乙烯

赖可溱^a, 孙雨鑫^a, 李林萍^a, 施晓庆^a, 周小松^c, 李宁^a, 高旸钦^a^,^b, 戈磊^a^,^b()

^a 中国石油大学(北京)新能源与材料学院, 重质油加工国家重点实验室, 北京 102249
^b 东营国安化工有限公司, 山东东营 257400
^c 岭南师范学院化学化工学院, 广东湛江 524048

收稿日期:2025-09-08 接受日期:2025-12-10 出版日期:2026-06-18 发布日期:2026-05-18
通讯作者: *电子信箱: gelei08@sina.com/gelei@cup.edu.cn (戈磊).
基金资助:
国家自然科学基金(52473327);国家自然科学基金(51572295);国家自然科学基金(21273285);国家重点研发计划(2021YFA1501300);国家重点研发计划(2019YFC1907602)

Defect-mediated dual-site synergy in Zn-CuInS₂ enables orbital-tailored high performance photocatalytic CO₂-to-ethylene conversion

Kezhen Lai^a, Yuxin Sun^a, Linping Li^a, Xiaoqing Shi^a, Xiaosong Zhou^c, Ning Li^a, Yangqin Gao^a^,^b, Lei Ge^a^,^b()

^a State Key Laboratory of Heavy Oil Processing, College of New Energy and Materials, China University of Petroleum Beijing, Beijing 102249, China
^b Dongying Guoan Chemical Co., Ltd, Circular Economy Industrial Park, Dongying 257400, Shandong, China
^c School of Chemistry and Chemical Engineering, Lingnan Normal University, Zhanjiang 524048, Guangdong, China

Received:2025-09-08 Accepted:2025-12-10 Online:2026-06-18 Published:2026-05-18
Contact: *E-mail: gelei08@sina.com/gelei@cup.edu.cn (L. Ge).
Supported by:
National Natural Science Foundation of China(52473327);National Natural Science Foundation of China(51572295);National Natural Science Foundation of China(21273285);National Key R&D Program of China(2021YFA1501300);National Key R&D Program of China(2019YFC1907602)

摘要/Abstract

摘要：

利用光催化技术将二氧化碳(CO₂)转化为高附加值燃料, 是实现碳中和目标的关键路径之一. 在众多产物中, 乙烯(C₂H₄)等C2产物因其工业应用价值而备受关注. 但该过程面临着CO₂分子难以活化, 多电子转移动力学过程缓慢, 以及C-C偶合能垒高等诸多挑战. 传统的催化剂因活性位点结构单一, 难以同时调控CO₂活化与C-C耦合这两个关键过程, 限制了C2产物的生成. CuInS₂材料因天然具备双金属位点及优异的可见光响应性能而被视为生成C2产物的潜在候选材料, 但依然存在光生载流子复合率高, 产物选择性差等问题. 因此, 采用原子掺杂与缺陷工程相结合的手段, 协同调控活性位点的几何构型和电子结构, 是突破C₂H₄产物选择性瓶颈的关键.

本文通过一步溶剂热法成功构筑了具有自发形成硫空位(S_v)的Zn掺杂CuInS₂(Zn-CIS)光催化剂, 揭示了Zn掺杂诱导S_v形成并协同构建Cu-Zn双活性位点的作用机制. X-射线衍射和高分辨透射电镜证明Zn²⁺优先取代In³⁺位点, 导致显著的晶格收缩. 密度泛函理论计算表明, 这种取代引起了体系电荷不平衡, 从而通过热力学自发的电荷补偿形成了S_v. S_v作为浅施主缺陷, 使费米能级显著上移0.375 eV, 增强了材料的n型半导体特性与整体还原能力, 并提升了光生载流子的分离与传输效率. Bader电荷分析与X-射线吸收近边结构谱共同证实了电子从S_v向邻近Zn位点的转移. 扩展边X-射线吸收精细结构谱则表明, Zn-S键长缩短且配位数约为3, 为Zn掺杂促进S_v形成提供了关键结构证据. 结合原位漫反射傅立叶变换红外光谱和吉布斯自由能计算, 明确了CO₂制乙烯的反应路径为*CO₂ → *COOH → *CO → *CHO → *COCHO → C₂H₄. 同时, 理论计算从原子尺度揭示了Zn和Cu双位点协同活化机制. Zn掺杂产生了相邻的Cu-Zn双位点, 将C-C耦合位点间距从3.97 Å缩短至2.60 Å, CO₂分子通过Cu-C (1.96 Å)与Zn-O (1.90 Å)键强化学吸附于Cu-Zn双位点, 导致显著弯曲(O-C-O键角122.3°)及C-O键不对称拉长(1.23和1.34 Å)而实现高效活化. 态密度分析进一步从电子层面阐明, S_v引起的电荷重分布使邻近Zn位点由电子受体转为电子给体, 其激活的Zn 3d轨道与CO₂成键轨道耦合(4σ/1π), 同时, Cu的3d轨道与CO₂的2π*反键轨道产生d-p杂化. 这两种协同作用共同促进了CO₂的吸附与活化. 这种“缺陷介导的轨道调控”使速决步的能垒降低了0.41 eV, 促进了高效的*CO → *CHO → *COCHO二聚化, 使C₂H₄产率相较于CuInS₂提高了5.9倍, 达到15.9 μmol g^-1 h^-1, 且C₂H₄的电子选择性为77.5%.

综上, 本研究通过缺陷介导的双位点工程, 实现了光催化CO₂向乙烯的高效高选择性转化, 且从轨道层面阐明了Zn掺杂与硫空位协同促进CO₂活化与C-C偶联的机制, 为太阳能碳资源转化及碳中和目标推进提供助力.

关键词: 光催化CO₂还原, Zn掺杂CuInS₂, 硫空位, C-C偶联

Abstract:

The photocatalytic conversion of CO₂ into high-value fuels represents a promising strategy for achieving carbon neutrality by utilizing solar energy. Overcoming kinetic barriers in multi-electron transfer and C-C coupling is critical for photocatalytic CO₂-to-C₂H₄ conversion. Herein, Zn-doped CuInS₂ (Zn-CIS) with spontaneously generated sulfur vacancies (S_v) was designed and constructed for highly selective photocatalytic CO₂ reduction. Experimental and density functional theory studies reveal that Zn²⁺ preferentially substitutes In³⁺ sites, inducing S_v formation via charge compensation. S_v acts as an electron reservoir, elevating the Fermi level (E_f) by 0.375 eV and prolonging lifetime of photogenerated charge carriers. Moreover, Zn²⁺ substitution creates adjacent Cu-Zn dual sites with a 2.60 Å spacing, enabling an asymmetric coordination where CO₂ bonds via Cu-C and Zn-O interactions. Furthermore, S_v-mediated charge redistribution activates the Zn 3d orbitals, driving their coupling with the CO₂ bonding orbitals (4σ/1π), which synergizes with Cu 3d-CO₂ 2π* antibonding hybridization and promotes the adsorption and activation of CO₂molecules. This dual-site synergy reduces the energy barrier of the rate-determining step by 0.41 eV and drives efficient *CO → *CHO → *COCHO dimerization, resulting in a 15.9 μmol g^-1 h^-1 C₂H₄ yield, 5.9-fold enhancement with 77.5% electron selectivity. This work highlights the effectiveness of defect-mediated dual-site engineering, coupled with orbital-level insights, facilitating efficient C2 product formation and provides a new paradigm for solar-driven carbon resource conversion.

Key words: Photocatalytic CO₂ reduction, Zn-doped CuInS₂, Sulfur vacancies, C-C coupling

赖可溱, 孙雨鑫, 李林萍, 施晓庆, 周小松, 李宁, 高旸钦, 戈磊. 缺陷介导的Zn-CuInS₂双位点协同催化: 轨道调控实现高效光催化CO₂转化制乙烯[J]. 催化学报, 2026, 85: 153-167.

Kezhen Lai, Yuxin Sun, Linping Li, Xiaoqing Shi, Xiaosong Zhou, Ning Li, Yangqin Gao, Lei Ge. Defect-mediated dual-site synergy in Zn-CuInS₂ enables orbital-tailored high performance photocatalytic CO₂-to-ethylene conversion[J]. Chinese Journal of Catalysis, 2026, 85: 153-167.

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图/表 6

Fig. 1. (a) Schematic diagram of the synthesis route of Zn-CuInS2. XRD patterns (b), enlarged XRD patterns (c), and ESR spectra (d) of the as-prepared catalysts. (e) The interplanar spacing of CuInS2 and 3Zn-CIS. TEM images of CuInS2 (f) and 3Zn-CIS (h). HRTEM images of CuInS2 (g) and 3Zn-CIS (i). (j) Element mapping of 3Zn-CIS.

Fig. 2. (a) The formation energy of Sv at different sites in the Zn-CIS model. (b) The Wf of CuInS2, Zn-CIS without Sv and Zn-CIS with Sv. (c) Bader charge visualization model of Zn-CIS without Sv and Zn-CIS with Sv. Surface potential under dark and light irradiation and corresponding KPFM images of CuInS2 (d-f) and 3Zn-CIS (g-i).

Fig. 3. XPS spectra of Cu 2p (a), In 3d (b), S 2p (c) and Zn 2p (d). (e) Normalized XANES spectra at the Zn K-edge of the Zn foil, ZnS and 3Zn-CIS. (f) Magnitude of Fourier transforms of the k2-weighted Zn K-edge EXAFS spectra. k2-weighted Zn K-edge EXAFS spectra (g), the wavelet-transformed EXAFS data of Zn foil (h), ZnS (i), and 3Zn-CIS (j).

Fig. 4. Gas generation rate (a) and electron selectivity (b) of CuInS2 and Zn-CIS. (c) Cyclic stability tests of 3Zn-CIS. (d) Electron selectivity using recycled 3Zn-CIS. (e) Control experiments for photocatalytic CO2 reduction over 3Zn-CIS. (f) mass spectrometry spectrum of 13CO2 isotope experiments on 3Zn-CIS (the insert picture is the zoomed-in part with a pink dashed frame). (g) EIS of CuInS2 and Zn-CIS. Transient photocurrent (h) and TRPL spectra (i) of CuInS2 and 3Zn-CIS.

Fig. 5. (a) In-situ DRIFTS spectra of 3Zn-CIS. CO2 adsorption model, differential charge and bader charge of CuInS2 (b) and Zn-CIS (c) (the electron-density isosurface was plotted at 0.0004 e Å-3 for CuInS2 and 0.004 e Å-3 for Zn-CIS, the pink and green zones indicate electron accumulation and depletion, respectively). CO adsorption model of CuInS2 on In atom (d) and Cu atom (e). CO adsorption model of Zn-CIS on Zn atom (f) and Cu atom (g). (h) ∆G plot of *CO conversion. (i) Proposed reaction pathway for photocatalytic CO2RR to C2H4 in Zn-CIS. (j) ΔG plot of CuInS2 and Zn-CIS.

Fig. 6. (a) COHP and ICOHP of Cu-C in CuInS2, Zn-CIS without Sv and Zn-CIS with Sv. (b) COHP and ICOHP of In-O in CuInS2, Zn-O in Zn-CIS without Sv and Zn-CIS with Sv. (c) DOS of free CO2 molecule, CO2 absorbed on CuInS2 and Zn-CIS. (d) d-band center of Zn-CIS without Sv and Zn-CIS with Sv.

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缺陷介导的Zn-CuInS₂双位点协同催化: 轨道调控实现高效光催化CO₂转化制乙烯

Defect-mediated dual-site synergy in Zn-CuInS₂ enables orbital-tailored high performance photocatalytic CO₂-to-ethylene conversion

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