S型CuInS2@CoS2异质结促进电荷转移以实现高效光催化CO2还原

doi:10.1016/S1872-2067(24)60066-5

催化学报 ›› 2024, Vol. 63: 190-201.DOI: 10.1016/S1872-2067(24)60066-5

S型CuInS₂@CoS₂异质结促进电荷转移以实现高效光催化CO₂还原

王福林^a^,¹, 李祥伟^a^,¹, 卢康强^a, 周漫^b^,^*(), 余长林^c^,^*(), 杨凯^a^,^*()

^a江西理工大学化学化工学院, 江西赣州 341000
^b赣南医科大学药学院, 江西赣州 341000
^c广东石油化工学院化学工程学院, 广东茂名 525000

收稿日期:2024-04-24 接受日期:2024-06-02 出版日期:2024-08-18 发布日期:2024-08-19
通讯作者: *电子信箱: yangkai@jxust.edu.cn (杨凯),baiyuwawa-zhouman@163.com (周漫),yuchanglinjx@163.com (余长林).
作者简介:
¹共同第一作者.
基金资助:
国家自然科学基金(22366018);国家自然科学基金(5236005);国家自然科学基金(22272034);江西省自然科学基金重点项目(20232ACB203022);江西省自然科学基金重点项目(20224ACB213010);江西双千人才培养计划(jxsq2023201086);江西双千人才培养计划(jxsq2023102141);江西双千人才培养计划(jxsq2023102142);江西双千人才培养计划(jxsq2023102143);江西理工大学清江拔尖人才计划(JXUSTQJBJ2020005);江西省自然科学基金(20224BAB203018);江西省研究生创新专项基金项目(YC2022-S659)

Molten salt construction of core-shell structured S-scheme CuInS₂@CoS₂ heterojunction to boost charge transfer for efficient photocatalytic CO₂ reduction

Fulin Wang^a^,¹, Xiangwei Li^a^,¹, Kangqiang Lu^a, Man Zhou^b^,^*(), Changlin Yu^c^,^*(), Kai Yang^a^,^*()

^aSchool of Chemistry and Chemical Engineering, Jiangxi University of Science and Technology, Ganzhou 341000, Jiangxi, China
^bSchool of Pharmacy, Gannan Medical University, Ganzhou 341000, Jiangxi, China
^cSchool of Chemical Engineering, Key Laboratory of Petrochemical Pollution Process and Control, Guangdong Province, Guangdong University of Petrochemical Technology, Maoming 525000, Guangdong, China

Received:2024-04-24 Accepted:2024-06-02 Online:2024-08-18 Published:2024-08-19
Contact: *E-mail: yangkai@jxust.edu.cn (K. Yang), baiyuwawa-zhouman@163.com (M. Zhou), yuchanglinjx@163.com (C. Yu).
About author:
¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22366018);National Natural Science Foundation of China(5236005);National Natural Science Foundation of China(22272034);Key Projects of Jiangxi Provincial Natural Science Foundation(20232ACB203022);Key Projects of Jiangxi Provincial Natural Science Foundation(20224ACB213010);Jiangxi Province “Double Thousand” Talent Training Plan(jxsq2023201086);Jiangxi Province “Double Thousand” Talent Training Plan(jxsq2023102141);Jiangxi Province “Double Thousand” Talent Training Plan(jxsq2023102142);Jiangxi Province “Double Thousand” Talent Training Plan(jxsq2023102143);Program of Qingjiang Excellent Young Talents, JXUST(JXUSTQJBJ2020005);Jiangxi Provincial Natural Science Foundation(20224BAB203018);Jiangxi Province Graduate Innovation Special Fund Project(YC2022-S659)

摘要/Abstract

摘要：

利用太阳能将CO₂和H₂O转化为CO, CH₄和CH₃OH等碳基燃料是一种清洁和可持续技术. 然而, 较弱的氧化还原能力和严重的电荷重组阻碍了CO₂光还原技术的实际应用. 为应对该挑战, 多组分体系的构建是提高光催化性能的最有效途径之一. 近年来, S型异质结受到研究人员的广泛关注, 为复合体系的光催化剂提供了新的发展方向. S型异质结通常由具有更负的导带(CB)电位的还原型半导体(RP)和具有更正的价带(VB)电位的氧化型半导体(OP)组成. 在S型异质结中, 强内建电场的存在驱动电子和空穴分别在RP的CB和OP的VB上积累. 这种积累克服了II型异质结氧化还原能力弱的缺点, 并且有效改善了单个半导体电子-空穴对快速复合和光吸收范围有限的问题. 因此, 构建匹配良好的S型异质结构和建立强大的内建电场是提高CO₂光转换效率的重要策略.

本文通过两步熔盐法设计合成了核壳结构的CuInS₂@CoS₂(CIS-CS) S型异质结光催化剂. 熔盐法不仅有利于高结晶CuInS₂的形成, 使CuInS₂与CoS₂充分接触, 实现电子高效转移, 还可以为光催化CO₂还原提供更多的比表面积和活性位点. 合成的CuInS₂@CoS₂异质结构表现出较好的CO₂光还原性能, 光照2 h下CO的产率为239 μmol g^‒1 h^‒1, 分别是纯CuInS₂和CoS₂的21.7倍和26.5倍. X射线粉末衍射、扫描电镜、透射电镜和氮气等温吸附脱附曲线等表征测试证明了CuInS₂@CoS₂复合材料的结构特征. 采用光电化学测试、光致发光光谱和时间分辨光致发光光谱研究了催化剂的载流子分离和重组行为. 原位光照X射线光电子能谱和功函数计算证明了异质结符合S型电荷转移机制, 开尔文探针力显微镜证明了异质结具有更大的内建电场强度. 在黑暗条件下, 由于CoS₂和CuInS₂在界面上的费米能级存在差异, 当两种材料复合时, 电子会自发地从CoS₂迁移到CuInS₂, 直到费米能级达到平衡, 从而在复合材料的界面处产生了强内建电场. 在光照下, 电子由CuInS₂转移到CoS₂, 内建电场的存在诱导了电荷的定向迁移使得光生载流子能够有效分离, 从而提高了CuInS₂@CoS₂异质结的光催化活性. 此外, 原位光照傅里叶变换红外光谱研究了光催化CO₂还原反应的中间体, 并进一步通过密度泛函理论计算证实了CuInS₂@CoS₂异质结降低了*COOH和*CO的形成能.

综上, 通过两步熔融盐法成功合成了CuInS₂@CoS₂(CIS-CS) S型异质结光催化剂. S型异质结构的形成有效增强了材料的内建电场, 并促进光生载流子的高效分离和转移, 从而获得了优异的光催化CO₂还原为CO的性能. 本文为通过熔盐方法设计合成S型异质结光催化剂提供了参考.

关键词: S型异质结, 熔融盐, CuInS₂, CoS₂, CO₂光还原

Abstract:

Weak redox ability and severe charge recombination pose significant obstacles to the advancement of CO₂ photoreduction. To tackle this challenge and enhance the CO₂ photoconversion efficiency, fabricating well-matched S-scheme heterostructure and establishing a robust built-in electric field emerge as pivotal strategies. In pursuit of this goal, a core-shell structured CuInS₂@CoS₂ S-scheme heterojunction was meticulously engineered through a two-step molten salt method. This approach over the CuInS₂-based composites produced an internal electric field owing to the disparity between the Fermi levels of CoS₂ and CuInS₂ at their interface. Consequently, the electric field facilitated the directed migration of charges and the proficient separation of photoinduced carriers. The resulting CuInS₂@CoS₂ heterostructure exhibited remarkable CO₂ photoreduction performance, which was 21.7 and 26.5 times that of pure CuInS₂ and CoS₂, respectively. The S-scheme heterojunction photogenerated charge transfer mechanism was validated through a series of rigorous analyses, including in situ irradiation X-ray photoelectron spectroscopy, work function calculations, and differential charge density examinations. Furthermore, in situ infrared spectroscopy and density functional theory calculations corroborated the fact that the CuInS₂@CoS₂ heterojunction substantially lowered the formation energy of *COOH and *CO. This study demonstrates the application potential of S-scheme heterojunctions fabricated via the molten salt method in the realm of addressing carbon-related environmental issues.

Key words: S-scheme heterojunction, Molten salt, CuInS₂, CoS₂, CO₂photoreduction

王福林, 李祥伟, 卢康强, 周漫, 余长林, 杨凯. S型CuInS₂@CoS₂异质结促进电荷转移以实现高效光催化CO₂还原[J]. 催化学报, 2024, 63: 190-201.

Fulin Wang, Xiangwei Li, Kangqiang Lu, Man Zhou, Changlin Yu, Kai Yang. Molten salt construction of core-shell structured S-scheme CuInS₂@CoS₂ heterojunction to boost charge transfer for efficient photocatalytic CO₂ reduction[J]. Chinese Journal of Catalysis, 2024, 63: 190-201.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60066-5

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图/表 6

Scheme 1. Schematic illustration of the synthesis procedure for CuInS2@CoS2.

Fig. 1. (a) XRD patterns of all samples. (b) Enlarged spectra of the region enclosed by green rectangle in (a). (c) FT-IR spectra of all samples. SEM images of CoS2 (d), CuInS2 (e), and CIS-CS (40) (f). TEM (g) and HRTEM (h) images of CIS-CS(40). (i) Elemental distribution mappings of CIS-CS(40).

Fig. 2. (a) (αhν)2 vs. hν plot of CoS2 and CuInS2. (b) Mott-Schottky plot of CoS2. (c) Mott-Schottky plot of CuInS2. (d) Energy band structure of CuInS2 and CoS2. (e) Surface potential of CuInS2. (f) Surface potential of CIS-CS(40). (g) Transient photocurrents of the samples. (h) Steady-state fluorescence spectra of samples. (i) Contact angle between the sample surface and reaction solution.

Fig. 3. (a) Product yields of CuInS2, CoS2, and CIS-CS (40). (b) Photocatalytic CO2 activity diagram of all samples. (c) Photocatalytic experiments under various conditions. (d) Mass spectrum of products obtained using 13CO2 instead of CO2. (e) Performance cycling tests of CIS-CS (40). (f) XRD patterns before and after the reaction over CIS-CS(40).

Fig. 4. Density of states of CoS2 (a), CuInS2 (b), and CIS-CS(40) (c). Work functions over CoS2 (d) and CuInS2 (e). (f) CIS-CS(40) differential charge density diagram. Cu 2p (g), In 3d (h), S 2p (i) XPS spectra of the samples.

Fig. 5. In situ FT-IR spectra (a) and the corresponding 3D color mapping surface with projection (b) over CIS-CS(40). (c) Reaction energy barrier of CO2 reduction on CoS2, CuInS2, and CIS-CS(40). (d) S-scheme heterojunction charge transfer path.

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S型CuInS₂@CoS₂异质结促进电荷转移以实现高效光催化CO₂还原

Molten salt construction of core-shell structured S-scheme CuInS₂@CoS₂ heterojunction to boost charge transfer for efficient photocatalytic CO₂ reduction

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