ZnIn2S4/MOF-808微球结构S型异质结光催化剂的制备及其光还原CO2性能研究

doi:10.1016/S1872-2067(23)64480-8

催化学报 ›› 2023, Vol. 51: 180-192.DOI: 10.1016/S1872-2067(23)64480-8

ZnIn₂S₄/MOF-808微球结构S型异质结光催化剂的制备及其光还原CO₂性能研究

宋明明, 宋相海, 刘鑫, 周伟强(), 霍鹏伟()

江苏大学化学化工学院, 绿色化学与化工技术研究院, 江苏镇江212013

收稿日期:2023-04-13 接受日期:2023-06-15 出版日期:2023-08-18 发布日期:2023-09-11
通讯作者: *电子信箱: wqzhou@ujs.edu.cn (周伟强), huopw@ujs.edu.cn (霍鹏伟).
基金资助:
国家自然科学基金(22078131);国家自然科学基金(22108102);镇江市科技规划社会发展项目(SH2021013);江苏省青年学者基金(BK20210782);中国博士后科学基金奖学金获得者(2022M720057)

Enhancing photocatalytic CO₂ reduction activity of ZnIn₂S₄/MOF-808 microsphere with S-scheme heterojunction by in situ synthesis method

Mingming Song, Xianghai Song, Xin Liu, Weiqiang Zhou(), Pengwei Huo()

Institute of Green Chemistry and Chemical Technology, School of Chemistry & Chemical Engineering, Jiangsu University, Zhenjiang 212013, Jiangsu, China

Received:2023-04-13 Accepted:2023-06-15 Online:2023-08-18 Published:2023-09-11
Contact: *E-mail: wqzhou@ujs.edu.cn (W. Zhou), huopw@ujs.edu.cn (P. Huo).
Supported by:
National Natural Science Foundation of China(22078131);National Natural Science Foundation of China(22108102);Science and Technology Planning Social Development Project of Zhenjiang City(SH2021013);Jiangsu Provincial Founds for Young Scholars(BK20210782);Fellowship of China Postdoctoral Science Foundation(2022M720057)

摘要/Abstract

摘要：

近年来,能源过度消耗导致的温室效应引起人们广泛关注.通过不同半导体材料间能带交错排列构建异质结,用于将CO₂转化为高附加值产品是解决该问题的可行方法之一.其中,S型异质结的还原型光催化剂与氧化型光催化剂具有交错带结构,使各自存在的弱空穴与弱电子复合,极大提高光生载流子的透过率和电荷利用率,有效实现强电子-空穴对分离.
在半导体中,ZnIn₂S₄由于能带结构适当、可见光响应范围广和化学性质稳定等优点,在CO₂减排领域表现出较好的性能.但其光吸收能力低、光生载流子分离效率低和光生电子的迁移过程缓慢,这些缺点导致单一ZnIn₂S₄在光催化领域的应用受限.在目前半导体研究中,MOF-808制备方法简单、比表面积大以及框架结构稳定,是一种理想的催化材料.因此,本文利用MOF-808与ZnIn₂S₄偶联形成合适的交错带结构,构建S型异质结以提高光催化CO₂还原活性.
本文采用原位合成法设计由三维花球ZnIn₂S₄和八面体MOF-808组成的阶跃式异质结(S型异质结).通过调控反应温度与时间设计不同尺寸的ZnIn₂S₄微球,并探索制备条件对光催化CO₂还原活性的影响.结果表明,当ZnIn₂S₄微球直径为6µm时,与MOF-808偶联所构建的复合光催化剂的CO₂还原活性最高.并且通过调控MOF-808比例,制备的S型异质结ZM₆-15%光催化剂的CO产率在辐照4h后达到8.21μmol g^‒1 h^‒1,分为别MOF-808(1.03μmol g^‒1 h^‒1)和ZnIn₂S₄(0.84μmol g^‒1 h^‒1)的8倍和10倍左右,明显提高了光催化CO₂还原性能.X射线衍射、扫描电镜、透射电镜和X射线光电子能谱(XPS)等研究结果表明,ZnIn₂S₄微球表面被MOF-808八面体粘附,这种紧密粘附的结构有利于ZnIn₂S₄与MOF-808之间载流子的转移和分离,从而提高光催化CO₂的还原效果.此外,电子顺磁共振和紫外光电子能谱等测试结果表明ZnIn₂S₄中存在弱空穴,MOF-808中存在弱电子.在光照下,光生电子通过界面接触快速从MOF-808导带中迁移到ZnIn₂S₄价带中并被消耗,为光生电子提供快速传输途径,提高了电子利用率.最终,MOF-808中存在光生空穴具有最高的氧化能力,ZnIn₂S₄中存在光生电子具有最高的还原能力.原位XPS测试与密度泛函理论计算结果进一步证明了ZnIn₂S₄与MOF-808之间的S型电荷转移机制.原位红外技术分析结果表明,S型异质结ZnIn₂S₄/MOF-808光催化剂通过Carbene途径将CO₂光催化还原为CO(CO₂→CO₂^*→COOH^*→CO^*→CO).综上,本文为合理设计S型异质结光催化剂,以实现高效光催化CO₂还原活性提供了新思路.

关键词: S型异质结, 形态作用, 光催化CO₂还原, 光生电子与空穴, 电荷转移机制

Abstract:

The design of a heterogeneous structure for photocatalysts has attracted significant attention. In this study, a step-scheme (S-scheme) heterojunction was designed using an in-situ synthesis method. The resulting heterojunction comprised 3D microspheres of ZnIn₂S₄ and octahedral MOF-808 (ZnIn₂S₄/MOF-808). During this process, we investigated the impact of the scale of the ZnIn₂S₄ microspheres on performance by controlling the growth of the ZnIn₂S₄ microspheres with various scales. The maximum catalytic activity was discovered to be achieved with ZnIn₂S₄ microspheres of 6 µm when coupled with MOF-808. Compared to pure ZnIn₂S₄ and MOF-808, the fabricated S-scheme ZnIn₂S₄/MOF-808 heterojunction exhibited notably improved photocatalytic CO₂ reduction performance. The performance of the CO yield of the optimized sample could reach 8.21 μmol g^‒1 h^‒1, which was approximately 10 and 8 times higher than those of ZnIn₂S₄ (0.84 μmol g^‒1 h^‒1) and MOF-808 (1.03 μmol g^‒1 h^‒1), respectively. Moreover, ultraviolet photoelectron spectroscopy, ESR, in situ X-ray photoelectron spectroscopy, and density functional theory calculations were used to study the charge transfer mechanism of the S-scheme heterojunction. In-situ FT-IR investigation established the Carbene pathway as the source of CO production (CO₂ → CO₂^* → COOH^* → CO^* → CO). This study provides an efficient method for designing an S-scheme heterojunction for photocatalytic CO₂ reduction.

Key words: S-scheme heterojunction, Morphological effect, Photocatalytic CO₂ reduction, Photogenerated electrons and holes, Charge transfer mechanism

宋明明, 宋相海, 刘鑫, 周伟强, 霍鹏伟. ZnIn₂S₄/MOF-808微球结构S型异质结光催化剂的制备及其光还原CO₂性能研究[J]. 催化学报, 2023, 51: 180-192.

Mingming Song, Xianghai Song, Xin Liu, Weiqiang Zhou, Pengwei Huo. Enhancing photocatalytic CO₂ reduction activity of ZnIn₂S₄/MOF-808 microsphere with S-scheme heterojunction by in situ synthesis method[J]. Chinese Journal of Catalysis, 2023, 51: 180-192.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(23)64480-8

https://www.cjcatal.com/CN/Y2023/V51/I8/180

图/表 10

Scheme 1. Preparation process of ZnIn2S4/MOF-808.

Fig. 1. (a) XRD patterns of the prepared samples. FT-IR spectra (b), nitrogen adsorption-desorption isotherms (c) and BJH pore size distributions (d) of MOF-808, ZIS and ZM6-15%.

Fig. 2. In-situ and ex-situ XPS spectra of MOF-808, ZIS and ZM6-15%. (a) Survey; (b) O 1s; (c) Zr 3d; (d) S 2p; (e) In 3d; (f) Zn 2p.

Fig. 3. TEM results of MOF-808 (a), ZIS (b), ZM6-15% (c). SEM results of MOF-808 (d), ZIS (e), ZM6-15% (f), and elemental mapping of C (g), O (h), Zr (i), In (j), S (k), Zn (l).

Fig. 4. UV-vis diffuse reflection spectra of different photocatalysts (a), band gap spectra (b), PL emission spectrum (c) and transient fluorescence spectrum (d) of MOF-808, ZIS and ZM6-15% materials monitored under 380 nm laser excitation.

Fig. 5. Transient photocurrent responses (a), EIS (b), LSV curves (c), and corresponding capacitance currents (d) of MOF-808, ZIS and ZM6-15%.

Fig. 6. CO yields (a) and production rate of CO (b) for different photocatalysts. (c) Kinetics curves of CO2 reduction over ZM6-15% under different conditions. (d) GC-MS results of 13CO2, produced over ZM6-15%.

Fig. 7. ESR spectra for DMPO/?O2- in methanol dispersion (a) and for DMPO/?OH in aqueous dispersion (b). In-situ FT-IR spectra for before (c) and after (d) photocatalytic reduction of ZM6-15%.

Fig. 8. UPS spectra of MOF-808 (a) and ZIS (b). Sketches of charge transfer before and after contact (c), side view of ZnIn2S4/MOF-808 structure (d) and the charge density difference for ZnIn2S4/MOF-808 (e).

Fig. 9. Proposed mechanism of the photocatalytic CO2 reduction over ZnIn2S4/MOF-808.

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ZnIn₂S₄/MOF-808微球结构S型异质结光催化剂的制备及其光还原CO₂性能研究

Enhancing photocatalytic CO₂ reduction activity of ZnIn₂S₄/MOF-808 microsphere with S-scheme heterojunction by in situ synthesis method

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[1]	蔡铭洁, 刘艳萍, 董珂欣, 陈晓波, 李世杰. 漂浮型Bi₂WO₆/C₃N₄/碳布S型异质结光催化材料用于高效净化水体环境[J]. 催化学报, 2023, 52(9): 239-251.
[2]	孙丽娟, 于晓慧, 唐丽永, 王伟康, 刘芹芹. 构建K₃PW₁₂O₄₀/CdS核壳S型异质结实现同步太阳能光催化分解水和选择性苯甲醇氧化反应[J]. 催化学报, 2023, 52(9): 164-175.
[3]	邵秀丽, 李可, 李静萍, 程强, 王国宏, 王楷. 揭示NiS@Ta₂O₅纳米纤维中梯型电荷转移路径及光催化CO₂转化性能[J]. 催化学报, 2023, 51(8): 193-203.
[4]	李世杰, 王春春, 董珂欣, 张鹏, 陈晓波, 李鑫. 新型MIL-101(Fe)/BiOBr S型异质催化剂用于高效光催化降解抗生素和还原六价铬: 光催化性能分析和光催化机理研究[J]. 催化学报, 2023, 51(8): 101-112.
[5]	李嘉明, 李源, 王小田, 杨直雄, 张高科. TiO₂上原子分散的Fe位点促进光催化CO₂还原: 增强的催化活性、 DFT计算和机制洞察[J]. 催化学报, 2023, 51(8): 145-156.
[6]	何厚伟, 王中辽, 代凯, 李素文, 张金锋. LSPR效应增强碳包覆In₂O₃/W₁₈O₄₉ S型异质结用于高效CO₂光还原[J]. 催化学报, 2023, 48(5): 267-278.
[7]	李瀚, 陶善仁, 万思杰, 邱国根, 龙庆, 余家国, 曹少文. ZnCdS纳米球和二苯并噻吩修饰的g-C₃N₄构成的S型异质结用于增强光催化产氢[J]. 催化学报, 2023, 46(3): 167-176.
[8]	陈成成, 刘芳庭, 张巧钰, 张正国, 刘琼, 方晓明. 理论设计和实验研究吡啶掺杂聚合氮化碳提升光催化CO₂还原性能[J]. 催化学报, 2023, 46(3): 91-102.
[9]	张志洁, 王雪盛, 唐慧玲, 李德本, 徐家跃. 调控Cs₃Bi₂Br₉@V_O-In₂O₃ S型异质结的费米能级和内建电场促进光生电荷分离和二氧化碳还原[J]. 催化学报, 2023, 55(12): 227-240.
[10]	吴优, 杨祎, 谷苗莉, 别传彪, 谭海燕, 程蓓, 许景三. 用于改进H₂O₂制备的1D/0D异质结的ZnIn₂S₄@ZnO S型光催化剂[J]. 催化学报, 2023, 53(10): 123-133.
[11]	王可, 程淼, 王楠, 张千一, 刘懿, 梁俊威, 管杰, 刘茂昌, 周建成, 李乃旭. 2D/2D超薄La₂Ti₂O₇/Ti₃C₂ Mxene肖特基异质结用于高效光催化CO₂还原[J]. 催化学报, 2023, 44(1): 146-159.
[12]	赵振龙, 边辑, 赵丽娜, 吴红君, 徐帅, 孙磊, 李志君, 张紫晴, 井立强. 2D ZnMOF/BiVO₄ S型异质结的构建及其可见光催化还原CO₂性能[J]. 催化学报, 2022, 43(5): 1331-1340.
[13]	赵君泽, 薛敏, 季梦夏, 王彬, 王雨, 李英杰, 陈自然, 李华明, 夏杰祥. “电子集流体”Bi₁₉S₂₇Br₃/BiOBr复合材料的制备及其增强光催化CO₂还原性能[J]. 催化学报, 2022, 43(5): 1324-1330.
[14]	徐阳锐, 朱晓蝶, 颜欢, 王盼盼, 宋旼珊, 马长畅, 陈自然, 储金宇, 刘馨琳, 逯子扬. 盐酸介导策略合成的具有优异光催化能力的ZnFe₂O₄小颗粒点缀一维苝二酰亚胺S型异质结[J]. 催化学报, 2022, 43(4): 1111-1122.
[15]	S. Wageh, Ahmed A. Al-Ghamdi, Omar A. Al-Hartomy, Maged F. Alotaibi, 王临曦. CdS/聚合物梯形产氢光催化剂及其原位光照电子转移机制[J]. 催化学报, 2022, 43(3): 586-588.