ZnIn2S4修饰TiO2的分级S型异质结用于促进光催化析氢

doi:10.1016/S1872-2067(23)64633-9

催化学报 ›› 2024, Vol. 59: 334-345.DOI: 10.1016/S1872-2067(23)64633-9

ZnIn₂S₄修饰TiO₂的分级S型异质结用于促进光催化析氢

张宝龙^a^,¹, 刘方璇^a^,¹, 孙彬^a^,^b^,^*(), 高婷婷^a^,^b, 周国伟^a^,^*()

^a齐鲁工业大学(山东省科学院)化学与化工学院, 山东省高校轻工精细化学品重点实验室, 济南市多尺度功能材料工程实验室, 山东济南 250353
^b烟台先进材料与绿色制造山东省实验室, 山东烟台 264006

收稿日期:2024-01-29 接受日期:2024-02-21 出版日期:2024-04-18 发布日期:2024-04-15
通讯作者: *电子信箱: binsun@qlu.edu.cn (孙彬), gwzhou@qlu.edu.cn (周国伟).
作者简介:
¹共同第一作者.
基金资助:
国家自然科学基金(52202102);国家自然科学基金(51972180);山东省自然科学基金(ZR2019BB030);山东省自然科学基金(ZR2020ME082);山东省高等学校青年创新团队发展计划(2021KJ056);烟台先进材料与绿色制造山东省实验室开放基金(AMGM2023F13);烟台先进材料与绿色制造山东省实验室开放基金(AMGM2021F05);山东省大学生创新创业训练计划(S202210431016);齐鲁工业大学科教产融合试点工程基础研究类项目(2023PY022)

Hierarchical S-scheme heterojunctions of ZnIn₂S₄-decorated TiO₂ for enhancing photocatalytic H₂ evolution

Baolong Zhang^a^,¹, Fangxuan Liu^a^,¹, Bin Sun^a^,^b^,^*(), Tingting Gao^a^,^b, Guowei Zhou^a^,^*()

^aKey Laboratory of Fine Chemicals in Universities of Shandong, Jinan Engineering Laboratory for Multi-scale Functional Materials, School of Chemistry and Chemical Engineering, Qilu University of Technology (Shandong Academy of Sciences), Jinan 250353, Shandong, China
^bShandong Laboratory of Advanced Materials and Green Manufacturing at Yantai, Yantai 264006, Shandong, China

Received:2024-01-29 Accepted:2024-02-21 Online:2024-04-18 Published:2024-04-15
Contact: *E-mail: binsun@qlu.edu.cn (B. Sun), gwzhou@qlu.edu.cn (G. Zhou).
About author:
¹Contributed equally to this work.
Supported by:
The National Natural Science Foundation of China(52202102);The National Natural Science Foundation of China(51972180);The Natural Science Foundation of Shandong Province(ZR2019BB030);The Natural Science Foundation of Shandong Province(ZR2020ME082);The Science and Technology Support Plan for Youth Innovation of Colleges and Universities of Shandong Province(2021KJ056);The Science Fund of Shandong Laboratory of Advanced Materials and Green Manufacturing at Yantai(AMGM2023F13);The Science Fund of Shandong Laboratory of Advanced Materials and Green Manufacturing at Yantai(AMGM2021F05);The Undergraduate Training Program on Innovation and Entrepreneurship of Shandong Province(S202210431016);The Science, Education and Industry Integration of Basic Research Projects of Qilu University of Technology(2023PY022)

摘要/Abstract

摘要：

利用半导体光催化裂解水制氢被认为是解决日益严重的环境污染和能源短缺问题的有效途径之一, 然而半导体光吸收范围窄、光生载流子复合率高以及光催化剂氧化还原能力差等问题限制了该技术的发展. 为克服这些难题, 构建能带结构匹配的S型异质结成为提高光催化活性的有效策略. 该结构能实现光生载流子的空间分离和转移, 有效地抑制其复合, 同时保留了光催化体系的强氧化还原能力.

本文利用原位化学浴沉积法成功地将ZnIn₂S₄纳米片修饰在花状TiO₂微球表面, 制备了具有独特分级结构的TiO₂/ZnIn₂S₄ S型异质结光催化材料, 并研究了其光催化析氢活性. Zeta电位结果表明, TiO₂带有正电荷, 可以率先吸附溶液中的S^2-并与后续加入的In³⁺和Zn²⁺原位反应生成ZnIn₂S₄, 进而构建稳定的TiO₂/ZnIn₂S₄异质结光催化剂. X射线粉末衍射、扫描电镜和透射电镜等结果证实了TiO₂/ZnIn₂S₄异质结光催化剂的成功制备. 紫外-可见漫反射结果表明, ZnIn₂S₄的引入明显增强了TiO₂的光吸收能力. 结合莫特-肖特基曲线、X射线光电子能价带谱和紫外光电子能谱等表征结果, 确定了TiO₂和ZnIn₂S₄的能带结构及费米能级位置. 光电流密度、电化学阻抗、表面光电压、荧光光谱和时间分辨荧光光谱等测试结果表明, TiO₂/ZnIn₂S₄异质结具有较好的光生载流子分离和转移效率以及更长的光生载流子寿命. 线性扫描伏安和接触角测试证明了TiO₂/ZnIn₂S₄异质结具有更低的过电势和良好的亲水性, 更有利于析氢反应发生. 通过阿伦尼乌斯方程对反应温度和析氢速率之间的关系进行拟合, 结果发现, TiO₂/ZnIn₂S₄异质结具有更低的析氢反应表观活化能, 从而更有利于光催化析氢反应发生. 非原位和原位X射线光电子能谱以及电子自旋共振光谱等结果表明, TiO₂/ZnIn₂S₄异质结遵循S型电子转移机理. 在模拟太阳光照射下, 最佳配比的TiO₂/ZnIn₂S₄异质结的光催化析氢速率达6.85 mmol g^-1 h^-1, 分别约为纯TiO₂和ZnIn₂S₄的171.2倍和3.9倍. 此外, 经六次循环后催化材料仍保持良好的光催化析氢活性, 表明具有紧密界面接触的分级结构异质结可以有效地抑制ZnIn₂S₄的光腐蚀, 且保持良好的结构稳定性.

综上, 本文构建了TiO₂/ZnIn₂S₄ S型异质结, 有效促进了光生载流子的空间分离和转移, 同时保留了其强氧化还原能力, 从而提高光催化析氢活性. 本研究为设计和合成高效的异质结光催化剂提供了参考.

关键词: TiO₂, 分级结构, ZnIn₂S₄, S型异质结, 光催化, 析氢

Abstract:

Photocatalytic water splitting to produce H₂ using semiconductor photocatalysts is a reliable approach to alleviating energy shortages and environmental pollution. However, the inadequate light-harvesting ability, rapid photogenerated carrier recombination, and inferior redox capacity of the individual photocatalysts restrict their photocatalytic activity. To address these limitations, a hierarchical S-scheme heterojunction of ZnIn₂S₄-nanosheet-decorated flower-like TiO₂ microspheres for enhancing photocatalytic H₂ evolution, purposely constructed through in situ chemical bath deposition, has been reported. The as-synthesized TiO₂/ZnIn₂S₄ heterojunctions exhibited ZnIn₂S₄-content-dependent photocatalytic activity for solar-driven H₂ evolution. As a result, the optimized TiO₂/ZnIn₂S₄ heterojunction exhibited a superior photocatalytic H₂ evolution rate of 6.85 mmol g^-1 h^-1, approximately 171.2- and 3.9-fold with respect to that obtained on pure TiO₂ and ZnIn₂S₄, respectively, mainly attributed to the unique hierarchical structure, extended light-harvesting ability, enhanced redox capacity, and improved separation and transfer efficiencies of the photogenerated carriers induced by the S-scheme heterojunctions. Simultaneously, a detailed analysis of the S-scheme electron transfer pathway in the TiO₂/ZnIn₂S₄ heterojunction was performed using in situ irradiated X-ray photoelectron spectroscopy and electron paramagnetic resonance spectroscopy. This study provides insights into the design of highly active heterojunction photocatalysts for sustainable solar-to-fuel energy conversion.

Key words: TiO₂, Hierarchical structure, ZnIn₂S₄, S-scheme heterojunction, Photocatalysis, H₂ evolution

张宝龙, 刘方璇, 孙彬, 高婷婷, 周国伟. ZnIn₂S₄修饰TiO₂的分级S型异质结用于促进光催化析氢[J]. 催化学报, 2024, 59: 334-345.

Baolong Zhang, Fangxuan Liu, Bin Sun, Tingting Gao, Guowei Zhou. Hierarchical S-scheme heterojunctions of ZnIn₂S₄-decorated TiO₂ for enhancing photocatalytic H₂ evolution[J]. Chinese Journal of Catalysis, 2024, 59: 334-345.

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图/表 10

Fig. 1. Schematic diagram of synthesis process of TiO2/ZnIn2S4 (a), Zeta potentials (b) of TiO2 and ZnIn2S4, XRD patterns (c) of TiO2, ZnIn2S4, and heterojunctions with different ZnIn2S4 content, N2 adsorption-desorption isotherms (d) and pore size distribution curves (e) of TiO2, ZnIn2S4, and TZ-2.

Fig. 2. FESEM images of TiO2 (a,b) and TZ-2 (c,d). TEM images of TiO2 (e) and TZ-2 (f,g). HRTEM image (h) and elemental mappings (i-n) of Ti, O, Zn, In, and S of TZ-2. The inset shows the fast Fourier transform patterns in (h).

Fig. 3. (a) XPS survey spectra of TiO2, ZnIn2S4, and TZ-2. High-resolution XPS spectra of Ti 2p (b), O 1s (c), Zn 2p (d), In 3d (e), and S 2p (f) of TiO2, ZnIn2S4, and TZ-2 with and without light irradiation.

Fig. 4. UV-vis diffuse reflectance spectra (a), Tauc plots (b), Mott-Schottky plots (c), VB-XPS spectra (d), UPS (e), and band structure diagram (f) of as-prepared samples.

Fig. 5. Photocatalytic H2 evolution (a) and photocatalytic H2 evolution rate (b) of as-obtained samples. Photocatalytic H2 evolution rate (c) of TZ-2 with and without sacrificial agents. AQY and UV-vis absorption spectra (d) of TZ-2. Recycling H2 evolution tests (e) of TZ-2. XRD patterns (d) of TZ-2 before and after photocatalytic reaction.

Table 1 Comparison of the photocatalytic H2 evolution rate of as-prepared TiO2/ZnIn2S4 heterojunction with other reported representative photocatalysts.

Photocatalyst	Sacrificial agent	H₂evolution rate (mmol g^-1 h^-1)	Enhancement factor vs. TiO₂	Ref.
ZnIn₂S₄/TiO_2-_x	MeOH	0.84	20.0	[65]
TiO₂@NC-A/ZnIn₂S₄	TEOA	2.80	—	[66]
TiO₂@ZnIn₂S₄	Lactic acid	1.24	24.2	[67]
rGO/TiO₂/ZnIn₂S₄	Na₂S/Na₂SO₃	0.46	71.1	[68]
g-C₃N₄/TiO₂/ZnIn₂S₄ (3 wt% Pt)	MeOH	6.53	6.9	[69]
TiO₂/ZnIn₂S₄	TEOA	6.03	3.7	[42]
Ti₃C₂@TiO₂/ZnIn₂S₄	Na₂S/Na₂SO₃	1.19	—	[70]
TiO₂/ZnIn₂S₄	TEOA	6.85	171.2	This work

Fig. 6. Transient photocurrent spectra (a), EIS Nyquist plots (b), SPV spectra (c), PL spectra (d), TRPL spectra (e), and LSV curves (f) of as-prepared samples.

Fig. 7. Linear relation between photocatalytic H2 evolution rate and temperature of TiO2 (a), ZnIn2S4 (b), and TZ-2 (c). (d) Corresponding comparison of apparent activation energy.

Fig. 8. EPR spectra of DMPO-?OH (a) and DMPO-?O2- (b) over TiO2, ZnIn2S4, and TZ-2 under light illumination. Schematic diagram of S-scheme mechanism over TiO2/ZnIn2S4 heterojunction: before contact (c), after contact (d), and light irradiation (e).

Fig. 9. Proposed photocatalytic H2 evolution mechanism of TiO2/ZnIn2S4 S-scheme heterojunction under simulated sunlight irradiation.

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ZnIn₂S₄修饰TiO₂的分级S型异质结用于促进光催化析氢

Hierarchical S-scheme heterojunctions of ZnIn₂S₄-decorated TiO₂ for enhancing photocatalytic H₂ evolution

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