双助催化剂Ag/Ti3C2/TiO2分层花状微球用于增强光催化产氢活性

doi:10.1016/S1872-2067(23)64462-6

催化学报 ›› 2023, Vol. 50: 273-283.DOI: 10.1016/S1872-2067(23)64462-6

双助催化剂Ag/Ti₃C₂/TiO₂分层花状微球用于增强光催化产氢活性

刘德法, 孙彬^*(), 白硕杰, 高婷婷, 周国伟^*()

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

收稿日期:2023-04-03 接受日期:2023-05-27 出版日期:2023-07-18 发布日期:2023-07-25
通讯作者: *电子信箱: binsun@qlu.edu.cn (孙彬), gwzhou@qlu.edu.cn (周国伟).
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(ZR2021ZD27);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);济南市高校院所创新团队(2018GXRC006);齐鲁工业大学科教产融合试点工程项目(2022PY062)

Dual co-catalysts Ag/Ti₃C₂/TiO₂ hierarchical flower-like microspheres with enhanced photocatalytic H₂-production activity

Defa Liu, Bin Sun^*(), Shuojie Bai, Tingting Gao, Guowei Zhou^*()

Key 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

Received:2023-04-03 Accepted:2023-05-27 Online:2023-07-18 Published:2023-07-25
Contact: *E-mail: binsun@qlu.edu.cn (B. Sun), gwzhou@qlu.edu.cn (G. Zhou).
Supported by:
National Natural Science Foundation of China(52202102);National Natural Science Foundation of China(51972180);Natural Science Foundation of Shandong Province(ZR2019BB030);Natural Science Foundation of Shandong Province(ZR2021ZD27);Natural Science Foundation of Shandong Province(ZR2020ME082);Science and Technology Support Plan for Youth Innovation of Colleges and Universities of Shandong Province(2021KJ056);Science Fund of Shandong Laboratory of Advanced Materials and Green Manufacturing (Yantai)(AMGM2023F13);Science Fund of Shandong Laboratory of Advanced Materials and Green Manufacturing (Yantai)(AMGM2021F05);Undergraduate Training Program on Innovation and Entrepreneurship of Shandong Province(S202210431016);Program for Scientific Research Innovation Team in Colleges and Universities of Jinan(2018GXRC006);Science, Education and Industry Integration of Basic Research Projects of Qilu University of Technology(2022PY062)

摘要/Abstract

摘要：

在“碳达峰、碳中和”背景下, 太阳能驱动的半导体光催化技术被认为是解决能源危机和环境问题的有效方法之一. 开发高效的半导体光催化材料是半导体光催化技术发展的重中之重. 在众多半导体光催化材料中, TiO₂因其无毒性、光化学稳定性良好和价格低廉等优点, 在光催化领域备受关注. 然而, 单一TiO₂较低的光生载流子的分离和转移效率是制约其进一步应用的关键问题. 通过负载助催化剂可以提供更多的活性位点、增强光吸收以及提高光生载流子的分离和转移效率, 被认为是提高光催化活性的有效策略.

本文利用静电自组装策略和光还原法成功地将双助催化剂Ti₃C₂纳米片和Ag纳米颗粒修饰在分层花状TiO₂微球表面, 构筑了Ag/Ti₃C₂/TiO₂复合光催化材料, 并考察其光催化产氢性能. Zeta电位测试结果表明, 带有相反表面电荷的分层花状TiO₂微球和Ti₃C₂纳米片可以通过静电作用构筑稳定的Ti₃C₂/TiO₂复合光催化材料. 同时, 基于Ti₃C₂/TiO₂复合材料的光催化性能, 在光照条件下Ag⁺可被还原为Ag而被固定在Ti₃C₂/TiO₂复合材料表面. 通过X射线粉末衍射、拉曼光谱、扫描电子显微镜和透射电子显微镜等证明成功制备了Ag/Ti₃C₂/TiO₂复合光催化材料. 此外, X射线光电子能谱也证明了复合材料中存在光生电子的分离和转移过程. 接触角测试结果表明, 构筑的Ag/Ti₃C₂/TiO₂复合材料具有较好的亲水性, 可以更好地吸附水分子以保证还原反应的进行. 紫外-可见漫反射光谱测试结果表明, Ti₃C₂和Ag助催化剂的引入提高了材料的光吸收能力. 荧光光谱、时间分辨荧光光谱、光电流密度和电化学阻抗等测试结果表明, Ag/Ti₃C₂/TiO₂复合材料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. 另外, 线性扫描伏安测试证明了Ag/Ti₃C₂/TiO₂复合材料具有低的过电势, 更加有利于析氢反应.

在模拟太阳光照射下, 最佳Ti₃C₂ (3 wt%)和Ag (2.5 wt%)含量的Ag/Ti₃C₂/TiO₂复合材料的光催化产氢速率为1024.72 μmol g^-1 h^-1, 分别约为单一TiO₂, Ti₃C₂/TiO₂复合材料和Ag/TiO₂复合材料的40, 2.3和1.8倍, 且三次循环利用后仍保持较好的光催化产氢活性. 光催化产氢活性的提高主要归因于Ti₃C₂和Ag双助催化剂的引入增强了光吸收能力和提高了光生载流子的分离和转移效率, 从而增强了TiO₂的光催化活性. 综上, 本文揭示了构建双助催化剂的复合光催化材料更加有利于促进光催化材料的光生电子-空穴对的分离和转移, 对高活性和高稳定性光催化剂的设计和性能调控有一定参考价值.

关键词: 分层花状TiO₂微球, 双助催化剂, 光催化, 协同效应, 产氢

Abstract:

Solar-powered semiconductor photocatalysis is considered a powerful strategy for addressing environmental pollution and energy crisis. Nevertheless, the separation and transfer abilities of photogenerated photocatalysts remain unsatisfactory. Herein, dual Ti₃C₂ nanosheets/Ag co-catalysts synergistically decorated hierarchical flower-like TiO₂ microspheres for boosting photocatalytic H₂ production were fabricated by electrostatic self-assembly and subsequent photoreduction procedures. The optimal Ag/Ti₃C₂/TiO₂ composite demonstrated an excellent photocatalytic H₂-production rate of 1024.72 μmol g^-1 h^-1 under simulated solar irradiation, achieving nearly 40, 2.3, and 1.8 folds with respect to that obtained on pristine TiO₂, optimized Ti₃C₂/TiO₂ composite, and Ag/TiO₂ composite, respectively. The considerably improved photocatalytic H₂-production activity is associated with the synergistic effect of the hierarchical flower-like structure of TiO₂, excellent electrical conductivity of Ti₃C₂, and surface plasmon resonance effect of Ag, which enhances the light absorption capacity and promotes the separation and transfer of photogenerated carriers. This study provides insight into the design of high-efficiency photocatalysts with dual co-catalysts for solar H₂ production.

Key words: Hierarchical flower-like TiO₂, microsphere, Dual co-catalysts, Photocatalysis, Synergistic effect, H₂ production

刘德法, 孙彬, 白硕杰, 高婷婷, 周国伟. 双助催化剂Ag/Ti₃C₂/TiO₂分层花状微球用于增强光催化产氢活性[J]. 催化学报, 2023, 50: 273-283.

Defa Liu, Bin Sun, Shuojie Bai, Tingting Gao, Guowei Zhou. Dual co-catalysts Ag/Ti₃C₂/TiO₂ hierarchical flower-like microspheres with enhanced photocatalytic H₂-production activity[J]. Chinese Journal of Catalysis, 2023, 50: 273-283.

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图/表 9

Fig. 1. Schematic of the formation process of Ag/Ti3C2/TiO2 composites.

Fig. 2. XRD patterns (a,b) and Raman spectra (c,d) of Ti3AlC2, Ti3C2, TiO2, TM-3%, and ATM-2.5%; the magnified Raman spectra in the range of 1200-1800 cm-1 in (d).

Fig. 3. FESEM images of TiO2 (a,b), TM-3% (c,d), and ATM-2.5% (e,f).

Fig. 4. TEM images of TiO2 (a), TM-3% (b), and ATM-2.5% (c). HRTEM images (d,e), EDS spectrum (f), and elemental mappings (g) of Ti, O, C, and Ag of ATM-2.5%.

Fig. 5. High-resolution XPS spectra of Ti 2p (a), O 1s (b), C 1s (c), and Ag 3d (d) of Ti3C2, TM-3%, and ATM-2.5%.

Fig. 6. N2 adsorption-desorption isotherms (a) and corresponding pore size distribution curves (b) of TiO2, Ti3C2, TM-3%, and ATM-2.5%.

Fig. 7. UV-vis diffuse reflectance spectra (a), band gap plots (b), PL spectra (c), TRPL spectra (d), transient photocurrent responses (e), and EIS Nyquist plots (f) of as-prepared samples.

Fig. 8. Photocatalytic H2 production (a) and photocatalytic H2-production rates (b) of as-prepared samples. Recycling test of photocatalytic H2 production over ATM-2.5% (c). AQY (d) of TiO2, TM-3%, and ATM-2.5% at 365 nm.

Fig. 9. Proposed mechanism and energy band structure for photocatalytic H2 production over Ag/Ti3C2/TiO2 composites under simulated solar irradiation.

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双助催化剂Ag/Ti₃C₂/TiO₂分层花状微球用于增强光催化产氢活性

Dual co-catalysts Ag/Ti₃C₂/TiO₂ hierarchical flower-like microspheres with enhanced photocatalytic H₂-production activity

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