通过氟掺杂调控TiO2的d带中心以增强光催化产H2O2活性

doi:10.1016/S1872-2067(23)64645-5

催化学报 ›› 2024, Vol. 60: 219-230.DOI: 10.1016/S1872-2067(23)64645-5

通过氟掺杂调控TiO₂的d带中心以增强光催化产H₂O₂活性

赵艳艳^a, 张淑敏^b, 吴珍^c, 朱必成^d, 孙国太^d, 张建军^d^,^*()

^a商洛学院生物医药与食品工程学院, 陕西商洛 726000
^b长沙学院应用环境光催化湖南省重点实验室, 湖南长沙 410022
^c鄂尔多斯应用技术学院化学工程学院, 内蒙古鄂尔多斯 017000
^d中国地质大学(武汉)材料与化学学院, 太阳燃料实验室, 湖北武汉 430074

收稿日期:2024-01-30 接受日期:2024-02-29 出版日期:2024-05-18 发布日期:2024-05-20
通讯作者: *电子信箱: zhangjianjun@cug.edu.cn (张建军).
基金资助:
国家自然科学基金(52202375);国家自然科学基金(52372294);国家自然科学基金(22302183);国家自然科学基金(22362004);陕西省教育厅协同创新项目(22JY015)

Regulation of d-band center of TiO₂ through fluoride doping for enhancing photocatalytic H₂O₂ production activity

Yanyan Zhao^a, Shumin Zhang^b, Zhen Wu^c, Bicheng Zhu^d, Guotai Sun^d, Jianjun Zhang^d^,^*()

^aCollege of Biology Pharmacy and Food Engineering, Shangluo University, Shangluo 726000, Shaanxi, China
^bHunan Key Laboratory of Applied Environmental Photocatalysis, Changsha University, Changsha 410022, Hunan, China
^cDepartment of Chemical Engineering, Ordos Institute of Technology, Ordos 017000, Inner Mongolia, China
^dLaboratory of Solar Fuel, Faculty of Materials Science and Chemistry, China University of Geosciences, Wuhan 430074, Hubei, China

Received:2024-01-30 Accepted:2024-02-29 Online:2024-05-18 Published:2024-05-20
Contact: *E-mail: zhangjianjun@cug.edu.cn (J. Zhang).
Supported by:
National Natural Science Foundation of China(52202375);National Natural Science Foundation of China(52372294);National Natural Science Foundation of China(22302183);National Natural Science Foundation of China(22362004);Specialized Research Fund of Education Department of Shaanxi Province(22JY015)

摘要/Abstract

摘要：

光催化产双氧水(H₂O₂)以太阳光、水和空气中的氧气作为原料, 将光能转变为化学能, 是一种绿色高效节能环保的新技术, 具有较好的应用前景. 光催化产H₂O₂主要包括三个关键步骤: (1) 催化剂在高能入射光激发下产生光生电子和空穴; (2) 光生电子-空穴对分离并迁移到催化剂表面; (3) 光生电子与催化剂表面吸附的氧气发生反应生成超氧自由基, 其继续与水和光生电子反应, 产生H₂O₂. 因此, 氧气在催化剂表面吸附性能的强弱对光催化产H₂O₂的性能有着重要影响. d带中心理论表明, 金属的d带能级高低决定了催化剂表面活性位点对小分子物质的吸附强度, 能级越高, 催化剂对小分子物质的吸附能力越强. TiO₂具有制备简单、无毒、理化性质稳定、导价带位置跨越多个氧化还原电位等诸多优势, 在光催化生产H₂O₂领域具有较好的应用前景. 提升TiO₂的d带中心可以提高其对小分子物质如O₂的吸附性能, 有效提升其光催化产H₂O₂的活性.

本文从氟离子掺杂提升TiO₂的d带中心增强对O₂的吸附性能入手, 通过第一性理论计算、电子顺磁共振实验、飞秒瞬态吸收光谱等方法研究光生载流子的传输机理, 阐明F/TiO₂光催化产H₂O₂活性增强机制, 并对TiO₂光催化产H₂O₂的前景提出了展望. 首先, 分别以钛酸四异丙酯和氟化铵作为钛源和氟源, 通过溶胶-凝胶法结合高温煅烧制得了F/TiO₂光催化剂. 第一性理论计算结果表明, F^‒体相掺杂导致TiO₂的电荷分布不均匀, 使得d带中心上移, 从而增强TiO₂与表面吸附O₂的相互作用, 降低表面氧的吸附能, 最终提高光催化生成H₂O₂的效率. 电子顺磁共振实验结果表明, 晶格中F^‒离子的存在诱导了还原性Ti³⁺中心的形成, 这些还原性Ti³⁺中心可以提供电荷补偿所需的额外电子. O₂温度程序解吸实验结果表明, F/TiO₂对O₂的化学吸附能力高于纯TiO₂, 说明较低的反键轨道占用率可以增强Ti³⁺对O₂的吸附. 飞秒瞬态吸收光谱结果表明, 光生电子从F/TiO₂的导带转移到Ti³⁺表面态和表面F^‒离子上, 加速了光生电子和空穴的分离; 光生电子与吸附在F/TiO₂表面的O₂发生反应, 加速了H₂O₂的生成. 光催化产H₂O₂性能实验结果表明, F^‒掺杂TiO₂后, 光催化生成H₂O₂的产率由277 μmol·g^‒1·h^‒1提高到了467 μmol·g^‒1·h^‒1. 循环实验结果表明, F/TiO₂使用前后形貌和晶体结构几乎没有改变, 且循环实验后氧空位和Ti³⁺中心依然存在, 说明制得的F/TiO₂光催化剂具有良好的稳定性.

综上所述, 本文借助第一性理论计算并结合实验结果, 从d带中心调控的角度揭示了F/TiO₂光催化产H₂O₂活性提高的机理, 阐明了光催化产H₂O₂的反应机制. 本研究为优化光催化剂与氧气之间的吸附强度, 提高光催化产H₂O₂的性能提供了一种新策略, 可为后续光催化产H₂O₂技术的改进和应用提供参考.

关键词: 反键轨道, d带中心, 氧吸附, 电荷转移, 双氧水生成

Abstract:

Titanium dioxide (TiO₂) has received extensive attention for photocatalytic hydrogen peroxide (H₂O₂) production, with the d-band center related to the adsorption performance, which affects the photocatalytic reaction process. Herein, an ingenious strategy to lower the antibonding-orbital occupancy in the Ti 3d orbital by fluoride ion (F^‒) doping is proposed, with density functional theory calculations predicting that F-doping into TiO₂ induces a non-uniform charge distribution and enables an upshift of the d-band center in F/TiO₂. This manipulation provides accessible active centers with favorable d-band energy levels, which can improve the charge-transfer behavior, strengthen the interaction between the adsorbed oxygen and the photocatalyst, and reduce the adsorption energy of oxygen, eventually promoting the photocatalytic H₂O₂ production rate. The experimental results further confirm that a lower antibonding-orbital occupancy can intensify the adsorption of atomic oxygen at the Ti sites. Electron paramagnetic resonance experiment reveals that the presence of F^‒ ions in the lattice induces the formation of Ti³⁺ centers that localize the extra electron needed for charge compensation. Femtosecond transient absorption (fs-TA) spectroscopy suggests that photogenerated electrons are transferred from the conduction band of F/TiO₂ to the Ti³⁺ surface states and surface F^‒ ions, expediting the separation of electrons and holes. Consequently, with F^‒ doping in TiO₂, the photocatalytic H₂O₂ production yields improved from 277 to 467 μmol·g^‒1·h^‒1, with ethanol as a sacrificial reagent. This study provides a new strategy for regulating the d-band center to optimize the adsorption strength between the photocatalyst and oxygen atoms and achieve enhanced photocatalytic H₂O₂ production performance.

Key words: Antibonding orbital, d-Band center, Oxygen adsorption, Charge transfer, Hydrogen peroxide production

赵艳艳, 张淑敏, 吴珍, 朱必成, 孙国太, 张建军. 通过氟掺杂调控TiO₂的d带中心以增强光催化产H₂O₂活性[J]. 催化学报, 2024, 60: 219-230.

Yanyan Zhao, Shumin Zhang, Zhen Wu, Bicheng Zhu, Guotai Sun, Jianjun Zhang. Regulation of d-band center of TiO₂ through fluoride doping for enhancing photocatalytic H₂O₂ production activity[J]. Chinese Journal of Catalysis, 2024, 60: 219-230.

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图/表 10

Fig. 1. Graphical illustration of regulation of d-band center over F/TiO2.

Fig. 2. (a) Preparation processes of F/TiO2. TEM image (b) and the corresponding HRTEM image (c) of F/TiO2. (d) HAADF image of F/TiO2 and the EDS mapping images of F, O, and Ti elements.

Fig. 3. XPS depth profiling spectra for F/TiO2 at different sputtering times with C 1s peak at 284.6 eV as a reference. Atomic percentage (at%) distribution of Ti, O, and F (a), and high-resolution spectra of Ti 2p (b), O 1s (c), and F 1s (d). Here, 0 s is equivalent to a standard surface scan without ion sputtering, with spectra obtained after 60-180 s of sputtering corresponding to the elemental composition of the pellet bulk. Strength of the ion gun: 1000, 2000 eV.

Fig. 4. (a) EPR and (b) DRS spectra of TiO2 and F/TiO2.

Fig. 5. Calculated electronic band structure of TiO2 before (a) and after (b) fluorination. Work functions of TiO2 (c) and F/TiO2 (d).

Fig. 6. DOS for TiO2 (a) and F/TiO2 (b). (c) Calculated Ti d orbital DOS for both TiO2 and F/TiO2 surface phases. (d) Schematic diagram illustrating the optimization of antibonding-orbital occupancy of Ti?Oads for strengthening the adsorption of active Ti sites toward atomic oxygen.

Fig. 7. (a) Zeta potential of the as-prepared TiO2 and F/TiO2 in DI water. (b) O2-TPD patterns of TiO2 and F/TiO2. In situ DRIFTS spectra of O2 adsorption over TiO2 (c) and F/TiO2 (d).

Fig. 8. Photocatalytic H2O2 production performance of the as-prepared samples with ethanol as the sacrificial reagent (a) and in pure water without sacrificial reagent (b), with the H2O2 production rates summarized in (c). (d) Cycling experiments over F/TiO2 photocatalyst. (e) Photocatalytic H2O2 (1 mmol·L?1) decomposition over the as-prepared samples. (f) Comparison of ORR for H2O2 production over F/TiO2 in O2, air, and N2 with ethanol as the sacrificial agent.

Fig. 9. (a) DMPO spin-trapping EPR spectra for superoxide radical (·O2?). (b) Amount of ·O2? over TiO2 and F/TiO2 photocatalyst. PL spectra (c), TRPL spectra (d), TPR experiments (e), and EIS analysis (f) of the as-prepared TiO2 and F/TiO2. Rs, Rct, and CPE represent the electrode solution resistance, interfacial charge transfer resistance, and constant phase element, respectively.

Fig. 10. Pseudocolor plots of TiO2 (a) and F/TiO2 (b). fs-TA spectra signals at indicated delay times measured with 325 nm pump pulse excitation over TiO2 (c) and F/TiO2 (d). (e) Normalized decay kinetic curves of GSB peaks in fs-TA spectra of TiO2 and F/TiO2. (f) Schematic diagrams for electrons transfer pathway and improved photogenerated carrier separation efficiency over F/TiO2.

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通过氟掺杂调控TiO₂的d带中心以增强光催化产H₂O₂活性

Regulation of d-band center of TiO₂ through fluoride doping for enhancing photocatalytic H₂O₂ production activity

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