飞秒瞬态吸收光谱研究ZnSe QDs/COF S型异质结光催化产H2O2中载流子传输机理

doi:10.1016/S1872-2067(24)60069-0

催化学报 ›› 2024, Vol. 63: 258-269.DOI: 10.1016/S1872-2067(24)60069-0

飞秒瞬态吸收光谱研究ZnSe QDs/COF S型异质结光催化产H₂O₂中载流子传输机理

赵艳艳^a, 杨春燕^b, 张淑敏^c, 孙国太^d, 朱必成^d, 王临曦^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西安医学院基础与转化医学研究所, 陕西西安 710021
^c长沙学院应用环境光催化湖南省重点实验室, 湖南长沙 410022
^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 430078

收稿日期:2024-05-08 接受日期:2024-05-27 出版日期:2024-08-18 发布日期:2024-08-19
通讯作者: *电子邮箱: wanglinxi@cug.edu.cn (王临曦),zhangjianjun@cug.edu.cn (张建军).
基金资助:
国家自然科学基金(22208332);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中心项目(22JY015);陕西省重点实验室项目(SLPT2301)

Investigating the charge transfer mechanism of ZnSe QD/COF S-scheme photocatalyst for H₂O₂ production by using femtosecond transient absorption spectroscopy

Yanyan Zhao^a, Chunyan Yang^b, Shumin Zhang^c, Guotai Sun^d, Bicheng Zhu^d, Linxi Wang^d^,^*(), Jianjun Zhang^d^,^*()

^aCollege of Biology Pharmacy and Food Engineering, Shangluo University, Shangluo 726000, Shaanxi, China
^bInstitute of Basic and Translational Medicine, Xi’an Medical University, Xi’an 710021, Shaanxi, China
^cHunan Key Laboratory of Applied Environmental Photocatalysis, Changsha University, Changsha 410022, Hunan, China
^dLaboratory of Solar Fuel, Faculty of Materials Science and Chemistry, China University of Geosciences, Wuhan 430078, Hubei, China

Received:2024-05-08 Accepted:2024-05-27 Online:2024-08-18 Published:2024-08-19
Contact: *E-mail: wanglinxi@cug.edu.cn (L. Wang), zhangjianjun@cug.edu.cn (J. Zhang).
Supported by:
National Natural Science Foundation of China(22208332);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);Shaanxi Province Key Research Office Project(SLPT2301)

摘要/Abstract

摘要：

过氧化氢(H₂O₂)作为一种绿色的氧化剂, 广泛应用于有机合成、消毒杀菌、废水处理和燃料电池等领域. 然而, 传统的蒽醌法制备H₂O₂不仅需要使用大量有机试剂且工艺复杂, 还易产生环境污染物. H₂和O₂直接合成法生产H₂O₂则因反应选择性和产率较低, 且反应物具有极高的爆炸风险而受限. 为了克服这些不足, 光催化生产H₂O₂作为一种绿色高效的替代方案近年来发展迅速, 该技术利用可再生的太阳光作为光源, 以水和空气中的氧气作为原料, 将光能转变为化学能, 具有绿色高效和节能环保的显著优势. 共价有机框架(COF)作为新型结晶多孔材料, 以其固有的孔隙率、可调孔径、有序通道、大比表面积、良好的热化学稳定性及丰富表面活性位点, 在光催化生产H₂O₂领域展现出巨大应用潜力. 尽管COF具有诸多优势, 但在实际应用中仍面临挑战, 如单一催化剂存在光生载流子易复合和氧化-还原能力弱等问题, 需要进一步优化和改进. 为了克服这些挑战, 构建异质结结构已被证明是一种有效提升单一催化剂光催化产H₂O₂效率的策略.

本文通过静电吸附组装法将ZnSe量子点与3D分层花状COF复合, 制备了一种具有高效光催化生产H₂O₂性能的ZnSe QDs/COF S型异质结光催化剂. 密度泛函理论计算结果表明, COF和ZnSe的费米能级分别为‒5.00和‒4.38 eV. 紫外-可见吸收光谱结合MS曲线结果表明, ZnSe QDs的导带(CB)和价带(VB)分别为‒1.82和0.98 eV, COF的CB和VB分别为‒0.64和1.96 eV. 理论上, COF可作为氧化型光催化剂, ZnSe可作为还原型光催化剂. 当二者接触时, ZnSe的自由电子会通过界面自发地转移到COF上, 直到两者的费米能级相等. 此时, 分别在ZnSe和COF上接近界面的区域形成电子耗尽层和电子积聚层, 使得ZnSe和COF在界面处分别带正电荷和负电荷, 从而形成内建电场. 光照下, 该内建电场的存在加速了光生电子从COF向ZnSe的转移, 有利于弱氧化还原能力的光生电子和空穴的复合, 而强氧化还原能力的光生电子和空穴得以保留并实现空间上的分离, 从而使得ZnSe QDs/COF S型异质结具有优于单一COF和ZnSe QDs的光催化性能. 光催化产H₂O₂实验结果表明, 当以10%-乙醇/水作为牺牲剂时, ZnSe QDs/COF的H₂O₂生成率可达1895 mol g^‒1 h^‒1. 飞秒瞬态吸收光谱(fs-TAS)结果表明, 在光催化过程中, 有三种主要的载流子传输通道: (1) COF导带上的光生电子快速转移到ZnSe QDs价带的过程; (2) COF中缺陷态诱导的光生载流子复合过程; (3) COF中导、价带上光生电子-空穴的复合过程. fs-TAS结果表明, ZnSe QDs/COF S型异质结中构建了一种新型的电子超快转移通道, 且为S型电子传递机制, 与原位辐照X射线光电子能谱结果一致.

综上所述, 本文成功构建了一种ZnSe QDs/COF S型异质结光催化剂, 有效提高了光催化产H₂O₂的性能, 为构建无机/有机S型异质结用于高效光催化产H₂O₂提供了理论和实验参考.

关键词: ZnSe量子点, 共价有机框架, S型异质结, 载流子传输和分离, 生产H₂O₂

Abstract:

Abstract: Hydrogen peroxide (H₂O₂) has gained widespread attention as a versatile oxidant and a mild disinfectant. Here, an electrostatic self-assembly method is applied to couple ZnSe quantum dots (QDs) with a flower-like covalent organic framework (COF) to form a step-scheme (S-scheme) photocatalyst for H₂O₂ production. The as-prepared S-scheme photocatalyst exhibits a broad light absorption range with an edge at 810 nm owing to the synergistic effect between the ZnSe QDs and COF. The S-scheme charge-carrier transfer mechanism is validated by performing Fermi level calculations and in-situ X-ray photoelectron and femtosecond transient absorption spectroscopies. Photoluminescence, time-resolved photoluminescence, photocurrent response, electrochemical impedance spectroscopy, and electron paramagnetic resonance results show that the S-scheme heterojunction not only promotes charge carrier separation but also boosts the redox ability, resulting in enhanced photocatalytic performance. Remarkably, a 10%-ZnSe QD/COF has excellent photocatalytic H₂O₂-production activity, and the optimal S-scheme composite with ethanol as the hole scavenger yields a H₂O₂-production rate of 1895 mol g^-1 h^-1. This study presents an example of a high-performance organic/inorganic S-scheme photocatalyst for H₂O₂ production.

Key words: ZnSe quantum dot, Covalent organic framework, S-scheme heterojunction, Carrier migration and separation, H₂O₂ production

赵艳艳, 杨春燕, 张淑敏, 孙国太, 朱必成, 王临曦, 张建军. 飞秒瞬态吸收光谱研究ZnSe QDs/COF S型异质结光催化产H₂O₂中载流子传输机理[J]. 催化学报, 2024, 63: 258-269.

Yanyan Zhao, Chunyan Yang, Shumin Zhang, Guotai Sun, Bicheng Zhu, Linxi Wang, Jianjun Zhang. Investigating the charge transfer mechanism of ZnSe QD/COF S-scheme photocatalyst for H₂O₂ production by using femtosecond transient absorption spectroscopy[J]. Chinese Journal of Catalysis, 2024, 63: 258-269.

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图/表 11

Fig. 1. (a) Schematic illustrating the preparation process for Z/T composites. TEM image (b) and HRTEM images (c,d) of Z/T-10%. (e) HAADF image of Z/T-10% and the corresponding EDS maps of C, N, O, Se, and Zn.

Fig. 2. (a) XRD patterns of ZnSe QDs, Ta-Dva COF, and Z/T-10%. The blue lines represent the standard diffraction pattern of cubic ZnSe crystals. (b) FTIR spectra of the as-prepared ZnSe QDs, Ta-Dva COF, and Z/T-10%.

Fig. 3. (a) UV-vis DRS spectra of ZnSe QDs, Ta-Dva COF, and Z/T-10%. Tauc plots (b) and Mott-Schottky plots (c) of ZnSe QDs and Ta-Dva COF. (d) Band diagrams of ZnSe QDs and Ta-Dva COF, and standard potentials of O2/?O2- and OH-/?OH.

Fig. 4. O 1s (a) and N 1s (b) spectra of Ta-Dva COF and Z/T-10% (in dark and under 365-nm LED irradiation). Zn 2p (c) and Se 3d (d) spectra of ZnSe QDs and Z/T-10% (in dark and under 365-nm LED irradiation).

Fig. 5. Calculated work functions of Ta-Dva COF (a) and ZnSe QDs (311) (b). (c) Schematic illustration of the S-scheme carrier transfer mechanism in Z/T composites before contact, after contact, and under light illumination.

Fig. 6. PL spectra (a), TRPL spectra (b), transient photocurrent density (c), and Nyquist plots (d) of Ta-Dva COF, ZnSe QDs, and Z/T-10%.

Fig. 7. Pseudocolor TA plots of pristine ZnSe QDs (a), bare Ta-Dva COF (b), and Z/T-10% S-scheme heterojunction (c). fs‐TAS spectra of pristine ZnSe QDs (d), bare Ta-Dva COF (e), and Z/T-10% S-scheme heterojunction (f) recorded at indicated delay times under 325 nm pump pulse with average pump power of ~73 μW.

Fig. 8. Normalized decay kinetics of pristine ZnSe QD probe at 440 nm (a), bare Ta-Dva COF probe at 480 nm (b), and Z/T-10% composite probe at 550 nm (c). (d) Schematic for the decay pathways of photogenerated electrons in Z/T-10% S-scheme heterojunction.

Fig. 9. (a) Photocatalytic production of H2O2 over the as-prepared samples with ethanol as sacrificial agent under 1-h light irradiation. (b) H2O2 yield over Z/T-10% with ethanol as the sacrificial agent under 5-h light irradiation. (c) H2O2 yield over Z/T-10% under different conditions. (d) H2O2 yield over Z/T-10% with Rhodamine B (10 mg L-1) as the sacrificial agent. (e) Photocatalytic decomposition of H2O2 (1 mmol L-1) over different samples in N2-saturated DI water. (f) Formation rate (Kf) and decomposition rate (Kd) over the photocatalyst.

Fig. 10. EPR signals of DMPO-·OH (a) and DMPO-·O2- (b). (c) In-situ DRIFTS spectra of Z/T-10% S-scheme heterojunction under H2O and O2.

Fig. 11. Proposed reaction pathway for H2O2 production over Z/T-10% S-scheme photocatalysts.

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飞秒瞬态吸收光谱研究ZnSe QDs/COF S型异质结光催化产H₂O₂中载流子传输机理

Investigating the charge transfer mechanism of ZnSe QD/COF S-scheme photocatalyst for H₂O₂ production by using femtosecond transient absorption spectroscopy

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