2D/3D ZnIn2S4/TiO2复合物的原位构筑及其提高的光催化性能

doi:10.6023/A21060265

摘要/Abstract

通过高温煅烧和油浴的方法构筑二维/三维(2D/3D) ZnIn₂S₄/TiO₂异质结, 应用于光催化降解罗丹明B (RhB)和四环素(TC), 来研究异质结的构筑对TiO₂可见光响应范围和光生载流子对分离效率的影响. 结果表明, TiO₂维持了MOFs的形貌, 显示窄的可见光响应范围和高的光生电荷复合率, 与ZnIn₂S₄纳米片复合后, TiO₂的比表面积增大, 光催化活性位点增多. 带隙宽度也由TiO₂的3.23 eV减小到ZnIn₂S₄/TiO₂-II的2.52 eV, 从而获得了更宽的可见光响应范围. 能带结构表明ZnIn₂S₄/TiO₂是type II型异质结, 提高了光生载流子对的分离与转移效率. 在可见光照射下, ZnIn₂S₄/TiO₂-II显示了最高的RhB光催化降解效率(93%), 分别是TiO₂和ZnIn₂S₄的18和2倍. 同时, ZnIn₂S₄/TiO₂-II也显示出比TiO₂和ZnIn₂S₄更高的TC降解效率(90%). 循环实验表明ZnIn₂S₄/TiO₂-II能保持良好的稳定性, 经5次循环实验后仍能降解83%的RhB. 研究表明基于MOFs衍生的TiO₂构筑2D/3D ZnIn₂S₄/TiO₂异质结是提高TiO₂光催化性能的一条有效途径.

关键词: 光催化, 二氧化钛, 金属有机框架材料, 异质结, 可见光响应

To study the influence of the construction of heterojunction on the visible-light response range and the photo-generated charge carriers separation efficiency of TiO₂, two dimensional/three dimensional (2D/3D) ZnIn₂S₄/TiO₂ heterojunctions were synthesized by high-temperature calcination followed by a facile oil bath method, and were investigated for the photodegradation of Rhodamine B (RhB) and tetracycline (TC). X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) were applied to investigate the composition, crystal structure, and morphology of the as-prepared specimens. UV-visible diffuse reflectance spectra (UV-vis DRS), electrochemical impedance spectroscopy (EIS), photocurrent measurement, photoluminescence (PL) spectra, and first-principles calculation were also performed to investigate the photoelectric property. The results showed TiO₂ maintains the morphology of metal-organic frameworks (MOFs) with narrow visible-light response range and high photo-generated charge recombination efficiency. After coupling with ZnIn₂S₄ nanosheets, a larger specific surface area was obtained with offering more active sites for photocatalytic reaction. The band gap of the composite was reduced from 3.23 eV of TiO₂ to 2.52 eV of ZnIn₂S₄/TiO₂-II, and thus obtaining an extended visible-light response range and enhancing visible light utilization rate. The energy band structure acquired from the UV-vis DRS and XPS valence band spectra indicated a construction of type II heterojunction in the ZnIn₂S₄/TiO₂composite, and thus improving the separation and transfer efficiency of photo-generated carrier pairs, which was confirmed by the PL, EIS and photocurrent test results. Under the visible light, ZnIn₂S₄/TiO₂ displayed signiﬁcantly enhanced photocatalytic activity than bare TiO₂and ZnIn₂S₄. Among of ZnIn₂S₄/TiO₂photocatalysts, ZnIn₂S₄/TiO₂-II possessed the highest photocatalytic degradation efficiency (93%) of RhB solution within 60 min, which was nearly 18 and 2 times higher than pristine TiO₂and ZnIn₂S₄, respectively. Besides, the ZnIn₂S₄/TiO₂-II photocatalyst also showed enhanced photocatalytic activity for TC degradation than pure TiO₂and ZnIn₂S₄. The cycle experiment showed that the ZnIn₂S₄/TiO₂-II photocatalyst could maintain good reusability, and it could still photodegrade 83% RhB after 5-cycle test. This work demonstrates that constructing 2D/3D ZnIn₂S₄/TiO₂ heterojunction based on MOFs-derived TiO₂ is an efficient strategy for significantly enhancing the photocatalytic activity of TiO₂.

Key words: photocatalysis, titanium dioxide, metal-organic frameworks, heterojunction, visible-light response

引用此文

刘欢, 李京哲, 李平, 张广智, 张广智, 张豪, 邱灵芳, 齐晖, 多树旺. 2D/3D ZnIn₂S₄/TiO₂复合物的原位构筑及其提高的光催化性能[J]. 化学学报, 2021, 79(10): 1293-1301.

Huan Liu, Li Li, Ping Li, Guangzhi Zhang, Xun Xu, Hao Zhang, Lingfang Qiu, Hui Qi, Shuwang Duo. In-situ Construction of 2D/3D ZnIn₂S₄/TiO₂ with Enhanced Photocatalytic Performance[J]. Acta Chimica Sinica, 2021, 79(10): 1293-1301.

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图/表 12

图1. 样品的XRD图

Figure 1. The XRD patterns of the specimens

图2. (a) MIL-125, (b) TiO2, (c) ZnIn2S4, (d) ZnIn2S4/TiO2-II的SEM图; ZnIn2S4/TiO2-II的TEM图(e)和HRTEM图(f)

Figure 2. SEM images of (a) MIL-125, (b) TiO2, (c) ZnIn2S4 and (d) ZnIn2S4/TiO2-II; TEM (e) and HRTEM (f) images of ZnIn2S4/TiO2-II

图3. TiO2、ZnIn2S4和ZnIn2S4/TiO2-II的N2吸附-解吸等温曲线(a)及其孔径分布图(b)

Figure 3. N2 adsorption-desorption isotherms (a) and corresponding pore diameter distribution (b) of TiO2, ZnIn2S4, and ZnIn2S4/TiO2-II

图4. ZnIn2S4/TiO2-II的XPS谱图: (a) 全谱图和O 1s (b), Ti 2p (c), S 2p (d), In 3d (e)和Zn 2p (f)的高分辨图谱

Figure 4. XPS spectra of ZnIn2S4/TiO2-II: (a) survey scan spectrum and high resolution spectra of O 1s (b), Ti 2p (c), S 2p (d), In 3d (e) and Zn 2p (f)

图5. TiO2、ZnIn2S4和ZnIn2S4/TiO2-II的UV-vis DRS图谱(a)及其相应的禁带宽度(b); TiO2和ZnIn2S4的XPS价带谱图(c)及其能带位置图(d)

Figure 5. UV-visible DRS spectra of TiO2, ZnIn2S4 and ZnIn2S4/TiO2-II (a) as well as the corresponding optical band gap (b); the XPS valence band spectra (c) and band edge positions (d) of TiO2 and ZnIn2S4

图6. TiO2, ZnIn2S4和ZnIn2S4/TiO2-II的PL谱图(a), 光电流(b), EIS图(c)及Zeta电势(d)

Figure 6. PL spectra (a), photocurrent responses (b), EIS plots (c) and Zeta potential (d) of the TiO2, ZnIn2S4 and ZnIn2S4/TiO2-II

图7. (a)不同光催化剂对RhB的降解效果图; (b) TiO2, ZnIn2S4和TiO2/ZnIn2S4-II对TC的降解效果图; (c)明暗循环(灰色方块)与可见光持续照射(红色圆点)下光催化活性比较

Figure 7. (a) Photocatalytic degradation curves of RhB by different photocatalysts; (b) photocatalytic degradation curves of TC in the presence of TiO2, ZnIn2S4 and TiO2/ZnIn2S4-II; (c) the comparison of photocatalytic activities between light-dark cycles (grey squares) and continuous irradiation (red dots) under visible light

图8. 光降解RhB的动力学曲线

Figure 8. The photodegradation kinetic curves of RhB

图9. ZnIn2S4/TiO2-II的光催化降解循环实验

Figure 9. Photocatalytic degradation cycle experiments of ZnIn2S4/ TiO2-II

图10. 不同俘获剂存在下活性物种俘获实验(a)及其相应的光催化降解率(b)

Figure 10. The capture experiments of active species (a) and corresponding photodegradation rates (b) in the presence of different scavengers

图11. ZnIn2S4/TiO2光催化剂降解RhB的机理图

Figure 11. Schematic of the photocatalytic mechanism for RhB photodegradation on ZnIn2S4/TiO2 photocatalyst

图12. ZnIn2S4/TiO2的制备过程示意图

Figure 12. Schematic diagram of preparation process of ZnIn2S4/TiO2

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2D/3D ZnIn₂S₄/TiO₂复合物的原位构筑及其提高的光催化性能

In-situ Construction of 2D/3D ZnIn₂S₄/TiO₂ with Enhanced Photocatalytic Performance

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