高效微纳结构TiO_2基光催化剂的制备及其光催化性能研究
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摘要
以TiO_2为基础的半导体光催化剂的在环境治理方面研究一直处于实验室研究阶段,没有达到实际应用,我们利用传统的掺杂及复合改性技术结合新兴的纳米材料制备技术对具有纳米结构的TiO_2光催化剂进行改性,然后利用改性后的光催化剂降解对氯苯酚以测试其活性,再结合现代表征技术,对光催化活性提高的机理和进行了细致,合理地分析.主要进行了高效微纳结构TiO_2基光催化剂的制备及其光催化性能研究。通过掺杂及复合改性技术制备出了Ni2+离子表面处理TiO_2纳米粒子光催化剂、B离子掺杂TiO_2光催化剂及SnO_2/TiO_2.N掺杂复合光催化剂,均实现了催化剂紫外和可见光催化活性的提高。在对催化剂的能带结构、表面缺陷等分忻表征的基础上,对这些催化剂的光催化机理进行了深入的探讨。在此基础上他成功地制备了Au与海胆状TiO_2复合微纳结构光催化剂和In离子掺杂TiO_2纳米管可见光催化剂,在光催化降解实验中分别得到了提高的紫外和可见光催化活性,结合表征数据,他在微观水平上探讨了界面光催化反应和相关的紫外及可见光催化机理。这些研究结果为新型纳米TiO_2基光催化剂的制备提供了有益的启示。
TiO_2 photocatalysis has attracted extensive attention as a promising technique for the degradation of inorganic and organic pollutants in water and air. However, TiO_2 photocatalysts have two inherent and significant drawbacks; the one is, the TiO_2 photocatalysts owned wide band-gap can not use solar irradiation or interior lighting efficiently, the other is, the photogenerated charge carriers (hole-electron pairs) can recombine. Therefore, to achieve the practical application of TiO_2, it is important to enhance the absorption of visible light and decrease the recombination of photogenerated carriers. Furthermore, the mechanisms of photocatalysis under visible light are still not clear, there is no suitable theoretical guidance for synthesis of high efficient photocatalyst under visible light.
The high efficient TiO_2 photocatalysts with nano-micro structures were fabricated by combining the traditional doping and coupling methods with the novel nanotechnology. The photodegradation of 4-chlorophenol was employed to evaluate the photocatalytic activities of the photocatalysts. The reasons of the enhanced photocatalytic activities had been investigated with the help of X-ray diffraction (XRD), Diffuse reflectance UV-Vis spectra, X-ray photoelectron spectra (XPS), surface photovoltage spectra (SPS) and so on.
The summary of the work are as follows:
1. Samples of pure TiO_2 and TiO_2-xBx were obtained with Ti (OC4H9)4 by sol-gel methods. Compared with the pure TiO_2, the samples of TiO_2-xBx exhibited higher photocatalytic activity under both ultraviolet and visible light irradiation. The reasons were discussed, based on the characterization with XRD, RAMAN, XPS, UV-Vis and PL spectra. The lattice O is substituted by B, and the orbital of B2p is mixed with O_2p orbital, which is responsible for the band gap narrowing. The raise of the photocatalytic activity is chiefly because B doping enhanced the absorption of visible light, and promoted the separation of photogenerated carriers.
2. In this work, sol-gel process was employed to prepare TiO_2 and Nickel-doped TiO_2 powder .The photodegradation of 4-chlorophenol was employed to evaluate the photocatalytic activities of the catalysts. Compared to TiO_2, Nickel -doped TiO_2 exhibited improved activity for degradation of 4-chlorophenol under both ultraviolet and visible light irradiation. The properties of these catalysts were investigated with the help of XRD, UV-Vis, IR, Raman spectra, SPS and other analytic methods. We found that Ni2+ was chemisorbed on the surface of TiO_2 and formed the ONiOO which introduced the energy level of surface states 2.84 eV above the valence band. This energy level not only generated response to visible light but also promoted the separation of photogenerated carriers. Thus, the activity under both ultraviolet and visible light irradiation was increased.
3. Indium doped TiO_2 nanotubes were fabricated by a two-step pre-doping method. It was found that the TiO_2 nanotubes with indium doped content at 3% exhibited the best photocatalytic activity being over twice as much as that of pure TiO_2 nanotubes on the photocatalytic degradation of 4-chlorophenol under visible light. Based on XRD, XPS and SPS, it can be inferred that when the doped content is low, the indium ion substitutes Ti into the TiO_2 lattice forming the InxTi1-xO_2 structure and the In doped energy-band narrows the band gap by mixing with Ti 3d states. With increasing the doped content, In2O3 comes up on the surface of InxTi1-xO_2 nanotubes to form the InxTi1-xO_2/In2O3 composite structure. This composite structure efficiently enhances the visible light response, promotes photogenerated carriers separation and increases the utilization of photogenerated carriers in photocatalytic reactions at the solid/liquid interface, resulting in the higher photocatalytic activity under visible light.
4. A composite photocatalyst with novel nanostructure was prepared by deposition of Au nanoparticles on needles of sea-urchin-like TiO_2 (s-TiO_2). The Au/s-TiO_2 composite photocatalyst presented higher photocatalytic activity than pure s-TiO_2 under ultraviolet irradiation. IR spectra and XPS analysis suggested that the two components, Au and TiO_2, in the composite might be linked by–O–C(=O)– groups. The transfer process of photogenerated carriers at the interface of s-TiO_2 and Au nanoparticles and the shift of Fermi level of the composite were inferred by SPS. The improved photocatalytic activity of the composite photocatalyst was attributed to the promoted utilization efficiency of the photogenerated carriers upon the deposition of the Au nanoparticles on the needles of s-TiO_2.
5. The SnO_2/TiO_2-N composite photocatalysts were prepared by depositing SnO_2 onto nitrogen doped TiO_2 nanoparticles. The composite catalysts present much higher photocatalytic activity than TiO_2 and nitrogen-doped TiO_2 under both ultraviolet and visible light irradiation. Diffuse reflectance UV-Vis spectra, XPS analysis and IR spectra show that the nitrogen species existed with two states: the doped N with responsibility for visible light response, the other N specie linking to Sn atom without contribution to visible light response. The enhanced visible light response caused by doped N and the promoted separation of photogenerated carrier driven by coupling with SnO_2 will be attributed to the higher light photocatalytic activity.
TiO_2 photocatalysis has attracted extensive attention as a promising technique for the degradation of inorganic and organic pollutants in water and air. However, TiO_2 photocatalysts have two inherent and significant drawbacks; the one is, the TiO_2 photocatalysts owned wide band-gap can not use solar irradiation or interior lighting efficiently, the other is, the photogenerated charge carriers (hole-electron pairs) can recombine. Therefore, to achieve the practical application of TiO_2, it is important to enhance the absorption of visible light and decrease the recombination of photogenerated carriers. Furthermore, the mechanisms of photocatalysis under visible light are still not clear, there is no suitable theoretical guidance for synthesis of high efficient photocatalyst under visible light.
The high efficient TiO_2 photocatalysts with nano-micro structures were fabricated by combining the traditional doping and coupling methods with the novel nanotechnology. The photodegradation of 4-chlorophenol was employed to evaluate the photocatalytic activities of the photocatalysts. The reasons of the enhanced photocatalytic activities had been investigated with the help of X-ray diffraction (XRD), Diffuse reflectance UV-Vis spectra, X-ray photoelectron spectra (XPS), surface photovoltage spectra (SPS) and so on.
The summary of the work are as follows:
1. Samples of pure TiO_2 and TiO_2-xBx were obtained with Ti (OC4H9)4 by sol-gel methods. Compared with the pure TiO_2, the samples of TiO_2-xBx exhibited higher photocatalytic activity under both ultraviolet and visible light irradiation. The reasons were discussed, based on the characterization with XRD, RAMAN, XPS, UV-Vis and PL spectra. The lattice O is substituted by B, and the orbital of B2p is mixed with O_2p orbital, which is responsible for the band gap narrowing. The raise of the photocatalytic activity is chiefly because B doping enhanced the absorption of visible light, and promoted the separation of photogenerated carriers.
2. In this work, sol-gel process was employed to prepare TiO_2 and Nickel-doped TiO_2 powder .The photodegradation of 4-chlorophenol was employed to evaluate the photocatalytic activities of the catalysts. Compared to TiO_2, Nickel -doped TiO_2 exhibited improved activity for degradation of 4-chlorophenol under both ultraviolet and visible light irradiation. The properties of these catalysts were investigated with the help of XRD, UV-Vis, IR, Raman spectra, SPS and other analytic methods. We found that Ni2+ was chemisorbed on the surface of TiO_2 and formed the ONiOO which introduced the energy level of surface states 2.84 eV above the valence band. This energy level not only generated response to visible light but also promoted the separation of photogenerated carriers. Thus, the activity under both ultraviolet and visible light irradiation was increased.
3. Indium doped TiO_2 nanotubes were fabricated by a two-step pre-doping method. It was found that the TiO_2 nanotubes with indium doped content at 3% exhibited the best photocatalytic activity being over twice as much as that of pure TiO_2 nanotubes on the photocatalytic degradation of 4-chlorophenol under visible light. Based on XRD, XPS and SPS, it can be inferred that when the doped content is low, the indium ion substitutes Ti into the TiO_2 lattice forming the InxTi1-xO_2 structure and the In doped energy-band narrows the band gap by mixing with Ti 3d states. With increasing the doped content, In2O3 comes up on the surface of InxTi1-xO_2 nanotubes to form the InxTi1-xO_2/In2O3 composite structure. This composite structure efficiently enhances the visible light response, promotes photogenerated carriers separation and increases the utilization of photogenerated carriers in photocatalytic reactions at the solid/liquid interface, resulting in the higher photocatalytic activity under visible light.
4. A composite photocatalyst with novel nanostructure was prepared by deposition of Au nanoparticles on needles of sea-urchin-like TiO_2 (s-TiO_2). The Au/s-TiO_2 composite photocatalyst presented higher photocatalytic activity than pure s-TiO_2 under ultraviolet irradiation. IR spectra and XPS analysis suggested that the two components, Au and TiO_2, in the composite might be linked by–O–C(=O)– groups. The transfer process of photogenerated carriers at the interface of s-TiO_2 and Au nanoparticles and the shift of Fermi level of the composite were inferred by SPS. The improved photocatalytic activity of the composite photocatalyst was attributed to the promoted utilization efficiency of the photogenerated carriers upon the deposition of the Au nanoparticles on the needles of s-TiO_2.
5. The SnO_2/TiO_2-N composite photocatalysts were prepared by depositing SnO_2 onto nitrogen doped TiO_2 nanoparticles. The composite catalysts present much higher photocatalytic activity than TiO_2 and nitrogen-doped TiO_2 under both ultraviolet and visible light irradiation. Diffuse reflectance UV-Vis spectra, XPS analysis and IR spectra show that the nitrogen species existed with two states: the doped N with responsibility for visible light response, the other N specie linking to Sn atom without contribution to visible light response. The enhanced visible light response caused by doped N and the promoted separation of photogenerated carrier driven by coupling with SnO_2 will be attributed to the higher light photocatalytic activity.
引文
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