多孔金属氧化物半导体材料的构建与性能的研究
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摘要
TiO2由于具有高化学稳定性、良好的光活性、低成本和无毒等特点而成为一种非常理想的半导体材料。但是由于TiO2禁带宽度很大(3.2eV),因此其仅能被太阳光中少于4%的紫外光所激发,严重限制其对于太阳光利用率。如何提高TiO2光的响应范围和量子效率成为光电材料研究的热点。本论文主要制备了几种非常有效的可见光催化剂：利用溶胶凝胶法制备N掺杂的TiO2反蛋白石结构薄膜；通过连续离子层吸附法制备了在CdS敏化N-TiO2反蛋白石薄膜；另外我们还通过一步溶剂热的方法制备了一种松果状多孔Fe3O4@Cu2O/Cu复合物,具有很高的光催化活性和稳定性。论文主要研究内容如下：
1.通过乳液聚合的方法制备了多种不同粒径的PS微球,然后利用垂直沉积的方法将PS球的胶体光子晶体模板组装到载玻片或FTO导电玻璃上,然后采用溶胶凝胶法在PS球光子晶体膜表面生成N掺杂-TiO2的前躯体,最后通过煅烧形成N-TiO2的反蛋白石薄膜结构。主要讨论了不同钛源的溶胶前驱体对薄膜的性质的影响,以及前驱体溶胶浓度对反蛋白石结构的影响。
2.利用连续离子层吸附的方法在N-TiO2反蛋白石骨架上复合CdS半导体材料。紫外可见漫反射光谱的测试显示CdS半导体材料的敏化增强了TiO2反蛋白石薄膜的光响应范围,提高了TiO2对于光的吸收率。光电流测试表明,CdS敏化的N-TiO2反蛋白石薄膜产生的光电流强度是TiO2反蛋白石薄膜的8倍,是N-TiO2反蛋白石薄膜的4倍。这种复合光电薄膜有望在太阳能电池和光解水等方面有得到应用。
3.通过一步溶剂热的方法制备了一种松果状多孔Fe3O4@Cu2O/Cu复合物,这种产物是由许多厚度为100nm的纳米片组成的空心结构。该复合物对甲基橙染料具有非常好的光催化降解效率,在光照20分钟后降解效率达到96%。另外该复合物具有比Fe3O4@Cu2O更好的光降解效率和稳定性,表明Cu存在于Fe3O4@Cu2O表面,不仅提高了Cu2O的催化活性,而且对Cu2O的光腐蚀具有抑制作用,提高了复合物的稳定性。磁性材料Fe3O4可以使产物通过磁性分离有效的回收和循环利用。这种新型的Fe3O4@Cu2O/Cu复合材料有望在染料污水处理和环境清洁方面得到应用。
Because of excellent chemical stability, high photoactivity, relatively low cost, and nontoxicity, TiO2has been considered as a promising semiconductor photocatalyst for energy and environment-related applications. However, as a large bandgap semiconductor (3.2eV), TiO2could only be activated by UV light which makes up only4%of the solar spectrum. To more efficiently utilize solar energy, it is highly desired to extend the photoresponse of TiO2-based materials to visible light region. This thesis focuses on developing some efficient visible light photocatalysts including N-dope TiO2inverse opals, CdS sensitized N-TiO2inverse opals and pine cone-like porous Fe3O4@Cu2O/Cu composites.
The main contents are summarized as follows:
1. The first chapter describes a facile emulsion polymerization approach to synthesize highly monodisperse polystyrene (PS) spheres using potassium persulfate as the initiator and polyvinylpyrrolidone (PVP) as a stabilizer, respectively. The PS colloidal photonic crystals films were fabricated on a microscope slides or FTO glass substrate by using vertical deposition method at45℃. Then a sol-gel process was used to assemble N-TiO2onto the PS photonic crystals films, followed by a calcination process to remove PS templates. The effects of titanium source and concentration on the resulting structure were investigated. Enhanced visible light photocatalytic activity was observed in this unique structure.
2. In the second chapter, CdS sensitized nitrogen doped titanium oxide inverse opal structure has been synthesized by an ionic layer adsorption and reaction (SILAR) route. The3D percolated periodical inverse opal structure provides numerous nucleation sites for the following CdS deposition. Also, the high surface area is beneficial for the photocatalysis process. Uv-vis diffuse reflectance spectra indicates that the CdS-N-TiO2inverse opals exhibits a good visible light absorption ability.The photocurrent density is enhanced by8times through CdS QD sensitization in comparison to the pristine TiO2inverse opal photoanodes. The as-obtained film may have potential applications in solar cells, hydrogen generation and so on.
3. In the last chapter, novel pine cone-like Fe3O4@Cu2O/Cu nanocomposites (NCs) with photomagnetic difunction were successfully synthesized via a one-pot solvothermal method on Fe3O4without any additional linker or reducer. The products were orderly assembled into many sheets with an average thickness of～100nm, possessing a porous structure. The samples show excellent photocatalytic activity such that MO degradation efficiency is about96%at an irradiation time of20min under visible light. Also, the composites present higher stability than Fe3O4@Cu2O. The above results demonstrate that Cu could improve the photocatalytic activity of NCs and also inhibit the photocorrosion behavior of NCs. These novel Fe3O4@Cu2O/Cu composite materials are ideal candidates in water treatment and environmental cleaning as well as in magnetic applications, etc.
1.通过乳液聚合的方法制备了多种不同粒径的PS微球,然后利用垂直沉积的方法将PS球的胶体光子晶体模板组装到载玻片或FTO导电玻璃上,然后采用溶胶凝胶法在PS球光子晶体膜表面生成N掺杂-TiO2的前躯体,最后通过煅烧形成N-TiO2的反蛋白石薄膜结构。主要讨论了不同钛源的溶胶前驱体对薄膜的性质的影响,以及前驱体溶胶浓度对反蛋白石结构的影响。
2.利用连续离子层吸附的方法在N-TiO2反蛋白石骨架上复合CdS半导体材料。紫外可见漫反射光谱的测试显示CdS半导体材料的敏化增强了TiO2反蛋白石薄膜的光响应范围,提高了TiO2对于光的吸收率。光电流测试表明,CdS敏化的N-TiO2反蛋白石薄膜产生的光电流强度是TiO2反蛋白石薄膜的8倍,是N-TiO2反蛋白石薄膜的4倍。这种复合光电薄膜有望在太阳能电池和光解水等方面有得到应用。
3.通过一步溶剂热的方法制备了一种松果状多孔Fe3O4@Cu2O/Cu复合物,这种产物是由许多厚度为100nm的纳米片组成的空心结构。该复合物对甲基橙染料具有非常好的光催化降解效率,在光照20分钟后降解效率达到96%。另外该复合物具有比Fe3O4@Cu2O更好的光降解效率和稳定性,表明Cu存在于Fe3O4@Cu2O表面,不仅提高了Cu2O的催化活性,而且对Cu2O的光腐蚀具有抑制作用,提高了复合物的稳定性。磁性材料Fe3O4可以使产物通过磁性分离有效的回收和循环利用。这种新型的Fe3O4@Cu2O/Cu复合材料有望在染料污水处理和环境清洁方面得到应用。
Because of excellent chemical stability, high photoactivity, relatively low cost, and nontoxicity, TiO2has been considered as a promising semiconductor photocatalyst for energy and environment-related applications. However, as a large bandgap semiconductor (3.2eV), TiO2could only be activated by UV light which makes up only4%of the solar spectrum. To more efficiently utilize solar energy, it is highly desired to extend the photoresponse of TiO2-based materials to visible light region. This thesis focuses on developing some efficient visible light photocatalysts including N-dope TiO2inverse opals, CdS sensitized N-TiO2inverse opals and pine cone-like porous Fe3O4@Cu2O/Cu composites.
The main contents are summarized as follows:
1. The first chapter describes a facile emulsion polymerization approach to synthesize highly monodisperse polystyrene (PS) spheres using potassium persulfate as the initiator and polyvinylpyrrolidone (PVP) as a stabilizer, respectively. The PS colloidal photonic crystals films were fabricated on a microscope slides or FTO glass substrate by using vertical deposition method at45℃. Then a sol-gel process was used to assemble N-TiO2onto the PS photonic crystals films, followed by a calcination process to remove PS templates. The effects of titanium source and concentration on the resulting structure were investigated. Enhanced visible light photocatalytic activity was observed in this unique structure.
2. In the second chapter, CdS sensitized nitrogen doped titanium oxide inverse opal structure has been synthesized by an ionic layer adsorption and reaction (SILAR) route. The3D percolated periodical inverse opal structure provides numerous nucleation sites for the following CdS deposition. Also, the high surface area is beneficial for the photocatalysis process. Uv-vis diffuse reflectance spectra indicates that the CdS-N-TiO2inverse opals exhibits a good visible light absorption ability.The photocurrent density is enhanced by8times through CdS QD sensitization in comparison to the pristine TiO2inverse opal photoanodes. The as-obtained film may have potential applications in solar cells, hydrogen generation and so on.
3. In the last chapter, novel pine cone-like Fe3O4@Cu2O/Cu nanocomposites (NCs) with photomagnetic difunction were successfully synthesized via a one-pot solvothermal method on Fe3O4without any additional linker or reducer. The products were orderly assembled into many sheets with an average thickness of～100nm, possessing a porous structure. The samples show excellent photocatalytic activity such that MO degradation efficiency is about96%at an irradiation time of20min under visible light. Also, the composites present higher stability than Fe3O4@Cu2O. The above results demonstrate that Cu could improve the photocatalytic activity of NCs and also inhibit the photocorrosion behavior of NCs. These novel Fe3O4@Cu2O/Cu composite materials are ideal candidates in water treatment and environmental cleaning as well as in magnetic applications, etc.
引文
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[1]J. Yang; X. Zhang; H. Liu, et al. Heterostructured TiO2/WO3 porous microspheres:Preparation, characterization and photocatalytic properties [J]. Catalysis Today,2013,201:195-202.
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[6]U. Shaislamov; H. Kim, B.L. Yang. CdS-sensitized TiO2 photoelectrodes for quantum dots-based solar cells [J]. Journal of Materials Research,2013,28(3): 497-501.
[7]C. Cheng; S.K. Karuturi; L. Liu, et al. Quantum-Dot-Sensitized TiO2 Inverse Opals for Photoelectrochemical Hydrogen Generation [J]. Small,2012,8(1):37-42.
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[9]Y. Guo; H. Zhang; Y. Wang, et al. Controlled Growth and Photocatalytic Properties of CdS Nanocrystals Implanted in Layered Metal Hydroxide Matrixes [J]. The Journal of Physical Chemistry B,2005,109(46):21602-21607.
[1]Z. Seddigi. Removal of Alizarin Yellow Dye from Water Using Zinc Doped WO3 Catalyst [J]. Bulletin of Environmental Contamination and Toxicology,2010,84(5): 564-567.
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[3]P. Lei; F. Wang; X. Gao, et al. Immobilization of TiO2 nanoparticles in polymeric substrates by chemical bonding for multi-cycle photodegradation of organic pollutants [J]. Journal of Hazardous Materials,2012,227-228(0):185-194.
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[8]L. Kong; W. Chen; D. Ma, et al. Size control of Au@Cu2O octahedra for excellent photocatalytic performance [J]. Journal of Materials Chemistry,2012, 22(2):719-724.
[9]C.-H. Kuo; Y.-C. Yang; S. Gwo, et al. Facet-Dependent and Au Nanocrystal-Enhanced Electrical and Photocatalytic Properties of Au-Cu2O Core-Shell Heterostructures [J]. Journal of the American Chemical Society,2010, 133(4):1052-1057.
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[13]T. Zeng; X.L. Zhang; Y.R. Ma, et al. A novel Fe3O4-graphene-Au multifunctional nanocomposite:green synthesis and catalytic application [J]. Journal of Materials Chemistry,2012,22(35):18658-18663.
[14]M. Zhang; X.W. He; L.X. Chen, et al. Preparation of IDA-Cu functionalized core-satellite Fe3O4/polydopamine/Au magnetic nanocomposites and their application for depletion of abundant protein in bovine blood [J]. Journal of Materials Chemistry,2010,20(47):10696-10704.
[15]A. Tschope; M.L. Trudeau, J.Y. Ying. Redox Properties of Nanocrystalline Cu-Doped Cerium Oxide Studied by Isothermal Gravimetric Analysis and X-ray Photoelectron Spectroscopy [J]. The Journal of Physical Chemistry B,1999,103(42): 8858-8863.
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[1]J. Yang; X. Zhang; H. Liu, et al. Heterostructured TiO2/WO3 porous microspheres:Preparation, characterization and photocatalytic properties [J]. Catalysis Today,2013,201:195-202.
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[3]U.V. Desai; C. Xu; J. Wu, et al. Hybrid TiO2-SnO2 Nanotube Arrays for Dye-Sensitized Solar Cells [J]. The Journal of Physical Chemistry C,2013,117(7): 3232-3239.
[4]L.B. Reutergadh, M. Iangphasuk. Photocatalytic decolourization of reactive azo dye:A comparison between TiO2 and us photocatalysis [J]. Chemosphere,1997, 35(3):585-596.
[5]X.T. Sui; H.Z. Tao; X.C. Lou, et al. CdS quantum dots-sensitized TiO2 nanotube arrays for solar cells [J]. Journal of Wuhan University of Technology-Materials Science Edition,2013,28(1):17-21.
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[1]Z. Seddigi. Removal of Alizarin Yellow Dye from Water Using Zinc Doped WO3 Catalyst [J]. Bulletin of Environmental Contamination and Toxicology,2010,84(5): 564-567.
[2]M.A. Rauf, S.S. Ashraf. Radiation induced degradation of dyes—An overview [J]. Journal of Hazardous Materials,2009,166(1):6-16.
[3]P. Lei; F. Wang; X. Gao, et al. Immobilization of TiO2 nanoparticles in polymeric substrates by chemical bonding for multi-cycle photodegradation of organic pollutants [J]. Journal of Hazardous Materials,2012,227-228(0):185-194.
[4]M. Pang, H.C. Zeng. Highly Ordered Self-Assemblies of Submicrometer Cu2O Spheres and Their Hollow Chalcogenide Derivatives [J].Langmuir,2010,26(8): 5963-5970.
[5]S.-K. Li; X. Guo; Y. Wang, et al. Rapid synthesis of flower-like Cu2O architectures in ionic liquids by the assistance of microwave irradiation with high photochemical activity [J]. Dalton Transactions,2011,40(25):6745-6750.
[6]Y. Bessekhouad; D. Robert, J.V. Weber. Photocatalytic activity of Cu2O/TiO2, Bi2O3/TiO2 and ZnMn2O4/TiO2 heterojunctions [J]. Catalysis Today,2005, 101(3-4):315-321.
[7]B. Zhou; H. Wang; Z. Liu, et al. Enhanced photocatalytic activity of flowerlike Cu2O/Cu prepared using solvent-thermal route [J]. Materials Chemistry and Physics, 2011,126(3):847-852.
[8]L. Kong; W. Chen; D. Ma, et al. Size control of Au@Cu2O octahedra for excellent photocatalytic performance [J]. Journal of Materials Chemistry,2012, 22(2):719-724.
[9]C.-H. Kuo; Y.-C. Yang; S. Gwo, et al. Facet-Dependent and Au Nanocrystal-Enhanced Electrical and Photocatalytic Properties of Au-Cu2O Core-Shell Heterostructures [J]. Journal of the American Chemical Society,2010, 133(4):1052-1057.
[10]Z. Wang; S. Zhao; S. Zhu, et al. Photocatalytic synthesis of M/Cu2O (M=Ag, Au) heterogeneous nanocrystals and their photocatalytic properties [J]. CrystEngComm,2011,13(7):2262-2267.
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[12]Q. Hua; F. Shi; K. Chen, et al. Cu2O-Au nanocomposites with novel structures and remarkable chemisorption capacity and photocatalytic activity [J]. Nano Research,2011,4(10):948-962.
[13]T. Zeng; X.L. Zhang; Y.R. Ma, et al. A novel Fe3O4-graphene-Au multifunctional nanocomposite:green synthesis and catalytic application [J]. Journal of Materials Chemistry,2012,22(35):18658-18663.
[14]M. Zhang; X.W. He; L.X. Chen, et al. Preparation of IDA-Cu functionalized core-satellite Fe3O4/polydopamine/Au magnetic nanocomposites and their application for depletion of abundant protein in bovine blood [J]. Journal of Materials Chemistry,2010,20(47):10696-10704.
[15]A. Tschope; M.L. Trudeau, J.Y. Ying. Redox Properties of Nanocrystalline Cu-Doped Cerium Oxide Studied by Isothermal Gravimetric Analysis and X-ray Photoelectron Spectroscopy [J]. The Journal of Physical Chemistry B,1999,103(42): 8858-8863.
[16]Y. Sun; B. Gates; B. Mayers, et al. Crystalline Silver Nanowires by Soft Solution Processing [J]. Nano Letters,2002,2(2):165-168.
[17]J. Li, H.C. Zeng. Hollowing Sn-Doped TiO2 Nanospheres via Ostwald Ripening [J]. Journal of the American Chemical Society,2007,129(51): 15839-15847.
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[19]Z. Ai; W. Ho; S. Lee, et al. Efficient Photocatalytic Removal of NO in Indoor Air with Hierarchical Bismuth Oxybromide Nanoplate Microspheres under Visible Light [J]. Environmental Science & Technology,2009,43(11):4143-4150.
[20]L. Huang; F. Peng; H. Yu, et al. Preparation of cuprous oxides with different sizes and their behaviors of adsorption, visible-light driven photocatalysis and photocorrosion [J]. Solid State Sciences,2009,11(1):129-138.