功能性半导体纳米晶组装体系的制备及其可见光响应性能研究
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摘要
光催化技术是指利用半导体材料受到光激发后产生的价带空穴和导电电子进行氧化和还原反应对有机污染物进行降解和光解水产氢的高级技术。光催化技术的关键是光催化剂,但是以TiO2为代表的传统光催化材料存在着不能利用可见光、量子效率低等缺点,进而限制了其应用。发展高效光催化剂需要拓展催化剂对可见光的光学吸收能力和提高光生载流子分离效率。通过对半导体纳米晶材料进行组装,可以利用窗口效应实现催化剂对光的多级吸收；同时,构筑异质结材料,可以为光生电子-空穴分离提供驱动力。本论文围绕以上内容,主要开展了以下几个方面的工作：
(1)采用光辅助电沉积的方法制备了CdSe纳米晶簇负载的TiO2纳米管阵列光电极。在光活化和电沉积反应的协同作用下,制备的CdSe纳米晶簇呈现良好的结晶性能并均匀沉积在电极表面和纳米管孔道内。透射电镜(TEM)和表面光电压谱(SPV)测试表明制备的CdSe纳米晶簇由尺寸不同的CdSe纳米晶粒梯度排列组装而成。在100mW cm-2的可见光照射下,CdSe纳米晶簇负载的TiO2纳米管阵列光电极在0 V(vs. SCE)偏压时,光电流密度达到了16 mA cm-2,比CdSe膜电极提高了8倍。CdSe纳米晶簇组装结构不仅可以实现对可见光的多级吸收,也有利于光生载流子在体系内的矢量传递。
(2)结合超声和水热还原法,制备了石墨烯负载的金属纳米簇(Au、Pt、Pd)复合材料,直径～2.0 nm的金属纳米簇均匀生长在石墨烯表面。XPS谱图表明,与金本征材料相比,负载在石墨烯表面的金属纳米簇的电子结构发生变化,从而具有优异的电学和催化性质。结合沉积-沉淀和光还原方法制备了石墨烯组装的金属纳米晶等离子共振光催化剂Ag@AgCl/RGO,在可见光区域表现出了强烈的Ag纳米晶的等离子共振吸收带。与Ag@AgCl相比,Ag@AgCl/RGO对罗丹明B的光催化降解速率提高了4倍以上。石墨烯的存在提供了激发态Ag纳米晶光生电子快速迁移的通道,从而抑制了等离子共振光催化体系内光生载流子的复合。
(3)采用室温沉积-沉淀法制备了石墨烯氧化物组装的磷酸银微球光催化剂。GO在Ag3PO4生长过程中起表面活性剂作用,Ag3PO4/GO异质结微球的结构形貌可以通过调整GO浓度和石墨烯氧化程度进行调整。可见光下,Ag3PO4/GO异质结微球在4min内实现了对10 ppm罗丹明B的完全降解,与单纯的Ag3PO4相比,光催化速率提高了4倍。活性物种检测试验发现光生空穴和O2·-自由基控制了光催化反应过程,石墨烯氧化物的存在利于Ag3PO4内光生电子-空穴对的分离,从而产生更多的活性氧物种参与光催化反应。
(4)以CdSe/CdS量子点为基本单元,β-环糊精为连接剂,利用超分子作用自组装制备了量子点组装结构。量子点表面负载的β-环糊精以二聚体形式存在,从而在量子点组装体系内形成了纳米空腔。这种新的结构不仅具备量子点的荧光性能,也具备了环糊精的分子识别能力。分析发现环糊精组装的量子点体系的荧光强度随双酚A分子浓度的升高而增强,在双酚A浓度0.04 ppm到2 ppm的浓度范围内,表现出良好的荧光响应特性。
以上结果表明,合理设计半导体纳米晶组装结构,可以显著增强光催化剂对可见光的吸收效果并实现光生载流子在催化剂体系内的高效矢量传递与分离,同时保持了光催化剂的稳定性。本论文对半导体纳米晶组装结构与其光学吸收能力、载流子分离效率之间关系的探索,为设计高效半导体纳米晶光催化剂提供了可行的手段,有利于推动光催化技术在污染控制领域的应用。
Photocatalytic reaction over semiconductor photocatalyst is an advantage process that employing photogenerated hole in valance band and excited electrons in conduction band in semiconductor, which could degrade organic pollutants via oxidation/reduction reaction and generate hydrogen via water splitting. The effectiveness of sunlight-driven photocatalytic processes is mainly dependent on the semiconductor's absorption capacity toward visible light and the quantum yield of photoconversion. However, the traditional photocatalyst, such as TiO2, can not absorb visible light as well as low quantum yield, which limit the development of photocatalysis. Nanostructure architectures assembled by semiconductor nanocrystal with well-defined geometrical shapes would facilitate multilevel absorption toward visible light. The heterojunction in the assembled system can provide a driving force for the seperation of photogenerated charge carriers. In this dissertation, several works have been done as follows:
(1) "Mulberry-like" CdSe nanoclusters with well-defined crystallinity have been assembled into vertically aligned TiO2 nanotubes by photo-assisted electrodeposition method to form new architecture for fabricating semiconductor nanocrystal sensitized photoelectrodes. The multiple staked "mulberry-like" CdSe nanoclusters, caused by the synergistic effect of photoetching and electrodeposition, broaden the absorption spectra to entire visible region with a promising behavior of photoinduced charge separation. A photocurrent density of 16 mA cm-2 was achieved under 100 mW cm-2 visible light illumination with 0 V bias potential (vs. SCE). The remarkable photoresponse should be ascribed to the high-quality of 3-D multij unction structure and the driving force for electron transfer in "mulberry-like" nanoclusters.
(2) Ultrafine metal nanodots with a size of -2.0 nm in a narrow size distribution are uniformly decorated on graphene sheet through a sonolytic followed by hydrothermal reduction route without extra reducing agent. X-rays photoelectron spectroscopy (XPS) spectra suggest the size-dependent alternation of electronic structure of metal nanodot on graphene sheet, giving rise to unusual electronic and catalytic properties. Graphene sheet grafted Ag@AgCl composite is fabricated by photoreducing AgCl/graphene oxide (GO) hybrids prepared by deposition-precipitation method. UV-vis absorption spectra of Ag@AgCl/reduced GO (RGO) hybrids exhibit strong absorbance in the visible region due to the surface plasmon resonance (SPR) absorption of Ag nanocrystal. Compared with bare Ag@AgCl nanoparticle, a four-fold enhancement in the photodegradation rate toward rhodamine B is observed over Ag@AgCl/RGO hybrids under visible light irradiation.
(3) Ag3PO4/graphene oxide (GO) hybrid microsphere was synthesized by a facile deposition-precipitation method. The morphology of the prepared hybrids microspheres could be modulated by the concentration of GO in the starting solution and the degree of oxidation of graphene sheet. In situ assembled Ag3PO4/GO microspheres exhibited almost four-fold enhancement in the photodegradation rate toward rodamine B under visible light compared with that of bare Ag3PO4. The specified photocatalytic experiments revealed that direct hole oxidation and O2·- radicals oxidation governed the photodegradation process over Ag3PO4/GO heteroj unction. This finding indicates that the heterojunction in the hybrids system facilitates charge separation and transfer from photo-excited Ag3PO4, keeping the high reactivity of the photogenerated charge carriers.
(4) Novel three-dimensionally nanostructure derived from CdSe/CdS quantum dot andβ-cyclodextrin was synthesized. Supramolecular interactions between the adjacentβ-cyclodextrins anchored on quantum dots are believed to drive the formation of nanocage structure in the frameworks. The novel nanostructure possesses both the optic properties of quantum dots and the molecule recognition ability of cyclodextrins, which allow a highly sensitive determination of bisphenol A at a dynamic range from 0.04 ppm to 2 ppm via significant fluorescence enhancement.
The above results illuminated that the well-defined nanostructure architectures assembled by semiconductor nanocrystal would efficiently expand the optical absorption of photocatalyst toward visible light and faciliate the photogenerated charge carriers transfer in the photocatalyst system, as well as keep the photostability of photocatalyst. These studies provide a feasible approach to design photocatalyst with high activity, which would promot the application of photocatalytic technology in pollution controlling.
(1)采用光辅助电沉积的方法制备了CdSe纳米晶簇负载的TiO2纳米管阵列光电极。在光活化和电沉积反应的协同作用下,制备的CdSe纳米晶簇呈现良好的结晶性能并均匀沉积在电极表面和纳米管孔道内。透射电镜(TEM)和表面光电压谱(SPV)测试表明制备的CdSe纳米晶簇由尺寸不同的CdSe纳米晶粒梯度排列组装而成。在100mW cm-2的可见光照射下,CdSe纳米晶簇负载的TiO2纳米管阵列光电极在0 V(vs. SCE)偏压时,光电流密度达到了16 mA cm-2,比CdSe膜电极提高了8倍。CdSe纳米晶簇组装结构不仅可以实现对可见光的多级吸收,也有利于光生载流子在体系内的矢量传递。
(2)结合超声和水热还原法,制备了石墨烯负载的金属纳米簇(Au、Pt、Pd)复合材料,直径～2.0 nm的金属纳米簇均匀生长在石墨烯表面。XPS谱图表明,与金本征材料相比,负载在石墨烯表面的金属纳米簇的电子结构发生变化,从而具有优异的电学和催化性质。结合沉积-沉淀和光还原方法制备了石墨烯组装的金属纳米晶等离子共振光催化剂Ag@AgCl/RGO,在可见光区域表现出了强烈的Ag纳米晶的等离子共振吸收带。与Ag@AgCl相比,Ag@AgCl/RGO对罗丹明B的光催化降解速率提高了4倍以上。石墨烯的存在提供了激发态Ag纳米晶光生电子快速迁移的通道,从而抑制了等离子共振光催化体系内光生载流子的复合。
(3)采用室温沉积-沉淀法制备了石墨烯氧化物组装的磷酸银微球光催化剂。GO在Ag3PO4生长过程中起表面活性剂作用,Ag3PO4/GO异质结微球的结构形貌可以通过调整GO浓度和石墨烯氧化程度进行调整。可见光下,Ag3PO4/GO异质结微球在4min内实现了对10 ppm罗丹明B的完全降解,与单纯的Ag3PO4相比,光催化速率提高了4倍。活性物种检测试验发现光生空穴和O2·-自由基控制了光催化反应过程,石墨烯氧化物的存在利于Ag3PO4内光生电子-空穴对的分离,从而产生更多的活性氧物种参与光催化反应。
(4)以CdSe/CdS量子点为基本单元,β-环糊精为连接剂,利用超分子作用自组装制备了量子点组装结构。量子点表面负载的β-环糊精以二聚体形式存在,从而在量子点组装体系内形成了纳米空腔。这种新的结构不仅具备量子点的荧光性能,也具备了环糊精的分子识别能力。分析发现环糊精组装的量子点体系的荧光强度随双酚A分子浓度的升高而增强,在双酚A浓度0.04 ppm到2 ppm的浓度范围内,表现出良好的荧光响应特性。
以上结果表明,合理设计半导体纳米晶组装结构,可以显著增强光催化剂对可见光的吸收效果并实现光生载流子在催化剂体系内的高效矢量传递与分离,同时保持了光催化剂的稳定性。本论文对半导体纳米晶组装结构与其光学吸收能力、载流子分离效率之间关系的探索,为设计高效半导体纳米晶光催化剂提供了可行的手段,有利于推动光催化技术在污染控制领域的应用。
Photocatalytic reaction over semiconductor photocatalyst is an advantage process that employing photogenerated hole in valance band and excited electrons in conduction band in semiconductor, which could degrade organic pollutants via oxidation/reduction reaction and generate hydrogen via water splitting. The effectiveness of sunlight-driven photocatalytic processes is mainly dependent on the semiconductor's absorption capacity toward visible light and the quantum yield of photoconversion. However, the traditional photocatalyst, such as TiO2, can not absorb visible light as well as low quantum yield, which limit the development of photocatalysis. Nanostructure architectures assembled by semiconductor nanocrystal with well-defined geometrical shapes would facilitate multilevel absorption toward visible light. The heterojunction in the assembled system can provide a driving force for the seperation of photogenerated charge carriers. In this dissertation, several works have been done as follows:
(1) "Mulberry-like" CdSe nanoclusters with well-defined crystallinity have been assembled into vertically aligned TiO2 nanotubes by photo-assisted electrodeposition method to form new architecture for fabricating semiconductor nanocrystal sensitized photoelectrodes. The multiple staked "mulberry-like" CdSe nanoclusters, caused by the synergistic effect of photoetching and electrodeposition, broaden the absorption spectra to entire visible region with a promising behavior of photoinduced charge separation. A photocurrent density of 16 mA cm-2 was achieved under 100 mW cm-2 visible light illumination with 0 V bias potential (vs. SCE). The remarkable photoresponse should be ascribed to the high-quality of 3-D multij unction structure and the driving force for electron transfer in "mulberry-like" nanoclusters.
(2) Ultrafine metal nanodots with a size of -2.0 nm in a narrow size distribution are uniformly decorated on graphene sheet through a sonolytic followed by hydrothermal reduction route without extra reducing agent. X-rays photoelectron spectroscopy (XPS) spectra suggest the size-dependent alternation of electronic structure of metal nanodot on graphene sheet, giving rise to unusual electronic and catalytic properties. Graphene sheet grafted Ag@AgCl composite is fabricated by photoreducing AgCl/graphene oxide (GO) hybrids prepared by deposition-precipitation method. UV-vis absorption spectra of Ag@AgCl/reduced GO (RGO) hybrids exhibit strong absorbance in the visible region due to the surface plasmon resonance (SPR) absorption of Ag nanocrystal. Compared with bare Ag@AgCl nanoparticle, a four-fold enhancement in the photodegradation rate toward rhodamine B is observed over Ag@AgCl/RGO hybrids under visible light irradiation.
(3) Ag3PO4/graphene oxide (GO) hybrid microsphere was synthesized by a facile deposition-precipitation method. The morphology of the prepared hybrids microspheres could be modulated by the concentration of GO in the starting solution and the degree of oxidation of graphene sheet. In situ assembled Ag3PO4/GO microspheres exhibited almost four-fold enhancement in the photodegradation rate toward rodamine B under visible light compared with that of bare Ag3PO4. The specified photocatalytic experiments revealed that direct hole oxidation and O2·- radicals oxidation governed the photodegradation process over Ag3PO4/GO heteroj unction. This finding indicates that the heterojunction in the hybrids system facilitates charge separation and transfer from photo-excited Ag3PO4, keeping the high reactivity of the photogenerated charge carriers.
(4) Novel three-dimensionally nanostructure derived from CdSe/CdS quantum dot andβ-cyclodextrin was synthesized. Supramolecular interactions between the adjacentβ-cyclodextrins anchored on quantum dots are believed to drive the formation of nanocage structure in the frameworks. The novel nanostructure possesses both the optic properties of quantum dots and the molecule recognition ability of cyclodextrins, which allow a highly sensitive determination of bisphenol A at a dynamic range from 0.04 ppm to 2 ppm via significant fluorescence enhancement.
The above results illuminated that the well-defined nanostructure architectures assembled by semiconductor nanocrystal would efficiently expand the optical absorption of photocatalyst toward visible light and faciliate the photogenerated charge carriers transfer in the photocatalyst system, as well as keep the photostability of photocatalyst. These studies provide a feasible approach to design photocatalyst with high activity, which would promot the application of photocatalytic technology in pollution controlling.
引文
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