纳米粒子的组装及其与导电聚合物的复合
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摘要
由于具有小尺寸、大比表面积等特性,纳米粒子拥有特殊的光学、磁学、电学及催化等性质,因此受到人们越来越密切的关注。目前,人们利用多种方法制备了具有不同尺寸和形貌的纳米粒子,并借助表面接枝改性技术,将含有功能性基团的分子修饰在它们的表面,为实现纳米粒子的组装提供了条件。在进一步的研究中,人们以这些功能化的纳米粒子为基本结构单元,通过范德华力、静电力、分子间氢键等超分子作用力,将它们组装成了具有不同形貌的组装体,从而为纳米器件的设计、构筑及应用奠定了基础。然而,稳定性差、容易聚集、不易长期存放等缺点是纳米粒子及其组装体所普遍存在的问题。为了解决这些问题,人们将聚合物引入纳米粒子的体系中。一方面,聚合物的引入提高了纳米粒子及其组装结构的稳定性;另一方面,由于纳米粒子的存在使得聚合物的强度、韧性等性能得到提高,从而实现了纳米粒子与聚合物功能的集成。在本文中我们首先以金纳米粒子为基本结构单元,通过改变实验条件实现了纳米粒子在硅片上的可控自组装,这对进一步理解带电荷纳米粒子的自组装行为具有很重要的意义。然后,我们采用种子法制备了具有花形结构的金纳米粒子,并得到了其在液-液界面的二维组装结构,这种组装结构在表面拉曼增强上具有潜在的应用前景。接下来,我们将聚合物引入到纳米粒子的组装体系中,成功地制备了聚吡咯(PPy)包覆金纳米簇的核壳复合物,此复合物有很好的稳定性并且对硼氢化钠还原亚甲基蓝的反应有良好的催化活性和可重复利用性。最后,我们利用原位聚合的方法制备了Fe_3O_4/SiO_2/PPy复合物,其中PPy壳层的厚度可以通过改变体系中吡咯单体的用量来调控。PPy具有很好的稳定性和生物相容性,因此我们所制备的Fe_3O_4/SiO_2/PPy复合物在生物医用上具有潜在的应用前景。
Nanoparticles (NPs) have attracted much attention due to their unique optical properties, magnetic properties and catalytic properties. In recent years, various methods have been used in synthesis NPs with different sizes and morphologies. These as-prepared NPs were using as building blocks to fabricate various self-assembly structures whose morphologes looked like chain, band and sphere, through van der Waals interaction, electrostatic interaction, hydrogen bond, and so forth. These omnifarious nanostructures displayed bright prospect for applications in nano-design and nano-device.
However, fragileness and aggregation were usually present in NPs and their self-assembly structures. In order to solve these problems, various functional polymers were introduced into the system. On one hand, polymers could improve the stability of NPs and their self-assembly structures. On the other hand, the existence of NPs could enhance the mechanical properties of polymers.
In chapter 2, sodium citrate stabilized gold (Au) NPs were prepared. Then, TGA-capped Au NPs were prepared by ligand exchange. The self-assembly behaviors of Au NPs on substrate were carefully investigated by changing the experimental conditions such as volume ratios of water/acetone, species of ligands and temperature. With decreasing the volume ratios of water/acetone, the dendritic grade of self-assembly structures increased. When the volume ratios of water/acetone were the same, the self-assembly structures of TGA-capped Au NPs had less branches than that of sodium citrate-stabilized Au NPs. Low temperature usually increased the dendritic grade of self-assembly structure. We have investigated these self-assembly behaviors from three different aspects including interparticle interaction, the mobile rate of NPs, and the evaporation rate of the solvent. The theory explanation was quite accordance with the experimental phenomenon. Therefore, our studies were useful for understanding the complex mechanism of the self-assembly of charged NPs, and indicated a protocol to NP-based nano- or micro-structures with controlled mophologies.
In chapter 3, we have successfully synthesized flower-like Au NPs using seeding approach. The results indicated dosage of hydroquinone played a key role in the formation of flower-like NPs. When the amount of hydroquinone was 100μL, no flower-like Au NPs appeared in the system. When the amount of hydroquinone and seed were 300μL and 50μL, respectively, flower-like Au NPs appeared in the system. However, further increasing the amount of hydroquinone, the size and morphology of NPs did not change. In the experiment, when the amount of hydroquinone was 1000μL, the size and morphology of flower-like NPs could be tuned through the dosage of seeds. NPs with different sizes and morphologies were also assembled on the liquid-liquid interface through reducing the surface charge of NPs. This self-assembly structure has potential application in surface enhanced Raman scattering.
In chapter 4, first, we have successfully synthesized Au superparticle/polypyrrole (SP/PPy) composites. In the preparation process, poly (N-vinylpyrrolidone) (PVP) played a key role; without it, PPy could not cover on the surface of SPs and form a complete shell. The influence of pyrrole monomer concentration on the morphology and shell thickness of resulting composites was also investigated in this chapter. The experimental results indicated the optimized concentrations of pyrrole monomer ranged between 1.14 and 2.28 mM. If the concentration was too high, pure PPy NPs would appear in the system. If the concentration was too low, pyrrole monomer would polymerize into PPy antennas and randomly grow on the surface of SPs. The resulting SP/PPy composites exhibited high catalytic activity and excellent stability in the catalysis applications, for instance, the reduction of MB dye with NaBH_4. Fe_3O_4/SiO_2/PPy nanocomposites were also successfully synthesized. Magnetic nanospheres with diameter of 200 nm were synthesized via a solvothermal reaction. Then, magnetic nanospheres were coated with SiO2 shell which originated from the hydrolysis and condensation of TEOS. The thickness of SiO2 shell could be tuned by the dosage of TEOS. Subsequently, PVP was grafted on the surface of Fe_3O_4/SiO_2, which provided active sites for pyrrole monomer loading on. Finally, PPy shell formed on the surface of Fe_3O_4/SiO_2 through oxidative polymerization. The thickness of PPy shell was controllable by adjusting the dosage of pyrrole monomer. Because of the stability and biocompatibility of PPy, the Fe_3O_4/SiO_2/PPy nanocomposites showed potential applications in biomedicine.
Nanoparticles (NPs) have attracted much attention due to their unique optical properties, magnetic properties and catalytic properties. In recent years, various methods have been used in synthesis NPs with different sizes and morphologies. These as-prepared NPs were using as building blocks to fabricate various self-assembly structures whose morphologes looked like chain, band and sphere, through van der Waals interaction, electrostatic interaction, hydrogen bond, and so forth. These omnifarious nanostructures displayed bright prospect for applications in nano-design and nano-device.
However, fragileness and aggregation were usually present in NPs and their self-assembly structures. In order to solve these problems, various functional polymers were introduced into the system. On one hand, polymers could improve the stability of NPs and their self-assembly structures. On the other hand, the existence of NPs could enhance the mechanical properties of polymers.
In chapter 2, sodium citrate stabilized gold (Au) NPs were prepared. Then, TGA-capped Au NPs were prepared by ligand exchange. The self-assembly behaviors of Au NPs on substrate were carefully investigated by changing the experimental conditions such as volume ratios of water/acetone, species of ligands and temperature. With decreasing the volume ratios of water/acetone, the dendritic grade of self-assembly structures increased. When the volume ratios of water/acetone were the same, the self-assembly structures of TGA-capped Au NPs had less branches than that of sodium citrate-stabilized Au NPs. Low temperature usually increased the dendritic grade of self-assembly structure. We have investigated these self-assembly behaviors from three different aspects including interparticle interaction, the mobile rate of NPs, and the evaporation rate of the solvent. The theory explanation was quite accordance with the experimental phenomenon. Therefore, our studies were useful for understanding the complex mechanism of the self-assembly of charged NPs, and indicated a protocol to NP-based nano- or micro-structures with controlled mophologies.
In chapter 3, we have successfully synthesized flower-like Au NPs using seeding approach. The results indicated dosage of hydroquinone played a key role in the formation of flower-like NPs. When the amount of hydroquinone was 100μL, no flower-like Au NPs appeared in the system. When the amount of hydroquinone and seed were 300μL and 50μL, respectively, flower-like Au NPs appeared in the system. However, further increasing the amount of hydroquinone, the size and morphology of NPs did not change. In the experiment, when the amount of hydroquinone was 1000μL, the size and morphology of flower-like NPs could be tuned through the dosage of seeds. NPs with different sizes and morphologies were also assembled on the liquid-liquid interface through reducing the surface charge of NPs. This self-assembly structure has potential application in surface enhanced Raman scattering.
In chapter 4, first, we have successfully synthesized Au superparticle/polypyrrole (SP/PPy) composites. In the preparation process, poly (N-vinylpyrrolidone) (PVP) played a key role; without it, PPy could not cover on the surface of SPs and form a complete shell. The influence of pyrrole monomer concentration on the morphology and shell thickness of resulting composites was also investigated in this chapter. The experimental results indicated the optimized concentrations of pyrrole monomer ranged between 1.14 and 2.28 mM. If the concentration was too high, pure PPy NPs would appear in the system. If the concentration was too low, pyrrole monomer would polymerize into PPy antennas and randomly grow on the surface of SPs. The resulting SP/PPy composites exhibited high catalytic activity and excellent stability in the catalysis applications, for instance, the reduction of MB dye with NaBH_4. Fe_3O_4/SiO_2/PPy nanocomposites were also successfully synthesized. Magnetic nanospheres with diameter of 200 nm were synthesized via a solvothermal reaction. Then, magnetic nanospheres were coated with SiO2 shell which originated from the hydrolysis and condensation of TEOS. The thickness of SiO2 shell could be tuned by the dosage of TEOS. Subsequently, PVP was grafted on the surface of Fe_3O_4/SiO_2, which provided active sites for pyrrole monomer loading on. Finally, PPy shell formed on the surface of Fe_3O_4/SiO_2 through oxidative polymerization. The thickness of PPy shell was controllable by adjusting the dosage of pyrrole monomer. Because of the stability and biocompatibility of PPy, the Fe_3O_4/SiO_2/PPy nanocomposites showed potential applications in biomedicine.
引文
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