聚苯乙烯基凝胶光子晶体的制备
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摘要
光子晶体(photonic Crystal)是一种介电常数可以周期性调制的结构,是在二十世纪八十年代末发展起来的一种全新的功能材料。介电常数不同的介质材料在空间中作周期性排列,可以改变在其间传播的光的性质。近年来,利用胶体晶体自组装性质与水凝胶的传统应用相结合制成的凝胶光子晶体在药物释放、光学开关、金属探针、生物传感器等新应用方面的研究蓬勃发展,在新材料开发及临床应用等方面取得巨大进展。
本论文主要通过选择制备方法和控制工艺条件,制备了两种光子晶体的组成单元-单分散聚苯乙烯微球和聚苯乙烯/2-丙烯酰胺基-2-甲基丙磺酸复合微球。主要研究内容包括以下两个部分:
第一部分,系统完整地考察和总结了聚苯乙烯的合成方法、合成路线、合成配方和反应条件,确立了适用于本实验室的单分散聚苯乙烯微球的制备方法,得到了高圆度、窄粒径分布的单分散聚苯乙烯微球,能够满足形成可见光波段胶体晶体的要求。然后,对于制备的单分聚苯乙烯微球,采用垂直沉积法自组装成面心立方晶体周期性结构。利用光纤光谱仪研究了面心立方胶体晶体的不完全光子带隙效应,利用场发射扫描电镜观察了胶体晶体的结构特点和缺陷情况。通过反射光谱图和扫描电镜照片判断、确定和优化了乳液聚合法主要制备工艺参数。最后,采用毛细力渗透法对聚苯乙烯微球组装的模板表面填充了含有2-丙烯酰胺基-2-甲基丙磺酸功能单体的前驱液,待前体溶液交联聚合后,用溶剂溶解法除去模板后制得带有磺酸基功能基团的反蛋白石结构凝胶光子晶体。该反蛋白石结构凝胶光子晶体表现出鲜艳的结构颜色,保持了长程有序的周期性结构,并对Ca~(2+)具有较强的吸附性,且Ca~(2+)的吸附量随着2-丙烯酰胺基-2-甲基丙磺酸功能单体含量的增大而增大。
第二部分,利用2-丙烯酰胺基-2-甲基丙磺酸对聚苯乙烯胶体晶体进行改性。采用湿化学方法,建立了在聚苯乙烯微球表面包覆功能单体的方法,优化了单分散聚苯乙烯/2-丙烯酰胺基-2-甲基丙磺酸微球的制备方法。扫描电镜表征结果表明,单分散聚苯乙烯/2-丙烯酰胺基-2-甲基丙磺酸微球的粒径分布较均匀,能够实现初步胶体晶体自组装。
Photonic crystal (PC) is a spatial periodic dielectric structure, which is a new kind of functional materials arised from the late 1980s. With different dielectric coefficient materials periodically arrayed in the space, photonic crystals (PCs) prevent the transmitting of some electromagnetic spectrum. In recent years, colloidal crystal self-assembly properties were coupled with traditional application of gel which was used in the drug release, optical switch, the metal probe, biosensor and other new applied research. In the development of new materials and its clinical application gained tremendous progress.
In this paper, monodisperse spheres of polystyrene(PS), Poly styrene/2-acrylamido--2 - methylpropane sulfonic acid( PSt/AMPS) which are the PCs units have been fabricated by controlling the synthesis condition. The main research include the following two parts: In the first part, monodisperse PS were fabricated systemically by different synthesis condition. In the experiments, PS spheres which were verified to suit for the requirements of fabricating opal PCs and satisfy the formation of colloidal crystal visible bands. Then, opal PCs with fcc structure were assembled with the monodisperse PS microspheres by vertical deposition method. According to the periodic structures, opal PCs were fabricated.
Then the stop band gap of the fcc structure is confirmed by Fiber Optic Spectrometer. The characteristics and defects of colloidal crystal were analyzed with Field Emission Scanning Electron Microscope(FESEM). Judging by Fiber Optic Spectrometer and FESEM images, the mainly factors for the synthesis of PS particles were optimized. Lastly, the precursors, the AMPS was infiltrated into the templates by induced capillary attraction method. By immersing the polymers in the solvent to remove the template, the well ordered three dimensional inverse opal photonic crystals are fabricated and show the vivid structural color. Finally, used the inverse opal photonic crystals containing AMPS to adsorp Ca~(2+), and the adsorption amounts of Ca~(2+) is increased with the AMPS content.
In the second part, a feasible way was found out for PSt/AMPS sphere’s synthesis. The FESEM observation showed a fare good inverse opal structure using wet chemistry method. And periodic structures were self-organized with these units by vertical deposition method. The IR confirmed the PSt/AMPS spheres were fabricated. Monodisperse PSt/AMPS nanoparticles were successful synthesized with a narrow size distributed relatively.
本论文主要通过选择制备方法和控制工艺条件,制备了两种光子晶体的组成单元-单分散聚苯乙烯微球和聚苯乙烯/2-丙烯酰胺基-2-甲基丙磺酸复合微球。主要研究内容包括以下两个部分:
第一部分,系统完整地考察和总结了聚苯乙烯的合成方法、合成路线、合成配方和反应条件,确立了适用于本实验室的单分散聚苯乙烯微球的制备方法,得到了高圆度、窄粒径分布的单分散聚苯乙烯微球,能够满足形成可见光波段胶体晶体的要求。然后,对于制备的单分聚苯乙烯微球,采用垂直沉积法自组装成面心立方晶体周期性结构。利用光纤光谱仪研究了面心立方胶体晶体的不完全光子带隙效应,利用场发射扫描电镜观察了胶体晶体的结构特点和缺陷情况。通过反射光谱图和扫描电镜照片判断、确定和优化了乳液聚合法主要制备工艺参数。最后,采用毛细力渗透法对聚苯乙烯微球组装的模板表面填充了含有2-丙烯酰胺基-2-甲基丙磺酸功能单体的前驱液,待前体溶液交联聚合后,用溶剂溶解法除去模板后制得带有磺酸基功能基团的反蛋白石结构凝胶光子晶体。该反蛋白石结构凝胶光子晶体表现出鲜艳的结构颜色,保持了长程有序的周期性结构,并对Ca~(2+)具有较强的吸附性,且Ca~(2+)的吸附量随着2-丙烯酰胺基-2-甲基丙磺酸功能单体含量的增大而增大。
第二部分,利用2-丙烯酰胺基-2-甲基丙磺酸对聚苯乙烯胶体晶体进行改性。采用湿化学方法,建立了在聚苯乙烯微球表面包覆功能单体的方法,优化了单分散聚苯乙烯/2-丙烯酰胺基-2-甲基丙磺酸微球的制备方法。扫描电镜表征结果表明,单分散聚苯乙烯/2-丙烯酰胺基-2-甲基丙磺酸微球的粒径分布较均匀,能够实现初步胶体晶体自组装。
Photonic crystal (PC) is a spatial periodic dielectric structure, which is a new kind of functional materials arised from the late 1980s. With different dielectric coefficient materials periodically arrayed in the space, photonic crystals (PCs) prevent the transmitting of some electromagnetic spectrum. In recent years, colloidal crystal self-assembly properties were coupled with traditional application of gel which was used in the drug release, optical switch, the metal probe, biosensor and other new applied research. In the development of new materials and its clinical application gained tremendous progress.
In this paper, monodisperse spheres of polystyrene(PS), Poly styrene/2-acrylamido--2 - methylpropane sulfonic acid( PSt/AMPS) which are the PCs units have been fabricated by controlling the synthesis condition. The main research include the following two parts: In the first part, monodisperse PS were fabricated systemically by different synthesis condition. In the experiments, PS spheres which were verified to suit for the requirements of fabricating opal PCs and satisfy the formation of colloidal crystal visible bands. Then, opal PCs with fcc structure were assembled with the monodisperse PS microspheres by vertical deposition method. According to the periodic structures, opal PCs were fabricated.
Then the stop band gap of the fcc structure is confirmed by Fiber Optic Spectrometer. The characteristics and defects of colloidal crystal were analyzed with Field Emission Scanning Electron Microscope(FESEM). Judging by Fiber Optic Spectrometer and FESEM images, the mainly factors for the synthesis of PS particles were optimized. Lastly, the precursors, the AMPS was infiltrated into the templates by induced capillary attraction method. By immersing the polymers in the solvent to remove the template, the well ordered three dimensional inverse opal photonic crystals are fabricated and show the vivid structural color. Finally, used the inverse opal photonic crystals containing AMPS to adsorp Ca~(2+), and the adsorption amounts of Ca~(2+) is increased with the AMPS content.
In the second part, a feasible way was found out for PSt/AMPS sphere’s synthesis. The FESEM observation showed a fare good inverse opal structure using wet chemistry method. And periodic structures were self-organized with these units by vertical deposition method. The IR confirmed the PSt/AMPS spheres were fabricated. Monodisperse PSt/AMPS nanoparticles were successful synthesized with a narrow size distributed relatively.
引文
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