反蛋白石型氧化锆光子晶体结构色的制备及呈色因素分析

发布时间：2018-10-29 22:36

【摘要】：结构色因具有亮度和饱和度高、永不退色、虹彩效应、附着力好、耐刮擦和环境友好性而日益受到国内外研究者的广泛关注。高饱和度超结构色剂具有广泛的应用前景,将会渗透并能取代现有的色剂在显示技术、防伪、探测、航空航天以及新型高技术产品的应用等领域,它具有很高的学术研究价值和应用潜力。光子晶体中的介电常数比达到某一特定的阈值对于完全光子禁带的产生具有很大的益处。完全光子禁带的产生有利于可见光的调控、自然光下结构色饱和度以及亮度的提高。在蛋白石型光子晶体材料中这个阈值约为4,但是研究表明在人工构筑的反蛋白石型光子晶体材料中这个阈值远远低于4。由于面心立方结构晶格点的球形对称所引起的简并,也使得蛋白石型光子晶体难以出现完全光子禁带,这就限制了它在结构色剂方面的应用,使反蛋白石型光子晶体有应用于结构色剂的潜力。本论文以制备反蛋白石型氧化锆光子晶体、分析其呈色现象为目标。先制备出聚苯乙烯(Polystyrene, PS)胶体微球,PS微球再通过胶体自组装排列而形成胶体晶体,以此胶体晶体为模板剂,通过向模板剂的空隙中添加高介电常数的氧化锆前驱体溶胶原位固化干燥以后,经过煅烧而除去模板剂形成氧化锆-空气的具有高介电比的反蛋白石型光子晶体。采用了红外光谱、XRD、SEM、紫外-可见光谱等分析仪器为表征手段,并且以数码相机捕捉其呈色效果。主要研究工作是合成PS亚微米级微球及微球表面形态和微球粒径大小的分析、PS胶体晶体模板剂制备工艺探讨以及反蛋白石型氧化锆光子晶体材料制备工艺分析。具体包括以下几个方面：以无皂乳液聚合法合成了PS亚微米级微球,分析了其粒径的分布情况以及红外光谱中官能团信息,探讨了碳酸氢钾用量、苯乙烯磺酸钠用量、引发剂用量以及反应时间对PS微球粒径大小以及微球表面形态的影响,最后分析了PS的成球机理。利用蒸发自组装技术,以自制的PS微球为原料制备了PS胶晶模板剂,研究分析了微球浓度、组装温度、乳液高度、组装面积对PS胶晶模板剂微观排列形貌以及呈色效果的影响,以正交试验确定了以上因素的主次因素和水平。采用胶晶模板法,以PS胶体晶体为模板剂,制备了反蛋白石型氧化锆光子晶体,研究了前驱体浓度、模板剂与前驱体质量比、浸渍次数、煅烧温度和保温时间对产物氧化锆的物相以及微观形貌的影响,以正交试验确定了上述因素的主次因素和水平。研究了不同的煅烧气氛对反蛋白石型氧化锆光子晶体的微观形貌和宏观呈色的影响,推测分析了还原气氛中煅烧的样品在自然光的照射下产生的结构色的饱和度更好的原因,证明了以PS胶晶模板法制备的反蛋白石型氧化锆光子晶体作为一种新型的结构色剂具有较大的研究潜力。
[Abstract]:Due to its high brightness and saturation, never fading, iridescent effect, good adhesion, scratch resistance and environmental friendliness, structural color has attracted more and more attention from researchers at home and abroad. High saturation superstructure coloring agents have a wide application prospect, which will permeate and replace the existing color agents in the fields of display technology, anti-counterfeiting, detection, aerospace and the application of new high-tech products, etc. It has high academic research value and application potential. The ratio of dielectric constant in photonic crystals to a certain threshold is of great benefit for the generation of complete photonic bandgap. The generation of complete photonic band gap is beneficial to the regulation of visible light and the enhancement of structure color saturation and brightness under natural light. This threshold is about 4 in opal photonic crystal materials, but it is far below 4 in artificial opal photonic crystal materials. Due to the degeneracy caused by spherical symmetry of lattice points in face-centered cubic structures, it is difficult for opal photonic crystals to have complete photonic bandgap, which limits their application in structural coloring agents. The inverse opal photonic crystals have the potential to be used as structural coloring agents. The aim of this thesis is to prepare inverse opal type zirconia photonic crystal and analyze its color phenomenon. Polystyrene (Polystyrene, PS) colloidal microspheres were prepared first, then PS microspheres were arranged by colloid self-assembly to form colloidal crystals, and the colloidal crystals were used as templates. After in-situ curing and drying of zirconia precursor with high dielectric constant, the template was calcined to form a zirconia-air opal photonic crystal with high dielectric ratio. The infrared spectrum, XRD,SEM, UV-Vis spectrum and other analytical instruments were used as the characterization means, and the color effect was captured by digital camera. The main work of this paper is to analyze the surface morphology and particle size of PS submicron microspheres, the preparation process of PS colloidal crystal template and the preparation process of inverse opal zirconia photonic crystal materials. The details include the following aspects: PS submicron microspheres were synthesized by soap-free emulsion polymerization. The distribution of particle size and the functional group information in infrared spectrum were analyzed. The amount of potassium bicarbonate and sodium styrenesulfonate were discussed. The effects of the amount of initiator and reaction time on the particle size and surface morphology of PS microspheres were investigated. Finally, the mechanism of PS pelletizing was analyzed. The effects of concentration, temperature, emulsion height and assembly area of PS microspheres on the morphology and color effect of PS colloidal template were studied and analyzed by using the evaporative self-assembly technique. The primary and secondary factors and the level of the above factors were determined by orthogonal test. The inverse opal type zirconia photonic crystal was prepared by colloidal template method with PS colloidal crystal as template. The concentration of precursor, the mass ratio of template to precursor, and the times of impregnation were studied. The effects of calcination temperature and holding time on the phase and micromorphology of zirconia were studied. The main and secondary factors and the level of the above factors were determined by orthogonal test. The effects of different calcination atmosphere on the microscopic morphology and macroscopic color of inverse opal type zirconia photonic crystal were studied. The reason why the structure color saturation of calcined samples in the reduction atmosphere was better under the irradiation of natural light was inferred and analyzed. It is proved that the inverse opal type zirconia photonic crystal prepared by PS gel crystal template method has great potential as a new structural color agent.
【学位授予单位】：陕西科技大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O734

【相似文献】