【摘要】：結(jié)構(gòu)色因具有亮度和飽和度高、永不退色、虹彩效應(yīng)、附著力好、耐刮擦和環(huán)境友好性而日益受到國(guó)內(nèi)外研究者的廣泛關(guān)注。高飽和度超結(jié)構(gòu)色劑具有廣泛的應(yīng)用前景,將會(huì)滲透并能取代現(xiàn)有的色劑在顯示技術(shù)、防偽、探測(cè)、航空航天以及新型高技術(shù)產(chǎn)品的應(yīng)用等領(lǐng)域,它具有很高的學(xué)術(shù)研究?jī)r(jià)值和應(yīng)用潛力。光子晶體中的介電常數(shù)比達(dá)到某一特定的閾值對(duì)于完全光子禁帶的產(chǎn)生具有很大的益處。完全光子禁帶的產(chǎn)生有利于可見(jiàn)光的調(diào)控、自然光下結(jié)構(gòu)色飽和度以及亮度的提高。在蛋白石型光子晶體材料中這個(gè)閾值約為4,但是研究表明在人工構(gòu)筑的反蛋白石型光子晶體材料中這個(gè)閾值遠(yuǎn)遠(yuǎn)低于4。由于面心立方結(jié)構(gòu)晶格點(diǎn)的球形對(duì)稱所引起的簡(jiǎn)并,也使得蛋白石型光子晶體難以出現(xiàn)完全光子禁帶,這就限制了它在結(jié)構(gòu)色劑方面的應(yīng)用,使反蛋白石型光子晶體有應(yīng)用于結(jié)構(gòu)色劑的潛力。本論文以制備反蛋白石型氧化鋯光子晶體、分析其呈色現(xiàn)象為目標(biāo)。先制備出聚苯乙烯(Polystyrene, PS)膠體微球,PS微球再通過(guò)膠體自組裝排列而形成膠體晶體,以此膠體晶體為模板劑,通過(guò)向模板劑的空隙中添加高介電常數(shù)的氧化鋯前驅(qū)體溶膠原位固化干燥以后,經(jīng)過(guò)煅燒而除去模板劑形成氧化鋯-空氣的具有高介電比的反蛋白石型光子晶體。采用了紅外光譜、XRD、SEM、紫外-可見(jiàn)光譜等分析儀器為表征手段,并且以數(shù)碼相機(jī)捕捉其呈色效果。主要研究工作是合成PS亞微米級(jí)微球及微球表面形態(tài)和微球粒徑大小的分析、PS膠體晶體模板劑制備工藝探討以及反蛋白石型氧化鋯光子晶體材料制備工藝分析。具體包括以下幾個(gè)方面：以無(wú)皂乳液聚合法合成了PS亞微米級(jí)微球,分析了其粒徑的分布情況以及紅外光譜中官能團(tuán)信息,探討了碳酸氫鉀用量、苯乙烯磺酸鈉用量、引發(fā)劑用量以及反應(yīng)時(shí)間對(duì)PS微球粒徑大小以及微球表面形態(tài)的影響,最后分析了PS的成球機(jī)理。利用蒸發(fā)自組裝技術(shù),以自制的PS微球?yàn)樵现苽淞薖S膠晶模板劑,研究分析了微球濃度、組裝溫度、乳液高度、組裝面積對(duì)PS膠晶模板劑微觀排列形貌以及呈色效果的影響,以正交試驗(yàn)確定了以上因素的主次因素和水平。采用膠晶模板法,以PS膠體晶體為模板劑,制備了反蛋白石型氧化鋯光子晶體,研究了前驅(qū)體濃度、模板劑與前驅(qū)體質(zhì)量比、浸漬次數(shù)、煅燒溫度和保溫時(shí)間對(duì)產(chǎn)物氧化鋯的物相以及微觀形貌的影響,以正交試驗(yàn)確定了上述因素的主次因素和水平。研究了不同的煅燒氣氛對(duì)反蛋白石型氧化鋯光子晶體的微觀形貌和宏觀呈色的影響,推測(cè)分析了還原氣氛中煅燒的樣品在自然光的照射下產(chǎn)生的結(jié)構(gòu)色的飽和度更好的原因,證明了以PS膠晶模板法制備的反蛋白石型氧化鋯光子晶體作為一種新型的結(jié)構(gòu)色劑具有較大的研究潛力。
[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.
【學(xué)位授予單位】：陜西科技大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類號(hào)】：O734

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