製備均一粒徑有機無機核殼微小球; The preparation of monodisperse organic-inorganic core-shell spheres

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題名:	製備均一粒徑有機無機核殼微小球;The preparation of monodisperse organic-inorganic core-shell spheres
作者:	朱薇如;WeiJu Chu
貢獻者:	化學工程與材料工程研究所
關鍵詞:	二氧化矽中空球;光子晶體;擴散;Stober;均一粒徑;hollow sphere;monodisperse;diffusion;photonic crystal
日期:	2011-06-20
上傳時間:	2012-01-05 11:16:05 (UTC+8)
摘要:	本研究探討具有均一粒徑之有機-無機核殼結構粒子。根據粒子大小，主要可分為均一粒徑之微米級與次微米球。關於製備微米級有機-無機均一粒徑粒子，主要以硬模版法，先以分散聚合法將苯乙烯單體(Styrene)合成實心內核粒子，透過聚乙烯吡咯烷酮(穩定劑)穩定粒子防止凝聚，將四乙氧基矽烷包覆在實心內核上。微米級不同粒徑大小的聚苯乙烯(PS)球可由調整乙醇在乙醇水溶液中的重量百分比而製備出。將PS球均勻分散在乙醇中，透過Stőber方法將四乙氧基矽烷(TEOS)包覆在PS球上，形成均一粒徑的PS-TEOS核殼結構粒子。隨著TEOS加入量的增加，外殼厚度也隨之增加。最後以高溫鍛燒，可製備出不同粒徑與殼厚的二氧化矽中空球，粒徑約在1~2 μm間。製備次微米級有機-無機均一粒徑粒子方法與前者相同，亦使用硬模版法進行製備。首先使用無乳化劑乳化聚合法，在高溫下製備均一粒徑聚苯乙烯次微米球作為內核。製備PS球過程中，在單體轉化率約96%時，加入不同種類矽烷，快速合成均一粒徑有機-無機核殼次微米球。所使用的矽烷種類包含四乙氧基矽烷, 甲基三乙氧基矽烷(MTES) ,二甲基二乙基矽烷(DMDES), 3-甲基丙烯酸基丙基三甲氧基矽烷(MPS)。所得之均一粒徑核殼次微米球，其球徑皆在180~200 nm。經水洗測試發現，特定矽烷MTES與PS球內核的結合性良好；透過TEM儀器觀測，發現PS球轉化率低時，核殼球粒徑擴大，認為是矽烷擴散進PS球內核所致。此外，改變加入矽烷單體的時間，亦可製備出均一粒徑的核殼結構粒子。對於在PS球特定轉化率下，提高添加的矽烷單體量，可增大均一粒徑次微米球之粒徑。此類核殼結構粒子透過毛細力驅動，可製備成光子晶體作為應用。 The study was focused on the preparation of monodisperse organic-inorganic core-shell structures microspheres. According to the particles size, the preparations were divided into two parts: monodisperse microscale and submicroscale spheres. For the preparation of microscale monodisperse organic-inorganic particles, the core particles-styrene spheres were first produced by dispersion polymerization. With the help of polyvinylpyrrolidone, the phenomenon of particles aggregation were avoided, so the polystyrene(PS) spheres can be wrapped in tetraethoxysilane in the second step. Controlling the ethanol weight percent in ethanol solution affected the size of PS spheres. In the second step, the PS spheres were dispersed in ethanol with adding tetraethoxysilane step by step. After 24hrs, monodisperse PS-SiO2 structure was formed. The diameters of the core-shell particles raised up as the amount of tetraethoxysilane increased. The hollow spheres were obtained after taking the organic-inorganic particles to calcine under high temperature. The diameter range of hollow spheres diameter was 1~2μm. The method to synthesize submicroscale monodisperse organic-inorganic particles was similar to the way of producing microscale particles. Both the core parts were first prepared, and then silane was added to modify the organic core surface. For submicroscale organic-inorganic particles, different kinds of silane, including tetraethylsilane(TEOS), methyltriethoxysilane(MTES), dimethyldi- ethoxysilane(DMDES), 3-(Trimethoxysilyl)propyl methacrylate(MPS) were added during the polymerization of styrene by soap-free polymerization. The size of the organic-inorganic particles was about 180 nm to 210 nm. The core-shell structure was clearly observed under TEM. With the results of TGA and the TEM photograph indicating that silane were diffused into PS spheres. As the amount of silane increased, the diameter of core-shell particles increased, too. These organic-inorganic particles self-assembled photonic crystal after heating due to capillary force.
顯示於類別:	[化學工程與材料工程研究所] 博碩士論文

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