臺灣博碩士論文加值系統

本論文研究重點由三大方向組合而成：(1) 利用溶膠凝膠(Sol-Gel)法合成具高真圓度與單一分散特性之次微米級氧化鋅(Zinc Oxide; ZnO)微球粉體；(2) 利用化學浴沉積 (Chemical Bath Deposition; CBD) 法合成單一尺寸與單一分散性之次微米級ZnO微球；(3) 利用電泳自組裝(Electrophoretic Self-assembly; EPSA)方法，將乳化聚合(Emulsion Polymerization)法所合成之聚苯乙烯(Polystyrene; PS)微球(250 nm)，進行強制性電泳披覆之自組裝行為，以形成三維(3-D)的PS光子晶體模板，再將所製備之PS光子晶體模板進行顯微結構與光學性質之分析探討，以證實吾人所製備之光子晶體具有規則有序排列之最密堆積結構，且具有光子能隙現象，並藉由理論模擬PS微球所架構之面心立方(Face-centered Cubic; FCC)最密堆積結構的能帶結構圖，證實所量測之光子能隙為真實的能隙。
研究結果得知，吾人經由溶膠凝膠法搭配兩階段合成方式可成功製作出次微米級(90 nm ~ 500 nm)的ZnO微球，並具有高真圓度與單一分散性質；藉由化學浴沉積法亦成功合成奈米級至次微米級(50 nm ~ 300 nm)，並具單一尺寸與單一分散性質。於EPSA技術中特別著重膠體溶液之懸浮分散性的調控，當pH值呈鹼性條件下，PS微球粉體之分散效果良好，透過添加適量的十二烷基硫酸鈉(Sodium dodecyl sulfate; SDS)界面活性劑有助於獲致穩定之EPSA懸浮液。
最後利用此一新穎且低成本之電泳自組裝技術，使各種粒徑的單一分散性佳之聚苯乙烯微球均能披覆於銦錫氧化物(Indium Tin Oxide; ITO)玻璃基板上，並排列成三維(3-D)有序的蛋白石(Opal)結構，以獲得所欲求的PS微球光子晶體模板。由於PS微球所組裝的光子晶體模板之單分散的微球有高形變和材料去除(Material Removal)便利性的特點，可順利地避免於乾燥過程發生斷裂或孔洞產生等問題，故其應用範圍頗為廣泛。且此週期有序結構將可應用於製作新穎的光子晶體模板，以利吾人後續藉由模板誘導電泳技術將高介電常數材料如ZnO、TiO2等填充於模板中，再以高溫煆燒或HF腐蝕將原來的光子晶體材料移除之，以留下具高介電常數對比之反蛋白石結構(Inverse Opal Structure)期能增進光子能隙效應，以開發前瞻性發光二極體與太陽能電池等光伏特元件。

The major objectives of this study are aimed at achieving (a) high synthetic efficiency fabrication of monodispersive submicron-sized zinc oxide (ZnO) spheres with high sphericity by sol-gel process, (b) synthesis of monodispersed ZnO microspheres with narrow size distribution by chemical bath deposition (CBD) method, (c) electrophoretic self-assembly (EPSA) formation and microstructural characterization of 3-D photonic crystal (PhC) templates of polystyrene (PS) microspheres at average size of 250 nm by emulsion polymerization. Our goal is to investigate the photonic properties of such closely packed, ordered 3-D templates of PS spheres, which can manifest photonic bandgap (PBG) in accordance with our modeling results out of planar-wave expansion (PWE) simulation work for face-centered cubic (FCC) structures to verify the existence of real PBG in our tunable nanostructures PhC samples.
The results showed that two-step sol-gel process can produce monodispersed ZnO microspheres of 90~500 nm and CBD process is able to formulate ZnO microspheres of even smaller particle size (50~300 nm) in a narrow particle size distribution. It is essential to control the acidity of EPSA colloid with reasonably good stability. At basic conditions, the PS colloid can be obtained with good dispersivity by adding suitable amount of surfactant such as sodium dodecyl sulfate (SDS).
These uniformly sized ZnO and microspheres can be successfully formed as 3-D ordered templates of opal structure on transparent, conductive substrates such as indium-tin oxide (ITO) glasses through our novel EPSA route. To acquire pronounced PBG effect for photonic applications in developing LEDs or solar cells of high conversion efficiency, most of polystyrene microsphere templates are currently used due to its material flexibility to avoid defect or void introduction during the drying stage and to easily transform into inverse opal structure by infiltrating other oxides with high dielectric constant (e.g. ZnO or TiO2) through potential thermal or chemical material removal schemes such as pyrolysis or solvent dissolution or etching.

中文摘要 I
英文摘要 III
目錄 IV
圖目錄 VIII
表目錄 XIII
第一章 緒 論 1
1.1 光子晶體起源問世與光子能隙介紹 1
1.2 光子晶體及模板製程技術簡述 6
1.2.1 光子晶體製程技術 6
1.2.2 光子晶體模板製程技術 10
1.3 光子晶體之應用 14
1.4 電泳自組裝技術發展介紹 22
1.5 電泳懸浮液系統種類 25
1.6 研究目的及重點 31
第二章 理論基礎與文獻回顧 33
2.1 氧化鋅晶體結構與特性 33
2.1.1氧化鋅晶體結構 33
2.1.2 氧化鋅晶體光電特性 36
2.2 溶膠凝膠法基本原理 38
2.3 電泳自組裝機制 46
2.4 表面、界面與膠體之原理與應用 48
2.4.1膠體表面電位與工作電極對電雙層之影響 48
2.4.2膠體化學與DLVO理論簡述 54
2.5 定電壓與定電流之電泳披覆行為 61
2.6 蛋白石與反蛋白石光子晶體的結構與特性 63
第三章 實驗步驟與方法 71
3.1 溶膠凝膠法製備次微米級至奈米級ZnO微球 71
3.2 溶膠凝膠法合成ZnO微球相關反應參數 74
3.2.1調控母液與第二階段溶液之醋酸鋅濃度比 74
3.2.2改變母液添加溫度 75
3.2.3 ZnO微球經熱處理後之結構變化 76
3.3 化學浴合成法製備次微米ZnO微球 76
3.4化學浴合成法製備次微米ZnO微球相關反應參數 78
3.4.1控制縮合反應時間之影響 78
3.4.2控制緩衝溶液的含量 79
3.4.3添加不同錯合劑對ZnO微球顯微結構之變化 79
3.5 以EPSA技術自組裝PS微球膠體晶體。 79
3.6 分析儀器 84
3.6.1 冷場發射掃描式電子顯微鏡 84
3.6.2 多功能薄膜X光繞射儀 85
3.6.3 高解析穿透式電子顯微鏡 85
3.6.4 雷射粒徑分析儀 86
3.6.5 Zeta介面電位分析儀 87
3.6.6 紫外光及可見光譜分析儀 87
第四章 結果與討論 91
4.1 溶膠凝膠法製備次微米級ZnO微球 91
4.1.1調控母液與第二階段溶液之醋酸鋅濃度比 91
4.1.2改變母液添加溫度對微球結構之變化 93
4.1.3 ZnO微球顯微結構與晶相分析 97
4.1.4 經熱處理後之ZnO微球顯微結構分析 98
4.2化學浴合成法製備次微米ZnO微球 100
4.2.1不同縮合反應時間對ZnO微球分散性之影響 100
4.2.2不同緩衝溶液含量對ZnO顯微結構之影響 103
4.2.3控制錯合劑含量對ZnO微球顯微結構之變化 103
4.3以EPSA技術自組裝微球光子晶體 104
4.3.1 EPSA膠體溶液之配置與Zeta Potential分析 104
4.3.2 EPSA製程參數的控制與自組裝結構分析 107
4.4 光子晶體之光學性質分析 114
4.5光子晶體之理論模擬能帶結構 119
第五章 結論 131
第六章 未來研究方向 134
參考文獻 137
誌 謝 153
作者簡歷 155

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