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研究生: 許家豪
Chia-Hao Hsu
論文名稱: 利用迷你乳液製備四乙氧基矽烷/苯乙烯複合型奈米二氧化矽粒子之合成與特性研究
Synthesis and Characterization of Nano-Composite Silica Particles with Tetraethyl Orthosilicate/Styrene by miniemulsion
指導教授: 陳崇賢
Chorng-Shyan Chern
口試委員: 蔡大翔
Dah-Shyang Tsai
許榮木
Jung-Mu Hsu
學位類別: 碩士
Master
系所名稱: 工程學院 - 化學工程系
Department of Chemical Engineering
論文出版年: 2018
畢業學年度: 106
語文別: 中文
論文頁數: 115
中文關鍵詞: 迷你乳液四以氧基矽烷苯乙烯矽烷偶合劑複合型奈米二氧化矽粒子
外文關鍵詞: miniemulsion, Tetraethyl Orthosilicate, Styrene, silane coupling agent, nano-composite silica particles
相關次數: 點閱:435下載:0
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 本論文使用四乙氧基矽烷(TEOS)作為無機單體、苯乙烯(Styrene)作為有機單體,在迷你乳液系統中加入緩衝鹽類-碳酸氫鈉(NaHCO3)、共同安定劑-正十六烷(HD)、陰離子界面活性劑(SDS)、起始劑-偶氮二異丁腈(AIBN),以及矽烷偶合劑-3-(三甲氧基甲硅烷基)丙基丙烯酸酯(3-(Trimethoxysilyl)propyl methacrylate)。添加酸性觸媒(HCl)調整其pH值,促使TEOS做水解、縮合反應,在80 °C的環境下,合成有機-無機的複合型奈米二氧化矽。經過純化、離心等步驟後放入高溫爐中,在空氣下經過鍛燒程序(Calcination)於600 °C環境下燒結8個小時,將有機相全部去除留下無機相。改變其TEOS/Styrene比例及改變偶合劑含量,探討其粒子的各種性質。
並利用動態光散射粒徑分析儀(DLS)、高解析度場發射掃描式電子顯微鏡(SEM)、穿透式電子顯微鏡(TEM)、表面積及孔徑分析儀(BET)分析其粒徑約115至150 nm,比表面積約700 m2/g。以及使用熱重/熱示差分析儀(TGA),觀察其粒子熱穩定性,微分式掃描熱量分析儀(DSC),探討其合成時的吸放熱反應。


In this study, we used miniemulsion as the templates, tetraethyl orthosilicate (TEOS) as monomers in inorganic phase, styrene as monomers in organic phase, sodium bicarbonate (NaHCO3) as buffer salt, n-hexadecane (HD) as a costabilizer, sodium dodecyl sulfate (SDS) as a surfactant, azobisisobutyronitrile (AIBN) as a initiator and 3-(Trimethoxysilyl)propyl methacrylate as a coupling agent. An acidic catalyst (HCl) was added to adjust the pH so that TEOS underwent hydrolysis and condensation reactions to synthesize organic-inorganic composite nano-composite silica particles at 80 ℃. The particles were then purified, centrifuged, dried and placed in the furnace for calcination to remove all of the organic substances and only keep the inorganic substances. The properties of the particles were investigated as a function of the ratio of TEOS to Styrene and the amount of the coupling agent. The size and morphology of the particles were analyzed using DLS, SEM, TEM and BET. The particle size was approximately 115 to 150 nm and the surface area was approximately 700 m2/g. The thermal stability of the particles and their exothermic heat release reactions during synthesis were explored using TGA and DSC, respectively.

摘要 I Abstract II 致謝 III 總目錄 IV 圖目錄 VIII 表目錄 XII 第一章 序論 1 1.1 乳液的簡介 1 1.2 奈米二氧化矽材料的發展 3 1.3 研究目的 5 第二章 文獻回顧 6 2.1 奈米二氧化矽的製備與應用 6 2.1.1 二氧化矽 6 2.1.2 二氧化矽的製備 6 2.1.3 奈米二氧化矽的應用 7 2.2 奈米粒子改質 8 2.2.1 物理改質 9 2.2.2 化學改質 9 2.3 孔洞性材料的介紹 13 2.3.1 微孔洞奈米二氧化矽 13 2.4 溶膠-凝膠法 15 2.4.1 溶膠-凝膠法之反應機構 15 2.4.2 溶膠-凝膠法之控制變因 18 第三章 實驗藥品、儀器與方法 22 3.1 實驗藥品 22 3.2 實驗設備與儀器 26 3.3 實驗流程與步驟 29 3.4 鑑定與分析 32 3.4.1 稀釋液的配置 34 3.4.2 動態光散射粒徑分析儀 (Dynamic Light Scattering, DLS) 35 3.4.3 高解析度場發射掃描式電子顯微鏡 (High Resolution Field-Emission Scanning Electron Microscope, SEM) 36 3.4.4 表面積及孔徑分析儀 (Surface Area and Pore size distribution Analyzer, BET) 37 3.4.5 穿透式電子顯微鏡 (Field Emission Trans Electron Microscope, TEM) 39 3.4.6 熱重/熱示差分析儀 (Termal Analyzer, TGA) 40 3.4.7 微分式掃描熱量分析儀 (Differential Scaning Calorimeter, DSC) 41 第四章 實驗結果與討論 42 4.1 不同TEOS/Styrene比例之奈米二氧化矽製備與鑑定 44 4.1.1 時間對粒徑的分析 44 4.1.2 粒子型態分析 49 4.1.3 TGA分析 55 4.1.4 比表面積分析 56 4.1.5 鍛燒後粒子型態分析 58 4.2 改變偶合劑含量之奈米二氧化矽製備與鑑定 63 4.2.1 時間對粒徑的分析 63 4.2.2 粒子型態分析 65 4.2.3 TGA分析 67 4.2.4 比表面積分析 68 4.2.5 鍛燒後粒子型態分析 69 4.3 合成複合型奈米二氧化矽的DSC分析 72 4.3.1溫度效應的分析 72 4.3.2酸鹼效應的分析 74 4.3.3不同TEOS/Styrene比例之奈米二氧化矽的分析 77 4.3.4改變偶合劑含量之奈米二氧化矽的分析 79 第五章 結論 81 第六章 參考文獻 83 附錄 89

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