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研究生: 陳芝婷
Chih-Ting Chen
論文名稱: 潛在型硬化劑之微膠囊包覆技術開發
Development of Microcapsulation of Latent Curing Agent
指導教授: 邱顯堂
Hsien-Tang Chiu
口試委員: 邱士軒
Shih-Hsuan Chiu
李俊毅
Jiunn-Yih Lee
游進陽
Chin-Yang Yu
學位類別: 碩士
Master
系所名稱: 工程學院 - 材料科學與工程系
Department of Materials Science and Engineering
論文出版年: 2011
畢業學年度: 99
語文別: 中文
論文頁數: 74
中文關鍵詞: 異方性導電膜咪唑噴霧乾燥微膠囊
外文關鍵詞: Anisotropic conductive film (ACF), Imidazole, Spray dryer, Microcapsule
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  針對異方性導電膜(Anisotropic Conductive Film, ACF)未來應用之需求,期望開發出能快速硬化,儲存壽命長之配料系統,並能符合應用之性能。
  本研究選用咪唑化合物做為環氧樹脂之硬化劑。使用濕式研磨機降低硬化劑粒徑達奈米級,再以噴霧乾燥法製備微膠囊。咪唑之結構是利用傅立葉轉換紅外線光譜儀進行官能基分析及鑑定;利用熱重損失分析儀、熱示差掃描量熱儀與熱機械分析儀進行熱性質及熱機械性質之分析;以動態光散射儀及掃描式電子顯微鏡進行粒徑及型態學分析。
  物理學方面,以動態光散射儀量測濕式研磨之粒徑變化,證實隨研磨時間增加,粒子逐漸變小達奈米級;掃描式電子顯微鏡觀察微膠囊表面型態為完整球體,可知硬化劑已完全包覆。熱性質方面,由熱示差掃描量熱儀及熱重損失分析觀察硬化劑經微膠囊化前後與環氧樹脂反應發現:經由微膠囊包覆,能夠有效延遲環氧樹脂與硬化劑反應時間,可經由選擇殼層材質,製備不同反應速率之潛在型硬化劑。


For the requirement and application of anisotropic conductive film (ACF) in the future, the development of ACF formulation is expected to be rapid hardening and long shelf life.
In this study imidazole compounds were employed to be hardener of the epoxy. Wet-milling method is used to reduce the particle size of hardener into nano-size scale; moreover the milled hardeners were microencapsulated by spray dryer. The chemical structures of imidazole compounds were characterized by Fourier Transform Infrared Spectrometer (FT-IR). The thermal properties and thermal mechanical properties of epoxy resin/hardener system were analyzed by thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and thermal mechanical analysis (TMA) respectively. In addition the particle size and morphology of epoxy resin/ hardener system were characterized by dynamic light scattering (DLS) and scanning electron microscopy (SEM) respectively.
DLS analysis showed that an increase in milling time causes the decrease in particle size to nano-size scale. SEM observation demonstrated the hardeners were fully-coated on PU as sphere-shape microcapsules. From DSC and TGA analysis, the reaction time of epoxy/hardener system increased due to microencapsulation and the latent hardener in varied reaction rate might be prepared from different microencapsule shell material.

中文摘要......................................................................I 英文摘要.....................................................................II 誌謝........................................................................III 目錄.........................................................................IV 圖目錄.......................................................................VI 表目錄.....................................................................VIII 第一章 緒論..................................................................1 1-1 研究背景.................................................................1 1-2 前言.....................................................................2 第二章 文獻回顧.............................................................11 2-1 觸媒....................................................................11 2-2 濕式研磨................................................................15 2-3 噴霧乾燥................................................................24 2-4 受包覆方法影響之微球粒子結構............................................31 第三章 實驗部分.............................................................34 3-1 實驗流程................................................................34 3-2 實驗材料................................................................35 3-3 實驗儀器原理及操作程序..................................................37 3-3-1 傅立葉轉換紅外線光譜儀(Fourier Transform Infrared Spectrometer, FT-IR).............................................37 3-3-2 熱重損失分析儀(Thermal Gravimetric Analyzer, TGA)................37 3-3-3 熱示差掃描量熱儀(Differential Scanning Calorimeter, DSC).........38 3-3-4 掃描式電子顯微鏡/能量散佈分析儀(Scanning Electron Microscope/ Energy Dispersive Spectrometer, SEM/ EDS)............39 3-3-5 動態光散射儀(Dynamic Light Scattering, DLS)......................40 3-3-6 濕式研磨(Wet–milling)...........................................41 3-3-7 噴霧乾燥(Spray dryer) ...........................................42 3-3-8 熱機械分析儀(Thermo-mechanical Analyzer, TMA)....................43 第四章 結果與討論...........................................................45 4-1 環氧樹脂及硬化劑結構分析鑑定............................................45 4-2 環氧樹脂和硬化劑之硬化行為分析..........................................48 4-3 濕式研磨之粒徑變化分析..................................................51 4-4 微膠囊化(Spray dryer).................................................54 4-5 微膠囊化後硬化行為分析..................................................57 第五章 結論.................................................................64 參考文獻.....................................................................65 附錄.........................................................................71 作者簡介.....................................................................75

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