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| DC 欄位 | 值 | 語言 |
|---|---|---|
| dc.contributor.advisor | 謝國煌(Kuo-Huang Hsieh) | |
| dc.contributor.author | Hsien-Hung Huang | en |
| dc.contributor.author | 黃獻弘 | zh_TW |
| dc.date.accessioned | 2021-06-08T00:59:45Z | - |
| dc.date.copyright | 2015-02-04 | |
| dc.date.issued | 2015 | |
| dc.date.submitted | 2015-01-16 | |
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| dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/18323 | - |
| dc.description.abstract | 本論文研究主要分成三大個部分:
第一個部分乃是利用不同重量比的四乙氧基矽烷( Tetraethyl Orthosilicate , TEOS )加入奈米黏土中，使其進入奈米黏土的層與層之間，再使用酸當觸媒，使四乙氧基矽烷與奈米黏土進行溶膠-凝膠( Sol-Gel )反應，在奈米黏土的表面及層與層之間產生多孔性的二氧化矽無機粒子，利用此方法，使奈米黏土具有多孔洞的特性，並利用動態光散射雷射粒徑儀測試儀( Dynamic Light Scattring , DLS )、比表面積與孔隙分佈分析儀 ( Specific Surface Area & Pore Size Distribution Analyzer by as Adsorption Method )，測定其分散性和孔洞體積等等。第二部分乃是合成聚脲酯-醯亞胺膜( Poly( urea-imide ) film )，固定二苯基甲烷-4,4'-二異氰酸酯( Methylene Diphenyl Diisocyanate , MDI )的含量，調整不同比例的均苯四甲酸二酐( Pyromellitic Dianhydride , PMDA ) 和 4,4'-二氨基二苯醚( 4,4'-Oxydianiline , ODA )，再以一階段方法共聚合反應形成聚脲酯-醯亞胺，並利用熱重分析儀( Thermal Gravimetric Analysis , TGA )、拉力試驗機( Tensile Strength Test )，測定其熱性質、機械性質等等。第三部分乃是結合第一、二部分所合成之多孔性奈米黏土及聚脲酯-醯亞胺，製備出多孔性黏土/聚脲酯-醯亞胺奈米複材( Poly( urea-imide )/Clay ) Nanocomposite )，並研究不同添加量的多孔性改質黏土對聚脲酯-醯亞胺的性質影響，由實驗結果可以得知，隨著改質奈米黏土含量的增加，多孔性黏土/聚脲酯-醯亞胺奈米複合材料的熱性質、機械性質皆有所提升，並由於加入了多孔性的奈米黏土，介電性質有所下降。 | zh_TW |
| dc.description.abstract | In my thesis, it is composed of three major parts : In first part, I introduce different weight ratios of TEOS into layer of nano porous clay, and use acid as a catalyst to go through a condensation procedure named Sol-Gel reaction between TEOS and hydroxyl groups on the clay and thus resulting mesoporous silica inorganic nanoparticles or inside between layer and layer. On the basis of Dynamic Light Scattring ( DLS ), Specific Surface Area & Pore Size Distribution Analyzer, the dispersion property and pore volume can be controlled by varying the mass ratio TEOS/Clay and adding trace amount of acid as catalyst. The follow by second part, by utilizing One-step Method and different mass ratio of PMDA, ODA, and MDI, different structures of Poly( urea-imide )( PUI ) can be synthesized. The thermal stability and mechanical property are measured by Thermal Gravimetric Analysis ( TGA ) and Tensile Strength Test. The final parts is the combination of section one and two, Nano porous clay are blended with Poly( urea-imide ) to produce Poly( urea-imide )/Clay Nanocomposite. It can be determined by Thermal Gravimetric Analysis ( TGA ) and Tensile Strength Test that the thermal stability and mechanical property are enhanced by increasing the mass ratio between Clay and PUI. In addition, the dielectric constant is decreased with the increasing mass ratio of Clay/PUI. | en |
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| dc.description.tableofcontents | 致謝...................................................................................................................................I
中文摘要.........................................................................................................................II Abstract.........................................................................................................................III 目錄................................................................................................................................IV 圖目錄...........................................................................................................................VII 表目錄.............................................................................................................................IX 第一章 緒論...................................................................................................................1 1.1. 前言...........................................................................................................................1 1.2. 研究目的...................................................................................................................2 第二章 文獻回顧...........................................................................................................3 2.1. 黏土材料介紹...........................................................................................................3 2.1.1. 有機化的黏土改質........................................................................................6 2.2. 溶膠-凝膠( Sol-Gel )法............................................................................................7 2.2.1. 水解反應( Hydrolysis Reaction ) .................................................................9 2.2.2. 縮合反應( Condensation Reaction ) ...........................................................12 2.2.3. 均一粒徑分布之二氧化矽粒子..................................................................14 2.2.4. 以溶膠-凝膠法製備有機-無機混成材料方法...........................................17 2.3. 聚醯亞胺.................................................................................................................18 2.3.1. 聚醯亞胺之簡介 ( Polyimide , PI )............................................................18 2.3.2. 聚醯亞胺之合成( Polyimide Synthesis )....................................................20 2.3.3. 聚醯亞胺之特性與應用特性與應用......................................................... 25 2.3.4. 聚醯亞胺介電行為之影響因素因………………………………………. 27 2.3.5. 有機介電材料聚醯亞胺之應用…………………………………………..31 2.4. 聚胺酯-醯亞胺介紹................................................................................................33 2.4.1. 聚胺酯-醯亞胺合成.................................................................................. 34 2.5. 奈米複合材料.........................................................................................................36 2.5.1 有機-無機奈米複材料.................................................................................37 2.5.2高分子-黏土與改質黏土奈米複合材料......................................................38 2.6. 多孔材料介紹........................................................................................................42 2.6.1. 多孔洞高分子材料介紹.............................................................................43 2.6.2. 多孔洞有機-無機高分子複合材料............................................................45 第三章 實驗方法..........................................................................................................47 3.1. 實驗藥品…………………………………………………………………………47 3.2. 實驗儀器…………………………………………………………………………49 3.3. 實驗步驟…………………………………………………………………………52 3.3.1. 多孔性黏土製備………………………………………………………….52 3.3.2. 聚氨酯-醯亞胺製備……………………………………………………………55 3.3.3. 多孔性黏土/聚氨酯-醯亞胺之複合材料製備………………………………...57 3.4. 材料性質測試……………………………………………………………………59 3.4.1. 動態光散射雷射(Dynamic Light Scattring, DLS)粒徑儀測試……………….59 3.4.2. 傅立葉轉換紅外線光譜儀( Fourier-Transformed Infrared Spectra , FT-IR ) 分析測試……………………………………………………………………………....59 3.4.3. 熱重分析儀( Thermal Gravimetric Analysis , TGA )分析測試……………….59 3.4.4. 拉力試驗機( Tensile Strength Test )…………………………………………...59 3.4.5. X光繞射儀(X-ray Diffrectometer, XRD)……………………………………...59 3.4.6.介電量測儀( Agilent Precision LCR Meters，LCR )…………………………..60 3.4.7. 比表面積與孔隙分佈分析儀 ( Specific Surface Area & Pore Size Distribution Analyzer by as Adsorption Method )………………………………………………….60 第四章 結果與討論…………………………………………………………………62 4.1. 多孔性奈米黏土之傅立葉轉換紅外線光譜分析……………………..62 4.2. 多孔性奈米黏土之X光繞射測試分析……………………………....63 4.3. 多孔性奈米黏土之粒徑大小分析…………………………………….64 4.4. 多孔洞奈米黏土之比表面積與孔隙分佈分析……………………….71 4.5. 聚氨酯-醯亞胺以及多孔性黏土/聚氨酯-醯亞胺之熱重損失分( Thermal Gravimetric Analysis , TGA )………………………………………………..73 4.6. 聚氨酯-醯亞胺及多孔性奈米黏土/聚氨酯-醯亞胺之拉伸測試……..77 4.7. 聚氨酯-醯亞胺及多孔性奈米黏土/聚氨酯-醯亞胺之介電特性分析..79 第五章 結論…………………………………………………………………………81 參考文獻........................................................................................................................82 圖目錄 圖 2.1 黏土之結晶構造圖………………………………………………………5 圖 2.2 Sol-Gel水解反應機制圖…………………………………………………….9 圖 2.3 矽上取代基的誘導效應(R、OR、OH、OSi)…………………………………..10 圖 2.4 TEOS、H2O、Synasol於25℃的三相圖………………………………………11 圖 2.5矽烷氧化物縮合反應機制…………………………………………………...12 圖 2.6矽鹽在有水存在時的聚合反應示意圖………………………………………13 圖 2.7製作膠體粒子的三種不同方法……………………………………………....15 圖 2.8二氧化矽粒子成核成長機制示意圖…………………………………………15 圖 2.9 0.28M的四乙氧基矽烷在乙醇中以不同的氨濃度和水的濃度所製成的二氧化矽小球粒徑分佈……………………………………………………...16 圖 2.10 Kapton ( PMDA-ODA )化學結構…………………………………………….18 圖 2.11 二步合成法聚亞醯胺……………………………………………………..20 圖 2.12 一步合成法聚亞醯胺………………………………………………………...21 圖 2.13 加成型聚亞醯胺……………………………………………………………...22 圖 2.14 在不同頻率作用下極化機制對介電常數的影響…………………………27 圖 2.15 PU預聚法合成PUI…………………………………………………………...34 圖 2.16 以NH2( Amino )封端的PU預聚體和酸酐反應成PUI的機制……………34 圖 2.17 以-NCO封端的PI預聚體和二醇反應成PUI的機制………………………35 圖 2.18 高分子/黏土混成複合材料的種類…………………………………………..39 圖 2.19 原位聚合法製備高分子-黏土奈米複合材料之反應機制流程圖…………40 圖 2.20 孔洞的高分子薄膜機製圖…………………………………………………...43 圖 2.21 孔洞聚醯亞胺薄膜的合成機制圖…………………………………………44 圖 2.22 孔洞高分子複合材料示意圖…………………………………………...........46 圖 3.1 多孔性黏土示意圖…………………………………………………………….54 圖 3.2 反應單體結構圖……………………………………………………………….56 圖 3.3 聚氨酯-醯亞胺薄膜之製備流程圖……………………………………………56 圖 3.4 多孔性黏土/聚氨酯-醯亞胺之複合材料製備流程圖………………………58 圖 4.1多孔性奈米黏土之FT-IR圖……………………………………………………62 圖 4.2 多孔性奈米黏土之XRD圖…………………………………………………63 圖 4.3 NSP-Si-73粒徑分析結果………………………………………………………65 圖 4.4 NSP-Si-73-T11粒徑分析結果…………………………………………………65 圖 4.5 NSP-Si-73-T12粒徑分析結果…………………………………………………66 圖 4.6 NSP-Si-73-T13粒徑分析結果…………………………………………………66 圖 4.7 NSP-Si-73-T15粒徑分析結果…………………………………………………67 圖 4.8 C-NSP-Si-73粒徑分析結果……………………………………………………67 圖 4.9 C-NSP-Si-73-T11粒徑分析結果………………………………………………68 圖 4.10 C-NSP-Si-73-T12粒徑分析結果……………………………………………62 圖 4.11 C-NSP-Si-73-T13粒徑分析結果……………………………………………69 圖 4.12 C-NSP-Si-73-T15粒徑分析結果……………………………………………63 圖 4.13 聚氨酯-醯亞胺之TGA圖……………………………………………………74 圖 4.14不同比列改質黏土-聚脲酯-醯亞胺( MDI 0.5PMDA 0.5ODA )之TGA圖..75 圖 4.15不同比列改質黏土-聚氨酯-醯亞胺( MDI 0.8PMDA 0.2ODA )之TGA圖..75 圖 4.16不同比列改質黏土-聚氨酯-醯亞胺( MDI 0.9PMDA 0.1ODA )之TGA圖..76 表目錄 表 2.1 黏土種類………………………………………………………………………...4 表 2.2 加成型聚亞醯胺和縮合型聚亞醯胺之比較………………………………….24 表 2.3 聚醯亞胺與無機材料特性比較………………………………………………26 表 2.4 不同聚醯亞胺結構其極化能力對介電常數之影響…………………………28 表 2.5 不同聚醯亞胺結構其自由體積對介電常數之影響…………………………29 表 2.6 聚醯亞胺結構中氟基含量對介電常數之影響………………………………30 表 2.7 有機高分子低介電材料的基本特性………………………………………….32 表 2.8 Nylon 6 與Clay之熱性質及機械性質………………………………………..38 表 2.9 孔徑分類……………………………………………………………………….42 表 3.1不同重量比例的奈米黏土與四乙氧基矽烷之比例表……………………..52 表 4.1 改質黏土粒徑分析結果……………………………………………………….70 表 4.2 改質黏土孔洞體積、比表面積( BET )和孔洞直徑分析分析結果…………72 表4.3 經由燒結過後的改質黏土孔洞體積、比表面積( BET )和孔洞直徑分析分析結果………………………………………………………………………………72 表 4.4聚氨酯-醯亞胺之Td5%溫度…………………………………………………74 表 4.6改質黏土以不同比列混摻聚氨酯-醯亞胺( MDI 0.5PMDA 0.5ODA )之Td5%溫度……………………………………………………………………………77 表 4.6改質黏土以不同比列混摻聚氨酯-醯亞胺( MDI 0.8PMDA 0.2ODA )之Td5%溫度……………………………………………………………………………77 表 4.7改質黏土以不同比列混摻聚氨酯-醯亞胺( MDI 0.9PMDA 0.1ODA )之Td5%溫度……………………………………………………………………………77 表 4.8 聚氨酯-醯亞胺之Elongation ( % )和Tensile Strength ( MPa )…………….....78 表 4.9改質奈米黏土/聚氨酯-醯亞胺( MDI 0.5 PMDA 0.5 ODA )之Elongation和Tensile Strength………………………………………………………………..79 表 4.10改質奈米黏土/聚氨酯-醯亞胺( MDI 0.8 PMDA 0.2 ODA )之Elongation和Tensile Strength………………………………………………………………79 表 4.11改質奈米黏土/聚氨酯-醯亞胺( MDI 0.9PMDA 0.1 ODA )之Elongation和Tensile Strength………………………………………………………………..79 表 4.12聚氨酯-醯亞胺之介電常數…………………………………………………80 表 4.13改質黏土-聚脲酯-醯亞胺( MDI 0.5PMDA 0.5ODA )之介電常數………….81 表 4.13改質黏土-聚脲酯-醯亞胺( MDI 0.8PMDA 0.2ODA )之介電常數………….81 表 4.13改質黏土-聚脲酯-醯亞胺( MDI 0.9PMDA 0.1ODA )之介電常數………….81 | |
| dc.language.iso | zh-TW | |
| dc.title | 多孔性黏土及聚脲酯-醯亞胺複合材料之製備與性質探討 | zh_TW |
| dc.title | Synthesis and Characterization of Poly( urea-imide )/Clay Nanocomposite | en |
| dc.type | Thesis | |
| dc.date.schoolyear | 103-1 | |
| dc.description.degree | 碩士 | |
| dc.contributor.oralexamcommittee | 林江珍(Jiang-Zhen Lin),莊清男(Ching-Nan Chuang),陳思賢(Suz-Hsien Chen) | |
| dc.subject.keyword | 聚?酯-醯亞胺,聚醯亞胺,聚?酯,奈米黏土, | zh_TW |
| dc.subject.keyword | Polyimide,Polyurethane,Poly( urethane-imide ),Nanoclay, | en |
| dc.relation.page | 90 | |
| dc.rights.note | 未授權 | |
| dc.date.accepted | 2015-01-16 | |
| dc.contributor.author-college | 工學院 | zh_TW |
| dc.contributor.author-dept | 高分子科學與工程學研究所 | zh_TW |
| 顯示於系所單位： | 高分子科學與工程學研究所 | |
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