Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/3101
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dc.contributor林慶炫zh_TW
dc.contributor.author許志光zh_TW
dc.contributor.authorHsu, Chin-Kuangen_US
dc.contributor.other化學工程學系所zh_TW
dc.date2013en_US
dc.date.accessioned2014-06-06T05:31:07Z-
dc.date.available2014-06-06T05:31:07Z-
dc.identifierU0005-0108201311291900en_US
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dc.identifier.urihttp://hdl.handle.net/11455/3101-
dc.description.abstract第一部分為以DOPO進行親核性加成於在酸催化下的四種雙酚,包含雙酚A、4,4’-異亞丙基雙(2,6-二甲基苯酚)’ 、9,9’-二(4-羥基苯基)芴、雙(4-羥基苯基)環己烷,得到磷系酚基單體(1-4),接著經由兩步製程,得到雙胺單體(9-12)。以單體(9-12)與ODA以及二酸酐進行聚合得到共聚醯亞胺,由於四種雙胺結構上有相似程度,我們將單體9所製備的聚醯亞胺來與單體10所製備的聚醯亞胺進行比較,單體11所製備的聚醯亞胺與單體12所製備的聚醯亞胺進行比較。含單體10的聚醯亞胺其結構上有較多的methyl官能基,因此比含單體9的聚醯亞胺有較高的玻璃轉移溫度、模數、尺寸安定性、接觸角度、溶解度等優點。而含單體11的聚醯亞胺其結構上的芴官能基比單體10的環己烷立體障礙較大、較剛硬,因此玻璃轉移溫度較高。 第二部分為以脂肪族雙胺,分別利用傳統一步法與兩步法合成Benzoxazine單體(2),藉由氫譜追蹤分析,發現以傳統一步法尚無法解決Triazine快速生成的問題,因此改用兩步法製備。將單體(2)與環氧樹脂(CNE、DCPDE)進行共聚,探討其性質。以吸水率以及介電儀分析,均顯示出含脂肪族結構的固化物因極性較低,有較低的吸水率以及較低的介電常數,以固化物(2)/DCPDE吸水率1.149%,介電常數2.75最為優異。zh_TW
dc.description.abstract[Part 1] Four novel diamines (9-12) were prepared by a two-step procedure from phosphinated phenols (1-4), which were prepared from acid-fragmentation of four bisphenols, including Bisphenol A, 4,4′-isopropylidenebis(2,6-dimethylphenol), 9,9’-bis(4-hydroxyphenyl)fluorene, and cis(4-hydroxyphenyl)cyclohexane, followed by nucleophilic addition of 9,10-dihydro-oxa-10-phosphaphenanthrene-10-oxide (DOPO). Copolyimides based on (9-12)/ 4, 4’-diaminodiphenyl ether /dianhydride were prepared. Due to the structure similiarity, (9)-containing copolyimides are compared with (10)-containing copolyimide, while (11)-containing copolyimides are compared with (12)-containing copolyimide. The structure-property relationship on the copolyimides was discussed. (10)-Containing copolyimides with the tetramethyl substitutent display higer Tg, modulus, dimensional stability, contact angle, and better solubility than (9)-containing copolyimides. The fluorene structure make (11)-containing copolyimides exhibit higher Tg than (12)-contaiing copolyimides. [Part 2] An aliphatic benzoxazine (2) was prepared via one-pot and two-pot. By analysis of 1H-NMR of monomer (2), we found that monomer (2) prepared via one-pot still have triazine in cosolvent. Monomer (2) and epoxy(CNE/DCPDE) copolymerized in the curing system. The (2)/DCPDE thermoset has the lowest moisture absorption and dielectric constant due to the aliphatic group.en_US
dc.description.tableofcontentsPart I 第一章 緒論 2 第二章 文獻回顧 4 2-1聚醯亞胺的生成 4 2-2聚醯亞胺的改質 7 2-3磷系材料的開發 10 2-4 酸催化製備酚基單體 12 3-1藥品 15 3-2儀器設備 16 3-3實驗規劃 21 3-3-1實驗簡介 21 3-3-2單體(1-12)製備 22 3-3-3聚醯亞胺(O-series nad B-series)製備 25 3-4單體合成 26 3-4-1單體(1)的合成 26 3-4-2單體(2)的合成 27 3-4-3單體(3)的合成 28 3-4-4單體(4)的合成 29 3-4-5單體(5)的合成 30 3-4-6單體(6)的合成 31 3-4-7單體(7)的合成 32 3-4-8單體(8)的合成 33 3-4-9單體(9)的合成 34 3-9-10單體(10)的合成 35 3-4-11單體(11)的合成 36 3-4-12單體(12)的合成 37 3-5聚合物合成 38 3-5-1聚醯亞胺(B-9 )之共聚 38 3-5-2聚醯亞胺(O-series and B-series)之共聚 39 3-5-3聚醯亞胺(O-ODA and B-ODA)之合成 40 3-6聚醯亞胺薄膜製備 41 第四章 單體鑑定與分析 42 4-1 單體(1)-(4)合成討論與結構鑑定 42 4-1-1單體(2)光譜鑑定與分析 43 4-1-2單體(3)光譜鑑定與分析 47 4-1-3單體(4)光譜鑑定與分析 51 4-2單體(5)-(8)合成討論與結構鑑定 55 4-2-1 單體(5)光譜鑑定與分析 56 4-2-2 單體(6)光譜鑑定與分析 60 4-2-3 單體(7)光譜鑑定與分析 64 4-2-4 單體(8)光譜鑑定與分析 68 4-3 單體(9)-(12)合成討論與結構鑑定 72 4-3-1 單體(9)光譜鑑定與分析 73 4-3-2單體(10)光譜鑑定與分析 77 4-3-3單體(11)光譜鑑定與分析 81 4-3-4單體(12)光譜鑑定與分析 85 第五章 聚合物性質分析 89 5-1聚合物(B-9 WITH DIFFERENT RATIO)合成探討 89 5-1聚合物(O-SERIES AND B-SERIES)FTIR鑑定 90 5-3-1 TMA分析 93 5-3-2 DMA分析 96 5-3-3 TGA分析 98 5-3聚合物機械性質測試 102 5-4 X-RAY測試 105 5-4 接觸角(CONTACT ANGLE)測試 106 5-5 薄膜性質 108 第六章 結論 109 Part II 第一章 緒論 112 第二章 文獻回顧 114 2-1 BENZOXAZINE簡介 114 2-2低介電POLYBENZOXAZINE的開發 120 2-3 研究動機 125 3-1藥品 126 3-2儀器設備 127 3-3實驗規劃 131 3-3-1 實驗簡介 131 3-3-2 Benzoxazine單體合成 132 3-4 單體合成 133 3-4-1 單體(1)合成 133 3-4-2 單體(2)合成 134 3-4-3 單體(2)’合成 135 第四章 單體鑑定與分析 136 4-1 單體(1)光譜分析與鑑定 136 4-2 單體(2)光譜分析與鑑定 137 4-4 單體(2)傅立葉紅外線(FTIR)光譜分析 138 4-5 單體(2)之DSC鑑定 139 第五章 性質分析與討論 140 5-1 單體(2)''合成探討 140 5-2 POLYBENZOXAZINE合成與特性 145 5-3 共聚物固化 147 5-4 固化物熱性質分析 149 5-5 吸水性測試與比較 153 5-5電氣性質分析與比較 155 第六章 結論 156 參考文獻 157zh_TW
dc.language.isozh_TWen_US
dc.publisher化學工程學系所zh_TW
dc.relation.urihttp://www.airitilibrary.com/Publication/alDetailedMesh1?DocID=U0005-0108201311291900en_US
dc.subject聚醯亞胺zh_TW
dc.subjectPolyimideen_US
dc.subject低介電zh_TW
dc.subjectBenzoxazineen_US
dc.title新穎型磷系不對稱聚醯亞胺與低介電Benzoxazine之製備zh_TW
dc.titlePreparation of novel phosphinated unsymmetric polyimides and low-dielectric benzoxazineen_US
dc.typeThesis and Dissertationzh_TW
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