Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/3386
標題: Synthesis Characterization and properties of Epoxy/SiO2 and Polyimide/SiO2 nanocomposites
Epoxy/SiO2 和Polyimide/SiO2有機無機奈米複合材料之製備及性質研究
作者: 馮振嘉
chia, Feng Chen
關鍵字: sol-gel nanocomposites;溶膠-凝膠 奈米複合材料
出版社: 化學工程學系
摘要: 
本篇主要採用溶膠-凝膠法製備epoxy-SiO2和polyimide-SiO2 /有機/無機混成奈米複合材料;首先利用dopo改質icteos合成新型的偶合劑(dopo-icteos),並經由IR追蹤反應,再由1H,,13C and 31P-NMR,鑑定結構,新合成的偶合劑dopo-icteo當作溶膠-凝膠法的前驅物(presoursor),由於改直過的偶合劑含有苯環結構,所以跟有機高分子的相容性會提升,經由改質過的偶合劑改善有機相與無機相分離情形,再加以製備混摻型epoxy/SiO2型奈米複合材料,經由29Si-NMR可知道水解-縮合的程度,並知道內部為完整的網狀結構,並再由SEM、AFM觀察型態學,顯示良好的透光性和混合性,另外由DSC、TGA探討熱性質,可得Tg (160℃~169℃) ,而焦炭殘留率14% 到24%,代表熱性質有提升,從SEM 圖觀察並未有著一般無機材有的顯著顆粒分佈或是團塊聚集,代表有機/無機兩相間的差異並不很明顯,相分離的情況並不顯著,或許是環氧樹酯上的-COH基和-Si-OH基,兩者進行水解縮合後,形成-C-O-Si-鏈段,所以未有巨觀的相分離,而從AFM可以觀察到silica 粒徑大約為20nm,證明為奈米級材料,另外比起原來環氧樹酯,吸濕性也有所降低(1.2% ~0.7%),介電係數(3.29~3.17),比起原來的環氧樹酯稍微降低了一些,顯示經由導入dopo-icteos可以提升Tg,降低吸濕性、介電係數及介電損失,良好的熱安定性,另外製備的混摻型polyimide/SiO2經由29SiNMR可知道水解-縮合的很完全,內部為完整的網狀結構,熱重損失溫度在500℃以上,代表熱安定性很好,並且從AFM可以觀察到silica 粒徑大約為20nm而且有機/無機兩相排列的很整齊,證明為奈米級複合材料。

A novel phosphorus-containing tri-ethoxysilane (dopo-icteos) was synthesized from the addition reaction of 9,10-dihydro-9-oxa
-10-phosphaphenanthrene 10-oxide (dopo) and 3-(trieoxysilyl) isocyanate (icteos ). The structure was confirmed by IR spectrum,1H、13C、and 31P-NMR。Epoxy/SiO2 and PI/SiO2 nanocomposites were obtained from the in-situ curing of diglycidyl ether of bisphenol A /4,4-diaminodiphenylmethane /dopoicteos and poly amic acid /dopo-icteos,respectively。The resulted epoxy/SiO2 nanocomposites revealed exhibit higher glass transition temperatures (161~169℃) and char yield (21%~26%)。The phase separation of epoxy/SiO2 observed by SEM is not so obvious compared with the of Polyimide/SiO2 nanocomposites due to the dehydration reaction between hydroxyl group (-C-OH) of epoxy resin and the silanol group (-Si-OH) of silicon network。
From AFM images,the particle size of SiO2 is 20 nm in diameter , implying nanocomposites were achieved。The moisture absorption was lowered (1.2%~0.7%),and dielectrical constant was also lowered (3.29~3.17)。For PI/SiO2 system,from AFM images,the particle size of SiO2 is 20 nm in diameter,observed by AFM。
URI: http://hdl.handle.net/11455/3386
Appears in Collections:化學工程學系所

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