含中孔洞二氧化矽球之電活性聚亞醯胺複合材料之合成、鑑定及性質研究

Preparation, Characterization and Properties Studies of Electro-active Polyimide Composites Containing Mesoporous Silica Spheres

趙公義(Kung-Yi Chao)

指導教授 ： 葉瑞銘

中原大學/理學院/化學研究所/碩士(2011年)

https://doi.org/10.6840/cycu201101086

摘要

本研究論文主要在製備一系列具低介電常數及低熱傳係數之電活性聚亞醯胺/中孔洞二氧化矽複合薄膜材料。 首先，本實驗利用非介面活性劑以一步法製備含氨基之中孔洞矽球，其粒徑大小約500 nm。 其次，將適量之含氨基中孔洞矽球導入胺基封端之苯胺三聚體與二酸酐之反應溶液中，再進行熱縮合聚合反應至250 ℃，來製備一系列具電活性聚亞醯胺-中孔洞與無孔洞二氧化矽(EPI-AMS與ARS)之複合薄膜材料。
由研究結果顯示: 電活性聚亞醯胺中孔洞二氧化矽複合薄膜(EPIMS)較純的電活性聚亞醯胺薄膜(EPI)有低的介電係數與熱傳導係數；反之，電活性聚亞醯胺無孔洞二氧化矽質複合薄膜(EPIRS)則有較高的介電係數與熱係數。 由掃描式與穿透式電子顯微鏡得知二氧化矽粒子在聚亞醯胺薄膜基材中的分散狀況是均勻分散。 由熱失重分析儀(TGA) 、微分掃描分析儀(DSC)得知，二種複合膜材在熱性質與純的電活性聚亞醯胺沒有太大的差別，而機械性質可由動態機械分析儀(DMA)量測可得，因為中孔洞複合薄膜的交聯程度較好，所以其儲存模數較無孔洞的為佳。

關鍵字

電活性聚亞醯胺 ； 氨基中孔洞矽球 ； 胺基封端苯胺三聚體

並列摘要

In this study, we present the first synthesis and characterization of electroactive polyimide-mesoporous silica spheres with low dielectric constant and thermal conductivity simultaneously. First of all, amino-modified mesoporous silica spheres were synthesized by base-catalyzed sol-gel reactions of TEOS and APTES with fructose as non-surfactant template, followed by characterization by 13C-NMR and 29Si-NMR spectroscopy. Porosity of as-prepared amino-modified mesoporous silica spheres was determined by BET. Subsequently, the suitable amount of as-prepared mesoporous silica spheres was incorporated into the solution containing diamine of amine-capped aniline trimer (ACAT) and dianhydride of BSAA, followed by thermal imidization up to 250℃. Dispersion of silica spheres with/without porosity in polyimide matrix was identified by TEM observations.
It should be noted that the as-prepared composite membranes containing mesoporous silica spheres was found to show lower dielectric properties and thermal conductivity than the corresponding pure polyimide. However, the composite membranes containing raw silicon spheres without mesoporous structures was found to reveal higher dielectric properties and thermal conductivity than neat polymer membrane. Dielectric constant and thermal conductivity of as-prepared samples was determined by dielectric constant analyzer and Hot Disk, respectively. Moreover, thermal properties of all composite membranes were found to slightly higher than corresponding neat polymer membrane, as identified by thermal gravimetric analyzer (TGA) and differential scanning analyzer (DSC). Mechanical strength of as-prepared membranes was measured by dynamic mechanical analyzer (DMA).

並列關鍵字

amino-modified mesoporous silica spheres ； electroactive polyimide

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