Preparation, thermal properties, morphology, and microstructure of phosphorus-containing epoxy/SiO₂ and polyimide/SiO₂ nanocomposites

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• 作者：Ching Hsuan Lin ; Chen Chia Feng ; Ting Yu Hwang
• 关键词：Epoxy ; Polyimide ; Nanocomposites ; Sol– ; gel ; ²⁹Si NMR
• 刊名：European Polymer Journal
• 出版年：2007
• 期刊代码：35_00143057
• 类别：ms
• 出版时间：March 2007
• 卷：43
• 期：3
• 页码：725-742
• 文件大小：2582 K

摘要

A phosphorus-containing tri-ethoxysilane (dopo-icteos) reacting from the nucleophilic addition reaction of 9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (dopo) and 3-(trieoxysilyl) isocyanate (icteos) was synthesized. The structure of dopo-icteos was confirmed by ¹H, ¹³C, ³¹P NMR and IR spectra. A triethylamine catalyzed mechanism for the dopo-icteos synthesis was proposed and verified by NMR spectra. The phosphorus-containing epoxy/SiO₂ and polyimide/SiO₂ nanocomposites were prepared from the in-situ curing of diglycidyl ether of bisphenol A (DGEBA)/4,4-diaminodiphenylmethane(DDM)/dopo-icteos, and imidization of poly(amic acid) of pyromellitic dianhydride (PMDA)/4,4′-oxydianiline (ODA)/dopo-icteos, respectively. The microstructure and morphology were investigated by ²⁹Si NMR, scanning electron microscope (SEM), EDS (Si and P mapping) analysis and atomic force microscope (AFM). The thermal properties, flame retardancy and dielectric properties of the organic–inorganic hybrids were investigated by differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), limiting oxygen index (LOI), thermal gravimetric analysis (TGA) and dielectric analyzer (DEA).