Kim Youngkyoo, Ha Chang-Sik, Chang Taehyun, Lee Won-Ki, Goh Wanhee, Kim Hwajeong, Ha Youri, Ree Moonhor
Organic Nanoelectronics Laboratory, Department of Chemical Engineering, Kyungpook National University, Daegu 702-701, Republic of Korea.
J Nanosci Nanotechnol. 2009 Aug;9(8):4633-43. doi: 10.1166/jnn.2009.1081.
Here we report the influence of the polyimide precursor type on the surface morphology and properties of poly(p-phenylene biphenyltetracarboximide) (BPDA-PDA PI)/silica hybrid composite films. Two types of precursor polymer were employed: poly(p-phenylene biphenyltetracarboxamic acid) (BPDA-PDA PAA) and poly(p-phenylene biphenyltetracarboxamic diethyl ester) (BPDA-PDA PES). These precursor polymers were mixed with tetraethoxysilane in the presence of HCl and H2O, which led to the precursor mixture films that contain in-situ generated silica particles via sol-gel process. Then the precursor mixture films were subject to thermal imidization to make polyimide/silica hybrid composite films. Results showed that the PAA precursor has better compatibility with silica particles, which is mainly attributed to the early making of silyl ester bonds (as evidenced by X-ray photoelectron spectroscopy) between carboxylic acid groups in the PAA and hydroxyl groups in silanol molecules. Further evidences were provided by the measurement of surface nanomorphology, crystal nanostructure, thermal/mechanical properties, and optical birefringence.
在此,我们报道了聚酰亚胺前驱体类型对聚(对苯撑联苯四羧酸二亚胺)(BPDA - PDA PI)/二氧化硅杂化复合薄膜表面形态和性能的影响。使用了两种类型的前驱体聚合物:聚(对苯撑联苯四羧酸)(BPDA - PDA PAA)和聚(对苯撑联苯四羧酸二乙酯)(BPDA - PDA PES)。这些前驱体聚合物在盐酸和水存在的情况下与四乙氧基硅烷混合,这导致通过溶胶 - 凝胶过程形成含有原位生成二氧化硅颗粒的前驱体混合薄膜。然后将前驱体混合薄膜进行热亚胺化以制备聚酰亚胺/二氧化硅杂化复合薄膜。结果表明,PAA前驱体与二氧化硅颗粒具有更好的相容性,这主要归因于PAA中的羧酸基团与硅醇分子中的羟基之间早期形成了硅酯键(X射线光电子能谱证明)。通过表面纳米形态、晶体纳米结构、热/机械性能和光学双折射的测量提供了进一步的证据。