Yu Yang-Yen, Chien Wen-Chen, Lai Chiung-Lin
Department of Materials Engineering, Mingchi University of Technology, Taishan, Taipei Hsien 243, Taiwan.
J Nanosci Nanotechnol. 2009 Jul;9(7):4135-42. doi: 10.1166/jnn.2009.m22.
In this study, two types of the polyimide-silica hybrid thin films, 6FDA-ODA/SiO2 (FS0-FS50) and PMDA-ODA/SiO2 (PS0-PS40), with different silica content were synthesized by using the sol-gel method. TGA analysis showed that the thermal decomposition temperatures (T(d)) of FS and PS hybrid films were in the range of 457-505 degrees C and 458-516 degrees C, respectively. The T(d) increased with increasing the silica content. The measurement of contact angle and FTIR indicated that the hydrophilic and hydrolytic abilities were significantly improved when the silica content increased. The contact angle of PS0-PS40 films was in the range of 80.3-51.8 degrees. UV-Vis spectra showed that the cutoff wavelength of prepared hybrid films could be tunable through the silica content. The n&k analysis showed that the refractive index (n) of FS and PS hybrid films were in the range of 1.60-1.49 and 1.76-1.59, respectively, which could be controlled by the silica content. The extinction coefficients (k) are almost zero in the wavelength range of 300-900 nm, indicating the prepared hybrid films have an excellent optical transparency in the UV and visible region. TEM images showed that the particle size of silica in the hybrid thin films could be effectively controlled under sufficient content of coupling agent. Moreover, the results of SEM and AFM showed that the ratios of average roughness to thickness for all the prepared hybrid films were under 1.6%. It demonstrated that the prepared polyimide-silica hybrid thin films have an excellent film formability and planarity.
在本研究中,采用溶胶 - 凝胶法合成了两种不同二氧化硅含量的聚酰亚胺 - 二氧化硅杂化薄膜,即6FDA - ODA/SiO₂(FS0 - FS50)和PMDA - ODA/SiO₂(PS0 - PS40)。热重分析(TGA)表明,FS和PS杂化薄膜的热分解温度(T(d))分别在457 - 505℃和458 - 516℃范围内。T(d)随二氧化硅含量的增加而升高。接触角测量和傅里叶变换红外光谱(FTIR)表明,二氧化硅含量增加时,亲水性和水解能力显著提高。PS0 - PS40薄膜的接触角在80.3 - 51.8°范围内。紫外 - 可见光谱(UV - Vis)表明,所制备的杂化薄膜的截止波长可通过二氧化硅含量进行调节。n&k分析表明,FS和PS杂化薄膜的折射率(n)分别在1.60 - 1.49和1.76 - 1.59范围内,可由二氧化硅含量控制。在300 - 900nm波长范围内,消光系数(k)几乎为零,表明所制备的杂化薄膜在紫外和可见光区域具有优异的光学透明度。透射电子显微镜(TEM)图像显示,在偶联剂含量充足的情况下,杂化薄膜中二氧化硅的粒径可得到有效控制。此外,扫描电子显微镜(SEM)和原子力显微镜(AFM)结果表明,所有制备的杂化薄膜的平均粗糙度与厚度之比均低于1.6%。这表明所制备的聚酰亚胺 - 二氧化硅杂化薄膜具有优异的成膜性和平面度。