Conversion Process of Perhydropolysilazane to Silica※
Received date: 2021-12-31
Online published: 2022-04-18
Supported by
National Defense Basic Scientific Research Program of China(JCKY2020203B019); Excellent Member of the Youth Innovation Promotion Association, Chinese Academy of Sciences(CAS)
Perhydropolysilazane (PHPS) derived silica materials have received extensive attention due to their potential applications in fields of memory chip and flexible display encapsulation. However, the current understanding of PHPS conversion process is not deepened yet, which is unfavorable to further research. To clarify PHPS conversion process, this work systematically studied conversion mechanism from PHPS to silica, and investigated the influence of chemical composition and microstructure on volume shrinkage, refractive index and mechanical properties in the conversion process. The coating samples were prepared by hydrolysis and condensation reaction of PHPS under conversion condition of heat. Chemical composition and microstructure of the obtained samples were analyzed by Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, energy dispersive spectrometer and peak table mode of atomic force microscope. It is found that, when the conversion temperature is below 180 ℃, the conversion of PHPS is dominated by the hydrolysis and condensation reaction of Si—H and Si—N bonds, and its conversion degree is low. The formed samples show sea-island structure, which is composed of a dispersed silica phase and continuous PHPS phase. When the conversion temperature is in the range of 180~300 ℃, the transformation depends on oxidation reaction. It results in growth of silica phase, formation of bi-continuous phase, phase reverse between PHPS and silica phase with the temperature above 200 ℃, and formation of continuous silica phase. When the conversion temperature is in the range of 300~600 ℃, the silica network is basically formed, and it is densified by further treatment at higher temperature. The volume shrinkage, refractive index, and mechanical properties of PHPS converted samples depend on the conversion degree and phases’ distribution.
Dan Wang , Xiang Guo , Pengfei Li , Yulin Zhang , Caihong Xu , Zongbo Zhang . Conversion Process of Perhydropolysilazane to Silica※[J]. Acta Chimica Sinica, 2022 , 80(6) : 734 -740 . DOI: 10.6023/A21120621
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