氮化硅纤维的聚硅氮烷氧热交联法制备及其性能

doi:10.13475/j.fzxb.20210505807

摘要/Abstract

摘要：

为探究聚硅氮烷(PSZ)纤维氧热交联不熔化处理最佳工艺和氧热交联对PSZ纤维及氮化硅(Si₃N₄)纤维组成与结构的影响,以甲基二氯硅烷和二甲基二氯硅烷为原料,通过氨解、热聚合、熔融纺丝、氧热交联及裂解等工艺制备了Si₃N₄纤维。借助傅里叶红外光谱仪、扫描电子显微镜、X射线衍射仪等对样品的结构和性能进行测试与分析。结果表明:PSZ纤维在120 ℃保温12 h进行氧热交联后,其陶瓷产率较未处理纤维提升了约10.2％,最后在1 400 ℃保温2 h裂解可得到表面光滑平坦、无沟槽裂纹等缺陷的Si₃N₄纤维;将Si₃N₄纤维继续在空气气氛下于1 500 ℃氧化处理2 h,可在纤维表面氧化形成一层SiO₂,是典型的皮芯结构纤维。

关键词: 先驱体转化法, 聚硅氮烷, 氮化硅纤维, 氧热交联

Abstract:

To explore the optimum technology of oxygen thermal cross-linking for polysilazane (PSZ) fibers and the effect of oxygen thermal cross-linking on compositions and structures of PSZ fibers and silicon nitride (Si₃N₄) fibers, Si₃N₄ fibers were successfully prepared using methyldichlorosilane and dimethyldichlorosilane as raw materials by ammonolysis polycondensation, thermopolymerization, melt spinning, oxygen thermal cross-linking and pyrolysis. Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and some other measures were utilized to analyze the structure and properties of the samples. After the PSZ fibers cured at 120 ℃ for 12 h, its ceramic yields were higher than that of uncured PSZ fibers by about 10.2％. The Si₃N₄ fibers with smooth flat surface and without groove cracks and other defects were obtained by pyrolysis of the cured PSZ fibers at 1 400 ℃ for 2 h. Furthermore, a layer of SiO₂ crystalline phase was observed on the surface of the Si₃N₄ fibers after high-temperature oxidation in air at 1 500 ℃ for 2 h. The obtained fibers after oxidation was a typical type of skin-core structure fibers.

Key words: precursor derived method, polysilazane, silicon nitride fiber, oxygen thermal cross-linking

中图分类号:

TB34

李海龙, 陈建军, 鲍之豪, 熊艺莲, 林文鑫. 氮化硅纤维的聚硅氮烷氧热交联法制备及其性能[J]. 纺织学报, 2022, 43(08): 48-54.

LI Hailong, CHEN Jianjun, BAO Zhihao, XIONG Yilian, LIN Wenxin. Preparation and properties of silicon nitride fibers by oxygen thermal cross-linking of polysilazane[J]. Journal of Textile Research, 2022, 43(08): 48-54.

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纤维名称	O1s	N1s	C1s	Si2s	Si2p
PSZ纤维	2.79	16.02	38.97	21.01	21.22
Si₃N₄纤维	17.47	11.50	30.24	19.89	20.89