氮化硅纤维的聚硅氮烷氧热交联法制备及其性能  

Preparation and properties of silicon nitride fibers by oxygen thermal cross-linking of polysilazane

作　　者：李海龙 陈建军[1] 鲍之豪 熊艺莲 林文鑫 LI Hailong;CHEN Jianjun;BAO Zhihao;XIONG Yilian;LIN Wenxin(School of Materials Science and Engineering,Zhejiang Sci-Tech University,Hangzhou,Zhejiang 310018,China)

机构地区：[1]浙江理工大学材料科学与工程学院,浙江杭州310018

出　　处：《纺织学报》2022年第8期48-54,共7页Journal of Textile Research

基　　金：国家自然科学基金项目(51872262,51572243)。

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(Si_(3)N_(4))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Si_(3)N_(4)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1400℃保温2 h裂解可得到表面光滑平坦、无沟槽裂纹等缺陷的Si_(3)N_(4)纤维;将Si_(3)N_(4)纤维继续在空气气氛下于1500℃氧化处理2 h,可在纤维表面氧化形成一层SiO_(2),是典型的皮芯结构纤维。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(Si_(3)N_(4))fibers,Si_(3)N_(4) 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 Si_(3)N_(4) fibers with smooth flat surface and without groove cracks and other defects were obtained by pyrolysis of the cured PSZ fibers at 1400℃for 2 h.Furthermore,a layer of SiO_(2) crystalline phase was observed on the surface of the Si_(3)N_(4) fibers after high-temperature oxidation in air at 1500℃for 2 h.The obtained fibers after oxidation was a typical type of skin-core structure fibers.

关 键 词：先驱体转化法 聚硅氮烷 氮化硅纤维 氧热交联 

分 类 号：TB34[一般工业技术—材料科学与工程]