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以聚硅碳硅烷(polysilacarbosilane,PSCS)与乙酰丙酮锆为原料,用常压高温裂解法制备了Si-Zr-C-O纤维先驱体聚锆碳硅烷(polyzirconocar- bosilane,PZCS),经过熔融纺丝、空气预氧化、惰性气氛烧成等工艺,制得Si-Zr-C-O纤维。通过元素分析、Auger电子能谱、X射线衍射、核磁共振和扫描电子显微镜等一系列分析测试手段研究了Si-Zr-C-O纤维的组成结构与性能。结果表明:Si-Zr-C-O纤维的元素组成为SiC_(1.24)H_xO_(0.56)Zr_(0.0129) (摩尔比),平均强度为2.50Pa,平均直径为11μm,纤维表面光滑平坦,没出现孔洞、裂纹、沟槽等缺陷,直径均匀。Si-Zr-C-O纤维表层和内部元素组成不同。Si-Zr-C-O纤维为非晶SiC纤维,纤维中包含较多的不定形游离C和O,以不定形SiC_xO_y复合相的形式存在,Zr则与复合相中的O相结合。
Polyzirconocarbosilane (PZCS), a precursor of Si-Zr-CO fiber, was prepared by atmospheric pressure pyrolysis method using polysilacarbosilane (PSCS) and zirconium acetylacetonate as starting materials. After melt spinning, Air pre-oxidation, inert atmosphere firing process, prepared Si-Zr-CO fiber. The composition and properties of Si-Zr-C-O fibers were investigated by elemental analysis, Auger electron spectroscopy, X-ray diffraction, nuclear magnetic resonance and scanning electron microscopy. The results show that the elemental composition of Si-Zr-CO fiber is SiC 1.24 H x O 0.56 Zr 0.0129 (molar ratio), the average strength is 2.50 Pa, the average diameter is 11 μm, the fiber surface is smooth and flat, Cracks, grooves and other defects, uniform diameter. Si-Zr-C-O fiber surface and internal elements of different composition. Si-Zr-C-O fibers are amorphous SiC fibers. Fibers contain more amorphous C and O, exist in the form of amorphous SiC_xO_y phase, while Zr is combined with O in the composite phase.