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用聚碳硅烷与钛酸四正丁酯(titanium tetrabutoxide,TBT)在200℃氮气气氛中反应5h得到含过量TBT的聚钛碳硅烷(polytitanocarbosilane,TPTC)先驱体。将先驱体TPTC于160℃熔融纺丝制得原纤维后,经空气中100℃熟化处理20h,200℃交联处理20h及1200℃烧结可原位制得TiO2/SiO2纤维。利用红外光谱、核磁共振(13C,29Si)、X射线衍射、扫描电镜和能量散射X射线光谱分析表征发现:随着TBT量的增加,TPTC中的Si—H键含量减少,Si—O键增多;纤维由无定形SiO2和锐钛矿TiO2组成,表面光滑致密无明显缺陷,纤维表面为TiO2富集。
The precursors of polytitanocarbosilane (TPTC) with excess TBT were obtained by reacting polycarbosilane with titanium tetrabutoxide (TBT) in a nitrogen atmosphere at 200 ℃ for 5h. The precursor TPTC was melt-spun at 160 ℃ to prepare fibrils. The fibers were aged in air at 100 ℃ for 20h, then crosslinked at 200 ℃ for 20h and sintered at 1200 ℃. The results of IR, 13C, 29Si, XRD, SEM and energy dispersive X-ray diffraction showed that the content of Si-H bond and the number of Si-O bonds in TPTC decreased with the increase of TBT content The fibers consisted of amorphous SiO2 and anatase TiO2. The surface was smooth and dense with no obvious defects. The fiber surface was enriched with TiO2.