先驱体转化法原位制备TiO2膜层SiO2纤维  

PREPARATION IN SITU OF TiO_2 SURFACE LAYERS ON SiO_2 FIBERS BY PRECURSOR CONVERSION METHOD

作　　者：郭亚涤[1] 余煜玺[1] 程璇[1] 张颖[1] 

机构地区：[1]厦门大学材料学院,福建省特种先进材料重点实验室,福建厦门361005

出　　处：《硅酸盐学报》2009年第11期1873-1879,共7页Journal of The Chinese Ceramic Society

基　　金：福建省科技平台建设(2006L2003,2007H2004)资助项目

摘　　要：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。A precursor contained polytitanocarbosilane（TPTC） and an excess amount of titanium tetrabutoxide（TBT） was synthesized through the mild reaction of polycarbosilane with TBT at 200 ℃ for 5 h in nitrogen atmosphere.The polymer precursor was melt-spun at 160 ℃.The spun fiber was pre-heat-treated at 100 ℃ for 20 h,then cured at 200 ℃ for 20 h and subsequently fired up to 1 200 ℃ in air to obtain a TiO2/SiO2 fiber.The TPTC was characterized by Fourier transform infrared spectroscopy,nuclear magnetic resonance（^13C,^29Si）,X-ray diffraction,scanning electron microscopy and energy dispersive X-ray detection.The results show that：with the increase of TBT content,the amount of Si-H bonds in TPTC decreases while the content of Si-O bonds increases.The fiber is composed of anatase-TiO2 and amorphous silica,and has a smooth surface.The TiO2-SiO2 fiber has a TiO2/rich surface structure.

关 键 词：纤维 聚碳硅烷 二氧化钛 二氧化硅 

分 类 号：TB34[一般工业技术—材料科学与工程]