纺丝液参数对静电纺丝制备镁铝尖晶石纤维的影响  

Effect of Spinning Solution Parameters on Synthesis of Magnesium Aluminate Spinel Fibers via Electrospinning

作　　者：崔燚 魏恒勇[1,2] 王合洋 魏颖娜 林健[2] 卜景龙 王鹏 

机构地区：[1]华北理工大学材料科学与工程学院河北省无机非金属材料重点实验室,唐山063009 [2]同济大学材料科学与工程学院,上海201804

出　　处：《材料研究学报》2016年第2期115-122,共8页Chinese Journal of Materials Research

基　　金：国家自然科学基金51302064;华北理工大学青年基金Z201413资助项目~~

摘　　要：以无水氯化镁和无水氯化铝为原料,聚乙烯吡咯烷酮(PVP)为助纺剂,无水乙醇和N,N-二甲基甲酰胺(DMF)为溶剂,采用非水解溶胶-凝胶法制备纺丝前驱体溶液,利用静电纺丝技术获得镁铝尖晶石凝胶/PVP前驱体纤维,经900℃煅烧合成出镁铝尖晶石纤维。借助XRD,FTIR,SEM和TEM研究了凝胶化温度、凝胶用量和PVP用量等纺丝液参数对镁铝尖晶石纤维相组成及结构的影响。结果表明,直接添加混合溶液时,虽能合成出物相为镁铝尖晶石的纤维,但纤维交联严重,还出现了较多念珠状颗粒;当凝胶化温度为120℃时,纤维则出现了明显的断裂;纤维直径随凝胶用量和PVP用量的增加而增大。当凝胶化温度为100℃、凝胶用量为0.068 mol/L、PVP用量为0.045 g/m L时,纤维为镁铝尖晶石相,表面光滑、连续,直径均匀且细小,平均直径为121 nm,经1600℃煅烧后仍保持良好的纤维形貌。A solution for electro-spinning of fibers was prepared via non-hydrolytic sol-gel method with ethanol and dimethyl formamide（DMF） as solvent, Mg Cl2 and Al Cl3 as raw material and polyvinylpyrrolidone（PVP） as additive. With the above solution, precursor fibers of magnesia- alumina spinel were prepared by electrospinning technology, which then were calcined at 900℃ to finally produce fibers of magnesia- alumina spinel. The effect of gelation temperature, the content of gel and PVP on the phase composition and microstructure of magnesia-alumina spinel fibers was studied by XRD, FTIR, SEM and TEM. The result shows that magnesia- alumina spinel fibers could be produced with the fiber precursor prepared with the fresh solution which was not subjected to sol-gel treatment, but such fibers were crosslinked seriously and on which there existed significant amount of moniliform particles; For those made of the fiber precursor prepared with the solution after gelation at 120℃, such fibers were apt to fracture and the diameter of which increased with the increasing dosage of gel and PVP; For those made of the fiber precursor prepared with the solution after gelation at 100℃ with a dosage of 0.068 mol/L gel and 0.045 g/mL PVP, the fibers were smooth, continuous and homogeneous with an average diameter 121 nm, and furthermore, these fibers still showed good a morphology even after calcined at 1600℃.

关 键 词：无机非金属材料 静电纺丝 镁铝尖晶石 纤维 非水解溶胶-凝胶 

分 类 号：TQ343.41[化学工程—化纤工业]