以柠檬酸(CA)为配位剂与金属离子配合,水作为溶剂,乙二醇(EG)为酯化剂,通过聚合物前驱体法制备铌酸钾(KNbO3)粉体。研究了CA和EG的用量和pH值对溶胶性能的影响。采用X-射线衍射(XRD)和热失重分析(TG-DTA)研究了KNbO3晶相的形成过程,用透射电子显微镜(TEM)对所制得粉体的表面形貌进行了分析。结果表明,当前驱体溶胶的pH值为7.5,n(CA):n(金属离子)=3:1,n(CA):n(EG)=1:2时,可获得稳定性好的溶胶。凝胶前驱体在加热过程中先反应生成K3Nb7O19和K4Nb6O17,然后二者反应生成KNbO3。凝胶前驱体以不同的升温速率加热至700℃,对所得粉体的形貌影响较大,升温速率快,有利于粒状产物的形成;升温速率慢,易形成棒状产物。同时讨论了不同的升温烧结机制影响KNbO3形貌的原因。
With citric acid as chelating agent, ethylene alcohol as etherification agent and water as solvent, KNbO3 nanopowder was synthesized by polymeric precursor method. The effects of the amount of CA and EG as wellas pH value on the stability of the precursor Sol were investigated. The evolution of KNbO3 crystal phase was also investigated by XRD and TG-DTA. The results showed that a homogeneous precursor Sol could be formed at the case of n(CA) : n(metalion)=3 : 1, n(CA) : n(EG)=1 : 2 and pH= 7. 5. During the calcinations K3Nb7O19 and K4 Nb6 O17 occurred first and then reacted into KNbO3 Sintering process largely influences the morphology of the prepared productswhen the precursor Sol was heated to 700 ℃ at different temperature rising rate. Grain-like nanoparticles could be obtained with a rapid temperature rising rate, while nanorods were obtained with a slow rate. The forming mechanism of different morphologies of the prepared nanoparticles was also discussed.