以硝酸钴和二价M(M=Zn~(2+),Cu~(2+),Ni ~(2+))盐为原料,草酸盐为沉淀剂,通过水热过程获取MCo_2(C_2O_4)_3复合草酸盐中间体,对中间体在400~500℃范围内进行热处理2h,获得自组装的MCo_2O_4纳米粒子超结构材料.采用热失重(TGA)、X射线衍射(XRD)和透射电镜(TEM)分析手段,对中间体及目标产品的热稳定性、结晶度、形貌、结构进行表征.结果表明:中间体主要经历脱结晶水和草酸盐热分解两个过程,其热分解温度应高于370℃;获得的钴酸盐为纳米粒子的自组装超结构,纳米粒子颗粒细小均匀,粒度在15~30nm之间;目标产品的形貌、结晶度与样品的本性及助剂的种类存在相关性.
Using cobalt salt and M salt (M=Zn2+,Cu2+,Ni2+) as raw material and oxalate as precipitant,a series of mixed oxalate precipitates MCo2(C2O4)3 were prepared as intermediates with a hydrothermal approach.Then these intermediates were pyrolyzed at 400~500 ℃ about 2 hours and finally self-assembled nanoparticles super-structure material of MCo2O4 was achieved.A thermo-gravimetric analyzer (TGA),X-ray diffraction (XRD) device and transmission electron microscopy (TEM) were applied to characterize the heat stability,crystallization,morphology and structure of intermediates and target product.The results show that the thermo-gravimetric process of intermediates includes two stages:the loss of crystal water and the thermo-decomposition of oxalate,and the thermal-decomposition temperature should be set more than 370 ℃.The prepared products are superstructure material assembled by fine and homogeneous polyhedral particles,with the particle size of 15~30 nm.The morphology and crystallization of target product are influenced by the intrinsic properties of samples and the types of additives.