水热-热分解法合成系列MCo_2O_4自组装纳米材料  

Hydrothermal and Thermo-Decomposition Synthesis of Self-assembled MCo_2O_4 Nanomaterial

作　　者：马杰[1] 季婷婷[1] 贾奎法 侯炎炎 

机构地区：[1]上海理工大学理学院,上海200093

出　　处：《上海理工大学学报》2015年第6期520-526,共7页Journal of University of Shanghai For Science and Technology

基　　金：上海市自然科学基金资助项目(15ZR1428500)

摘　　要：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 =Zn^2＋,Cu^2＋,Ni ^2＋）as raw material and oxalate as precipitant,a series of mixed oxalate precipitates MCo_2（C_2O_4）_3 were prepared as intermediates with a hydrothermal approach.Then these intermediates were pyrolyzed at 400~500°C about 2 hours and finally self-assembled nanoparticles super-structure material of MCo_2O_4 was achieved.A thermogravimetric 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 than370 ℃.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.

关 键 词：钴酸盐 水热 热分解 自组装 纳米粒子 

分 类 号：O611.4[理学—无机化学]