水热-热分解法制备棒状和多面体状四氧化三钴
来源期刊：中南大学学报(自然科学版)2006年第6期
论文作者：杨幼平 黄可龙 刘人生 王丽平 刘素琴 张平民
文章页码：1103 - 1106
关键词：水热法;热分解;四氧化三钴;草酸钴
Key words：hydrothermal method; thermal decomposition; Co3O4; CoC2O4
摘 要：以Co(CH3COO)2·4H2O和H2C2O4·2H2O为原料,聚乙二醇(相对分子质量为20 000)为表面活性剂,在水-正丁醇溶剂体系中及水热条件下制备草酸钴前驱体;采用不同的热分解方法对草酸钴前驱体进行处理制备纯物相的棒状和多面体状四氧化三钴;并用热重-差热分析、红外光谱、X射线衍射和透射电镜对草酸钴前驱体和四氧化三钴产物的结构和形貌进行表征。研究结果表明:对草酸钴前驱体采用不同的热分解方法得到的四氧化三钴的形貌不同,将前驱体于400℃煅烧3 h得到直径约为0.1μm,长度可达1μm的纯物相棒状四氧化三钴;而采用二段热分解方法即将前驱体于350℃煅烧1 h,然后于750℃煅烧2 h时,得到多面体状四氧化三钴。
Abstract: The cobalt oxalate precursor was prepared by hydrothermal method using cobalt acetate and oxalic acid as raw materials, and polyethylene glycol with relative molecular mass of 20 000 as surfactant in water andn-butanol solvent system. The rod-like and polyhedron-like Co3O4 powders were obtained when the precursor was calcined by different thermal decomposition methods.The structure and morphology of cobalt oxalate precursor and Co3O4 product were characterized by thermogravimetry-differential thermal analysis, infrared spectrum, X-ray diffraction and transmission electron microscope. The results show that the morphologies of Co3O4 are changed with the precursor obtained by different thermal decomposition methods. The rod-like Co3O4 with about 0.1μm in diameter and 1μm in length can be obtained when the precursor is calcined at 400℃for 3 h, while the polyhedron-like Co3O4 can be obtained when the precursor is calcined at 350℃for 1 h and then at 750℃for 2 h.
