电池级Co3O4的制备与表征

Preparation and Characterization of Battery Grade Co_3O_4

以CoCl2·6H2O和NH4HCO3为原料，采用沉淀焙烧法制备电池级Co2O4。对合成过程的pH值、时间、温度、加料比以及对前躯体Co2（OH）2CO3的焙烧时间和温度进行了系统的研究，得出了最佳的制备条件：以n（CoCl2·6H2O）：n（NH4HCO3）=1：2．5，在温度80℃左右反应，pH值在8～9，搅拌反应20min，生成前驱体Co2（OH）2CO3,100℃烘干，600～820℃焙烧8h左右得纯相的Co3O4粉体。用ICP-AES、XRD、SEM／EDS、FT-IR、LGA、TG／DSC等分析测试技术对Co3O4粉体进行了表征。结果表明，Co3O4的粒径在4～10μm，平均粒径为7．3μm，比表面积为1．05m^2／g，粒径分布均匀，呈多面体形、类球形颗粒，杂质元素含量低，满足了电池级Co3O4的要求。

The battery grade Co3O4 was prepared from CoCl2·6H2O and NH4 HCO3 by means of precipitation and calcination. Systemic studies were conducted on the effects of pH of the solution, reaction time and temperature, the adding ratio of raw materials during the reaction process, and the calcination period and temperature of the precursor basic cobalt carbonate. The best preparation way was thus found. The precursor basic cobalt carbonate was made from the reaction between CoCl2 · 6H2O and NH4HCO3 with the molar ratio of 1 ： 2. 5, at 80 ℃ or so and pH 8 - 9 for 20 minutes. Then, the precursor basic cobalt carbonate was washed with de-ionized water, dried by heating or air flowing at a temperature less than 100 ℃, and baked at a temperature from 600 to 820 ℃ for about 8 h. Thus, the pure Co3O4 was made. Co3O4 powder characterization was analyzed by ICP-AES, XRD, SEM/EDS, FT-IR, LGA, and TG/DSC. It was found by the characterization study that the Co3O4 powder was at particle size ranging from 4 - 10 μm, average grain size of 7.3 μm, and specific area of 1.05 m^2/g. The powder showed a narrow distribution of particle size, and was polyhedral and sphereoidal, and met the requirement of the battery grade Co3O4.