Preparation and characterization of Co3O4 by wet precipitation-thermal decomposition with oxalate
LI Hui-ying1，WANG Wen-xiang1，LIU Ying1，YAN Ying-yan1，LIU Zhi-hong2
（1. Department of Heavy Metal Pollution Control and Comprehensive Utilization of Resources Key Laboratory，Guangdong Polytechnic of Environmental Protection Engineering，Foshan 528216，China 2. School of Metallurgy and Environment，Central South University，Changsha 410083，China）
Abstract：The cobalt oxide precursor was prepared by wet precipitation method with cobalt chloride as cobalt source，ammonium oxalate as precipitating agent，and Tween-80 as surfactant. The Co3O4 powder was obtained by thermal decomposition method. The morphology，crystal structure and thermal decomposition of precursor particles and Co3O4 powder were characterized by scanning electron microscope，X-ray diffractometer and thermal analyzer. Results show that the precursor of cobalt oxide prepared with oxalate as precipitant is CoC2O4·2H2O. Relatively pure Co3O4 powder can be obtained when the precursor is calcined at 600 ℃ for 4 h. The Co3O4 powder basically maintains the original shape of precursor，which are still needle (rod) shape and the edge of the particles become smooth.
[1] Wang G X, Chen Y, Konstantinov K, et al. Investigation of cobalt oxides as anode materials for Li-ion batteries[J]. Journal of Power Sources, 2002, 109: 142 147.[2] LI Wei-yang, XU Li-na, CHEN Jun. Co3O4 nanomaterials in lithium-ion batteries and gassensors[J]. Advanced Functional Materials, 2005, 15(5): 851-857.[3] WANG Chen-bin, TANG Chih-wei, GAU Shiue-jiun, et al. Effect of the surface area of cobaltic oxide on carbon monoxide oxidation[J]. Catalysis Letters, 2005, 101(1/2): 59 63. [4] Ichiyanagi Y, Kimishima Y, Yamada S. Magnetic study on Co3O4 nanoparticles[J]. Journal of Magnetism and Magnetic Materials, 2004, 272-276.[5] Liang S. Q., Liao L.W., Yin G.Q., et al. Optimization of preparing Co3O4 nanoparticles by homogeneous precipitation[J]. Inorg Chem Ind, 2006, 38(7): 21-24. [6] Guo X.Y. , Guo Q. S. Preparation of fine powder material with solution spray-oxidation [J].China Nonferrous Metall, 2010, 39( 4) : 54.[7] 刘宇慧, 汪礼敏, 张景怀. 液相沉淀法制备超细Co3O4粉体的研究[J] . 粉末冶金工业 2007, 17( 4):14-18.[8] ZengWW, HuangKL, YangYP, et al., Solvothermal synthesis and capacitance eperformance of Co3O4 with different morphologies[J]. Chin Acta Phys Chim Sin，2008，24( 2) : 263.[9] 相钰, 冯静, 刘晓寒等. 草酸沉淀法合成自组装纳米Co3O4及性质[J]. 无机化学学报 2010, 26( 3):525-528.[10] T.Ishikawa,E.Matijevic. Formation of uniform particles of cobalt compounds and cobalt ,Colloid Polym Sci[J]. 1991:179-186.[11] 何焕华．中国镍钴冶金[M]．北京: 冶金工业出版社, 2009, 321-323.[12] T. He, D.R. Chen, X.L. Jiao, et al. Co3O4 nanoboxes: surfactant-templated fabrication and microstructure characterization[J].Adv. Mater. 2006, 18: 1078-1082. [13] C.C. Li, X.M Yin, T.H. Wang, et al. Morphogenesis of highly uniform CoCO3 submicrometer crystals and their conversion to mesoporous Co3O4 for gas-sensing applications[J]. Chem. Mater. 2009, 21(20): 4984-4992.[14] St.G. Christoskova,et.al. Preparation and characterization of a higher cobalt oxide[J]. Materials Chemistry and Physics, 1999,60:39-43.[15] A.Malecki and J.P.Doumwec, Kinetics of Thermal Decomposition of Co3O4-Powder and Singles—The kinetic model[J]. Journal of Thermal Analysis,1990,36:215-222.[16] 蔡正千. 热分析[M]. 北京：高等教育出版社, 1993.[17] 陈镜泓. 热分析及其应用[M]. 北京：科学出版社, 1985.[18] 廖春发, 梁勇, 陈辉煌. 由草酸钴热分解制Co3O4及其物性表征[J]. 中国有色金属学报, 2004, 14(12):2131-2136.[19] 王玉棉, 李存增, 侯新刚. 表面活性剂在超细钴粉制备中的应用[J]. 兰州理工大学学报, 2006, 32(6):9-11.[20] 杨幼平, 刘人生, 黄可龙, 张平民. 碱式碳酸钴热分解制备四氧化三钴及其表征[J]. 中南大学学报(自然科学版), 2008,39(1):108-110.
2017, Vol. 27 
