Study of High Purity Cobalt Carbonate Nanocrystals Production by Microemulsion as Batteries Precursors

Mulaja Tshakatumba Constantin, Tshipeshi Makina Héritier, Ngoy Moïse Raphael Moramess, Mwema Mutamba Edouard
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Abstract

The precipitation of cobalt carbonate nanocrystals was achieved through the reaction of a pure and rich solution of cobalt sulphate (Co2+: 16.80 g/l) with a solution of carbonate solution (200 g/l). A surfactant was added to the reacting mixture in order to control the shape and size of generated crystallites. Two parameters were then varied i.e., the weight of surfactant agent and the precipitation time in accordance with Taguchi’s L4 full experimental procedure (22). Chemical and structural characterizations tests of the obtained precipitates were done through X-Rays Fluorescence (XRF), Scanning Electron Microscopy (SEM) and X-Rays Diffractometer (XRD); whereas the size of crystallites was assessed according to the Laue-Scherrer formula. The results obtained from the variance analysis (ANOVA) indicated an optimal size of cobalt carbonate’s crystallites of 13 nm with a cobalt content of 44.35% (equivalent to 89.45% of CoCO3) at ambient temperature under the following conditions: pH = 7; Mixing speed: 800 tr/min; Surfactant weight: 8 g; and a mixing time: 10 minutes. SEM images revealed an agglomeration of the obtained nanocrystals due to suspected drying conditions i.e., drying temperature and drying atmosphere. It is suggested that the experiment should be conducted under neutral conditions at a temperature below that of cobalt carbonate’s decomposition (181.41℃).
微乳法制备高纯碳酸钴纳米晶电池前驱体的研究
碳酸钴纳米晶的析出是通过纯富硫酸钴溶液(Co2+: 16.80 g/l)与碳酸钴溶液(200 g/l)的反应实现的。在反应混合物中加入表面活性剂以控制生成晶体的形状和大小。然后改变两个参数,即表面活性剂的重量和沉淀时间,按照田口的L4全实验程序(22)。通过x射线荧光(XRF)、扫描电子显微镜(SEM)和x射线衍射仪(XRD)对所得沉淀物进行了化学和结构表征;而晶体的大小则根据劳-谢勒公式进行评估。方差分析(ANOVA)结果表明,在环境温度下,当钴含量为44.35%(相当于CoCO3的89.45%)时,碳酸钴晶的最佳尺寸为13 nm: pH = 7;搅拌速度:800 tr/min;表面活性剂重量:8g;混合时间:10分钟。扫描电镜图像显示,由于干燥条件,即干燥温度和干燥气氛,所获得的纳米晶体出现团聚。建议在低于碳酸钴分解温度(181.41℃)的中性条件下进行实验。
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