Synthesis and Characterization of Nanocrystalline CoAl2O4 Spinel Powders
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摘要: 铝酸钴(CoAl2O4) 是目前世界上最耐候、耐光、耐热、耐化学品的尖晶石型钴蓝颜料, 为了解决传统钴蓝制备方法存在的能耗高、产品粒径分布不均匀、易团聚等问题, 尝试采用柠檬酸盐凝胶法合成了尖晶石型CoAl2O4纳米粉体, 对样品进行了TG-DSC、XRD、SEM等分析, 考察了前驱体凝胶的热分解过程, 以及煅烧温度对CoAl2O4晶化程度和粒度的影响. 确定了钴蓝最佳合成条件为: n(Co2+)/n(Al3+) =1∶3, 柠檬酸与金属离子摩尔比为1∶1, pH值约为6.5, 煅烧温度为800℃.结果表明, 采用柠檬酸盐凝胶法成功合成了平均粒径为60nm, 粒度分布均匀的尖晶石型CoAl2O4纳米粉体, 该法具有合成成本低、制备工艺简单、易操作等优点.Abstract: The citrate-gel method was applied to prepare nanocrystalline CoAl2O4 spinel powders in an attempt to reduce the temperature of preparation and the calcination times. By means of thermogravimetric analysis (TG), differential scanning calorimetry (DSC) and X-ray diffraction (XRD) techniques, the phase compositions of the precursor and its calcinations at different temperatures were investigated. The spinel CoAl2O4 powders were prepared in optimum conditions: n(Co2+)/(n(Al3+)) =1∶3, citric acid to Me mole ratio of 1∶1, pH value is about 6.5, 800 ℃ heat-treatment. The citrate-gel method was shown to be a convenient method of preparing homogeneous crystalline CoAl2O4 powders with an average particle size of 60 nm and a narrow size distribution.
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Key words:
- CoAl2O4 /
- citrate-gel method /
- nanocrystalline powder
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图 2 不同热处理温度的CoAl2O4粉体的XRD衍射图
Fig. 2. XRD patterns of CoAl2O4 partical heated at different temperatures
图 3 不同温度下热处理2 h样品的SEM照片
Fig. 3. SEM photographs of the sample calcined at different temperatures
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