研究了熔盐电解法制备CaB6的合成工艺, 确定了制备CaB6粉末的合成温 度、电解电压和电解时间. 同时, 对电解所生成的阴极产物的相组成、颗粒尺寸与 形貌进行了表征. 结果表明, CaCl2熔盐体系制备CaB6粉末的基本工艺条 件是: Ar气环境保护, 电解电压3.0 V, 900℃电解30 h. 所合成的CaB6晶体粉 末粒径范围为2-8μm, 颗粒形态规整, 为规则的长方体. 对电解过程中阴极进 行循环伏安扫描分析, 确定硼酸盐向阴极的扩散速率为控制电解过程 的重要环节.
The research is about synthesis process of CaB6 powder by molten salt electrolysis method. The synthesis temperature, electrolysis voltage, electrolysis time is identified. At the same time, under the conditions of different electrolysis time,the phase composition, particle size and shape of cathode products is analysised by X-ray diffraction and scanning electron microscope , experimental results show that synthesis process of CaB6 powder in CaCl2 molten salt system must have the basic conditions: protectiving environment of argon, electrolysis voltage is 3.0V, 900℃ insulation 30h, the range of CaB6 crystal particles size was 2μm～10μm, the morphology of particle is regular with rule cuboid massive crystal. The cathode electrolysis process conducted cyclic voltammetry scan analysis, a preliminary dynamic analysis and calculation to determine that chlorine borate proliferating to the cathode is control step of reaction.
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