研究采用CaCl2-NaCl混合熔盐电解制备CaB6晶体粉末的合成工艺,确定了电解反应的温度、电解电压、电解时间,对电流效率做了初步估算.同时,对电解生成的终产物的相组成、晶粒尺寸与形貌进行了X射线衍射、扫描电镜及能谱分析.实验结果表明,混合熔盐体系制备CaB6粉末的基本工艺条件是:氩气保护,电解槽电压2.8V,温度800℃下电解18h,所合成的CaB6粉末粒径范围为1~10μm,晶粒为规则的长方体.采用循环伏安法对电解阴极过程进行了定性分析.
Synthesis process of CaB6 crystal powder by molten salt electrolysis method is studied. The synthesis temperature, cell voltage are identified, current efficiency is estimated. The phase composition, particle size and shape of cathode products were analyzed by means of X-ray diffraction and scanning electron microscope. The basic electrolytic conditions is-electrolystic cell voltage:2.8 V,at 800 ℃ ,for 18 h.The size of CaB6 crystal particles is in the range of 1 - 10μm, the shape of crystal particle is regular cuboid. The cathodic electrode process is conducted of cyclic vohammetry analysis to determine the control step of reaction.