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采用燃烧合成–二次还原焙烧法制备CaB6多晶粉末,考察了二次还原焙烧温度和时间对焙烧效果的影响,采用X射线衍射、扫描电子显微镜、透射电子显微镜和激光粒度分析仪对CaB6多晶粉末进行表征。结果表明:Ca3B2O6副产物经二次还原焙烧后转化为CaB6,有利于提高CaB6的产率。随二次还原焙烧温度提高和时间延长,CaB6晶粒逐渐发育完善并长大;焙烧温度过高,产物中Mg3B2O6副产物进一步增多,降低了焙烧效果。合适的还原焙烧条件为:焙烧温度800℃;焙烧时间3～4 h。还原焙烧后得到的CaB6为多晶粉末,纯度大于95.3%。
CaB6 polycrystalline powder was prepared by combustion synthesis - secondary reduction roasting method. The effects of secondary reduction roasting temperature and time on calcination effect were investigated. XRD, SEM, TEM and laser particle size analyzer Crystal powder characterization. The results showed that the by - product of Ca3B2O6 was converted to CaB6 by secondary reduction roasting, which was beneficial to increase the yield of CaB6. With the increase of secondary reduction calcination temperature and the prolongation of time, CaB6 grains gradually developed and grew up. When the calcination temperature was too high, the byproduct of Mg3B2O6 in the product further increased, reducing the calcination effect. The appropriate reduction roasting conditions: roasting temperature 800 ℃; roasting time 3 ~ 4 h. CaB6 obtained after reduction roasting is a polycrystalline powder with a purity of more than 95.3%.