研究了以氧化镧(La2O3)、氧化硼(B2O3)和石墨(C)为原料采用两段焙烧工艺制备六硼化镧(LaB6)粉末的工艺路线。首先采用TG-DTA测试确定了La2O3、B2O3、C原料在室温至1100℃下的反应情况,随后采用X射线衍射分析了低温段(1100~1500℃)和高温段(1500~1700℃)的反应温度和保温时间对产品相组成的影响,从而确定两段焙烧法制备LaB6的工艺流程及参数,最后采用扫描电镜和ICP-MS分析方法分析了产品LaB6粉末的颗粒尺寸、形貌及纯度。实验结果表明,采用La2O3-B2O3-C体系制备LaB6,在1300℃保温4h,将原料B2O3中的B元素转化进入中间体,随后在1700℃高温反应4h可得到紫红色LaB6粉末,测试结果显示LaB6的含量大于99.9%,其中La和B的原子比为1∶6,粒径约为2μm。
A two-stage roasting process for producing lanthanum hexaboride(LaB6)powders using lanthanum oxide(La2O3),boric oxide(B2O3)and graphite(C)as raw materials was proposed.The reaction process of La2O3-B2O3-C system was analyzed by TG-DTA at the range of room temperature to 1100℃.And then,the effects of reaction temperature and holding time on phase composition,morphology,particle size and impurity content were characterized by X-ray diffraction(XRD),scanning electron microscope(SEM)and inductively coupled plasma mass spectroscopy(ICP-MS).The results showed B element in B2O3 was turned into the intermediates totally at 1300 ℃ with the holding time of 4h.Subsequently,after these intermediates were roasted at 1700 ℃ for 4h,a final purple-red product with 99.9% purity,2μm particle size and 1∶6La and B stoichiometric ratio could be obtained.