两段焙烧法制备六硼化镧工艺研究  

Study on Two-stage Roasting Process for Synthesis of Lanthanum Hexaboride

作　　者：石志霞[1] 余章龙[2] 孙静[1] 彭程[1] 段华英[1] 张碧田[1] 王星明[1] 储茂友[1] 

机构地区：[1]北京有色金属研究总院稀有金属与冶金材料研究所,北京100088 [2]北京有色金属研究总院动力电池研究中心,北京100088

出　　处：《材料导报》2015年第6期88-92,共5页Materials Reports

基　　金：国家自然科学基金面上项目(51171029)

摘　　要：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.

关 键 词：两段焙烧工艺 氧化硼 氧化镧 六硼化镧 

分 类 号：TQ133.3[化学工程—无机化工]