草酸盐沉淀法制备亚微米级SC2O3粉体的研究  

Preparation of Submicron Sc2O3 Powder through Oxalate Precipitation

作　　者：付国燕 王玮玮[1] 吕东[1] 刘诚[1] FU Guoyan;WANG Weiwei;LVDong;LIU Cheng(China ENFI Engineering Technology Co.,Ltd,Beijing 100038,China)

机构地区：[1]中国恩菲工程技术有限公司,北京100038

出　　处：《陶瓷学报》2020年第4期508-514,共7页Journal of Ceramics

基　　金：国家重点研发计划(2019YFC1907402)。

摘　　要：采用草酸沉淀法制备了Sc2O3亚微米粉体材料。研究了反应温度、沉淀剂用量、反应pH值等实验因素对钪沉淀回收率的影响,并利用XRD、SEM-EDS、激光粒度分析仪、傅里叶红外光谱仪(FTIR)、比表面积仪等对氧化钪粉体材料性质进行表征。研究结果表明,反应温度为80℃、草酸与氯化钪的摩尔比为1.5及反应体系的p H值为1.3时,钪沉淀回收率可达97%以上。结合TG-DTA结果及氧化钪粉体材料的FTIR和XRD结果可知,草酸钪前驱体在1100℃条件下焙烧获得氧化钪较纯净。氧化钪粒度细小均匀,体积中心径D50为7.586μm,90%的颗粒粒径小于16.050μm,基本上呈正态分布;比表面积为17.819 m2/g,具有良好的晶型结构;微观结构为形状完整的亚微米结构层状物,结合BET测试结果可得出,其表面含有一定的孔洞二级结构。Submicron Sc2 O3 powder was prepared by using oxalic acid precipitation. The effects of reaction temperature, precipitation dosage and p H value on the recovery rate of scandium precipitation were studied. Meanwhile, the Sc2 O3 powder was characterized by using XRD, SEM-EDS, laser particle size analyzer, Fourier infrared spectrometer(FTIR) and BET surface area measurement. It is showed that the recovery rate of scandium precipitation could be up to 97%, when the reaction temperature was 80 ℃, the molar ratio of oxalic acid to scandium chloride was 1.5 and the p H value was 1.3. According to the TG-DTA, FTIR and XRD results, it is demonstrated that the Sc2 O3 was relative pure after the oxalate precursor was calcined at 1100 ℃, with pretty high crystallinity. The Sc2 O3 powder has fine and uniform particles. Volume center diameter(D50) of the powder was 7.586 μm, while 90% of the particles have a size of less than 16.050 μm, with a normal size distribution profile. The powder exhibits a specific surface area of 17.819 m2/g, while it has a submicron layered structure, with surface containing certain secondary pores.

关 键 词：沉淀法 氧化钪 草酸 粉体材料 

分 类 号：TQ174.75[化学工程—陶瓷工业]