络合法制备不同形貌的铈锆固溶体及其性能研究  

Preparation and Properties of Ceria-Zirconia Solid Solution with Different Morphology by Complexometry

作　　者：赵臣[1] 税安泽[1] 李美澄 刘时剑 姚建城 陈秋群 黄诗耀 

机构地区：[1]华南理工大学材料科学与工程学院,广州510641

出　　处：《人工晶体学报》2014年第11期2840-2845,共6页Journal of Synthetic Crystals

基　　金：广东省省部产学研项目(2012B091100451);广东省重大科技专项(2010A080405004);禅城区产学研专项(2012B1023)

摘　　要：采用不同的络合剂(草酸、谷氨酸、苹果酸和酒石酸),通过络合法制备出玫瑰花状、块状、多孔网状的Ce0.77Zr0.23O2铈锆固溶体,利用热分析(TG-DSC)、X射线衍射分析(XRD)、扫描电镜(SEM)、比表面积和氢气程序升温还原分析(H2-TPR)等对前驱体及固溶体进行了测试表征。前驱体在450℃下煅烧2 h即可得到铈锆固溶体,700℃以后会发生晶粒长大的现象。其中以草酸为络合剂制备的玫瑰花状铈锆固溶体随着煅烧温度的升高,平均晶粒尺寸迅速增大,并发生分相,热稳定性较差;以酒石酸为络合剂制备的米粒状铈锆固溶体比表面积高达53.89 m2/g,900℃下煅烧2 h,平均晶粒尺寸依然小于20 nm,具有优良的储氧性能。Rose,plate,porous network like of Ce0. 77Zr0. 23O2 solid solution powders were prepared by the complexed-precipitation method using different complexing agents（ oxalic acid,glutamic acid,malic acid and tartaric acid）. The precursor and solid solutions were characterized by thermal analysis（ TG-DSC）,X-ray diffraction analysis（ XRD）,scanning electron microscope（ SEM）,specific surface area test and H2-temperature programmed reduction（ H2-TPR） etc. The cerium zirconium solid solution powders can be obtained by calcining the precursor at 450 ℃ for 2 h,and the grain growth occurred quickly exceeding700 ℃. For the rose like of Ce0. 77Zr0. 23O2 solid solution powders prepared with the oxalic acid,the average grain size increased rapidly,with enhancing calcination temperature,and the phase segregation happened,the thermal stability became bad. For rice grain like of Ce0. 77Zr0. 23O2 solid solution powders prepared with tartaric acid,the specific surface area achieved 53. 89 m2/ g,and the average grain size was smaller than 20 nm even at the calcination temperature 900 ℃ for 2 h,the oxygen storage capacity was excellent.

关 键 词：铈锆固溶体 络合反应 热稳定性 

分 类 号：TM26[一般工业技术—材料科学与工程]