硅酸盐学报

采用溶胶凝胶与低温自蔓延燃烧相结合的方法合成了纳米级超细Sm0.15Gd0.05Ce0.8O1.9粉体,选用的合成体系有:柠檬酸硝酸盐,甘氨酸硝酸盐,EDTA络合硝酸盐等方法。对所合成粉体进行了XRD,TEM及激光Raman光谱仪(laserRamanspectroscope,LRS)检测,研究了不同方法制备的粉体的结构及晶相。结果表明:XRD和LRS相结合能较好地表征固溶体的结构和纯度,几种方法合成的粉体为纯度高的掺杂氧化铈固溶体,晶粒尺寸较均匀,但分散性差。影响最终合成的超细粉体粒径的因素有:有机络合剂的种类、性质,有机络合剂与总金属阳离子比例及形成掺杂固溶体所需的温度。

Nano-scale Sm_0.15Gd_0.05Ce_0.8O_1.9 solid solution powder was synthesized by the combination of sol gel process and low temperature self-propagating combustion method. The processes used in the test include citric acid-nitrate, glycine-nitrate and ethylenediaminetetraacetic acid (EDTA) chelation-nitrate processes. The phase identification and morphology of the synthesized powder were measured by X-ray diffraction (XRD), transmission electron microscope (TEM) and laser Raman spectroscope (LRS), respectively. A combined analysis of XRD and LRS can give the precise information on the structure and phase purity of Sm_0.15Gd_0.05Ce_0.8O_1.9 solid solution powder. The samples synthesized by these methods are ceria doped solid solution powder with high purity, which have good crystal shape and homogeneous grain size but bad dispersion.The results show that the affecting factors on the average size of the synthesized ultrafine powder are the types and characterization of organic chelates, the ratio of organic chelates and total cation ions and the temperature for the formation of the solid solutions.