均匀沉淀水热法三维花球微/纳米Sm2O3的合成与表征

Synthesis and Characterization of Three-dimensional Flower Spherical Mirco/nano Sm2O3 By Homogeneous Precipitation Hydrothermal Method

摘要:

本文以六次甲基四胺(Hexamethylenetetramine, C6H12N4)和六水合硝酸钐[Sm(NO3)3·6H2O]为原料，采用均匀沉淀水热法合成Sm2O3前驱体Sm(OH)3，利用热重(TG)和X射线衍射(XRD)分析方法确定了得到微/纳米Sm2O3的适宜焙烧温度为800 °C。前驱体Sm(OH)3经800 °C焙烧后得到微/纳米Sm2O3，利用XRD和扫描电子显微镜(SEM)对产物的晶型、形貌及尺寸进行了表征。考察了反应时间、反应温度对产物形貌和尺寸的影响。结果表明：制得的微/纳米Sm2O3及其前驱体Sm(OH)3分别为立方和六方晶相结构；随着反应时间的增长，微/纳米Sm2O3的形貌由片状逐渐自组装为三维花球；随着反应温度的升高，微/纳米Sm2O3三维花球的粒径逐渐增大，组成三维花球结构的纳米片逐渐变厚且组装更加紧密。

Abstract:

The precursor Sm(OH)3 of Sm2O3 was synthesized by homogeneous precipitation hydrothermal method using hexamethylenetetramine(C6H12N4) and hydrated samarium nitrate[Sm(NO3)3·6H2O] as raw materials. The optimum calcination temperature (800 °C)was derived from thermogravimetry (TG) analysis and X-ray powder diffraction (XRD). The Sm2O3 mirco/nano particles were then prepared by calcining the precursors at 800 °C. The structures, morphologies and size of the Sm2O3 mirco/nano particles were characterized by XRD, scanning electron microscope (SEM). The influences of reaction temperature and time on the size and shape of the products were investigated. The results showed that Sm2O3 micro/nano particles and its precursor Sm(OH)3 were cubic and hexagonal crystalline, respectively. With the increase of the reaction time, mirco/nano Sm2O3 sheet structure gradually self-assembled into three-dimensional spherical flowers. The size of the Sm2O3 micro/nano particles decreased as the temperature increased, and the Sm2O3 nano-sheet structure become thicker and more closer.