(Y, Gd)2O3∶Eu3+纳米粒子制备过程中的合成动力学

金属学报, 2012, 48(6): 671-677. doi: 10.3724/SP.J.1037.2011.00735

(Y, Gd)₂O₃∶Eu³⁺纳米粒子制备过程中的合成动力学

1.1. 沈阳化工大学材料科学与工程学院~辽宁省稀土化学及应用重点实验室, 沈阳 1101422. 中国科学院金属研究所沈阳材料科学国家(联合)实验室, 沈阳 1100163. 东北大学材料与冶金学院, 沈阳 110819>

1.1. Key Laboratory for Rare-earth Chemical and Applying of Liaoning Province, School of Material Science and Engineering, Shenyang University of Chemical Technology, Shenyang 1101422. Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences,Shenyang 110016 3. Institute of Metallurgy and Materials, Northeastern University, Shenyang 110819>

基金项目: 辽宁省自然科学基金项目20062001和沈阳市科技攻关计划项目F10-053-2-00资助

关键词： (Y, Gd)₂O₃∶Eu³⁺纳米粒子 , synthesis kinetics , activation energy , micro-morphology

SYNTHESIS KINETICS OF (Y, Gd)₂O₃∶Eu³⁺ NANO-POWDERS DURING PROCESS OF PREPARATION

ZHU Hongyan , MA Weimin , WEN Lei , GUAN Renguo , MA Lei , WU Nan

Keywords： (Y, Gd)₂O₃∶Eu³⁺ nano-particle , 合成动力学 , 活化能 , 微观形貌

采用反向滴定共沉淀法制备出(Y, Gd)₂O₃∶Eu³⁺前躯体, 再在不同温度下煅烧, 获得(Y, Gd)₂O₃∶Eu³⁺纳米粒子, 用XRD和SEM对样品物相组成及形貌进行了表征; 用TG--DTA获得了样品在不同升温速率下的热分解曲线. 结果表明, 前躯体在煅烧过程中的物相变化分为3个阶段, 用Doyle-Ozawa法和Kissinger法分别计算出各个反应阶段的表观活化能, 其平均值分别为191.54, 557.05和236.58 kJ·mol^-1, 并建立了动力学方程; (Y, Gd)₂O₃∶Eu³⁺晶粒生长活化能是35.58 kJ·mol^-1, 纳米粒子形核过程中的晶粒长大由晶界扩散控制.

Using NH₃·H₂·O and NH₄HCO₃ blended solution as a complex precipitation agent, (Y, Gd)₂O₃∶Eu³⁺ nano--particles were synthesized by co--precipitation reaction. XRD and SEM were applied to analyze the crystallization and morphology of the sample. The thermal decomposition curves of samples were analysed by TG-DTA at different heating rates. Results showed that under the conditions of pH=10 and reverse titration, the change process of (Y, Gd)₂O₃∶Eu³⁺precursors is divided into three steps. The apparent activation energy of each step was calculated by using the Doyle--Ozawa and Kissinger methods. The calculated results are 191.54, 557.05 and 236.58 kJ·mol^-1. The dynamic equations have been also established. The activation energy of (Y, Gd)₂O₃∶Eu³⁺grain growth is 35.58 kJ·mol^-1, indicating that grain growing is primarily controlled by interfacial reaction during process of preparation.

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