硼酸镁微波水热合成、表征及发光性能  

Microwave hydrothermal synthesis,characterization and photoluminescence properties of magnesium borate

作　　者：胡应喜[1] 文帅[1] 郭瑞 李馨 罗静 刘霞[1] 

机构地区：[1]北京石油化工学院化学工程学院,北京102617

出　　处：《无机盐工业》2017年第12期16-19,共4页Inorganic Chemicals Industry

基　　金：国家级大学生创新创业训练计划资助(No.2015J00089)

摘　　要：以六水合硝酸镁、硼砂、氨水为原料,在微波水热条件下制备硼酸镁基质,经X射线衍射(XRD)、热重-差热分析(TG-DTA)、红外光谱分析(IR)及扫描电镜(SEM)分析表明硼酸镁基质的组成为7MgO·2B_2O_3·7H_2O,形貌为纳米薄片团簇而成的球状花。通过稀土铽(Tb^(3+))掺杂,先微波水热合成硼酸镁荧光粉前躯体7MgO·2B_2O_3·7H_2O:Tb3+,再经焙烧得硼酸镁荧光粉3MgO·B_2O_3:Tb^(3+)。实验表明,前驱体中Tb3+适宜掺杂量为1%(硝酸铽加入量为硝酸镁物质的量的1%),较佳的焙烧温度为650℃;在波长为246 nm激发光下,荧光粉以541 nm绿光发射为主,对应5D4—7F5特征跃迁。当Tb3+掺杂量增大时,由于发生浓度淬灭效应而使荧光粉发光减弱。Magnesium borate（7MgO·2B2O3·7H2O）,spherical flower-like morphologies,composed from nano-flake self-assemblies,was successfully prepared by microwave hydrothermal method with magnesium nitrate hexahydrate,borax and ammonia as reactants.The structure,properties and morphology were systematically characterized by XRD,TG-DTA,IR and SEM.Magnesium borate luminescent precursors（7MgO·2B2O3·7H2 O：Tb3＋） were synthesized by doping Tb3＋into the matrix material.After calcination,magnesium borate phosphor（3MgO·B2O3：Tb3＋） was obtained.Results of fluorescence spectra indicated that there was a strong green emission at 541 nm corresponding to the characteristic5 D4-7 F5 of Tb3＋ transition under excitation at 246 nm.The optimum doping concentration was 1%,and the optimum temperature was 650 ℃.The high concentration of doped Tb3 ＋ions could cause the luminescence intensity decrease,which may be ascribed to the concentration quenching effect.

关 键 词：水合硼酸镁 微波水热合成 荧光粉 发光性能 

分 类 号：TQ128.54[化学工程—无机化工]