LaPO_4纳米晶的超声固相化学反应合成与表征  

Solid-state chemical reaction synthesis and characterization of nanocrystalline LaPO_4 under ultrasonication

作　　者：李道华[1] 付佳颖[1] 李志能[1] 

机构地区：[1]内江师范学院化学化工学院,四川内江641112

出　　处：《西南民族大学学报（自然科学版）》2012年第5期792-796,共5页Journal of Southwest Minzu University(Natural Science Edition)

基　　金：四川省教育厅自然科学重点资助项目;四川省应用基础研究计划资助项目(No.07JY029-007)

摘　　要：在超声波作用下,通过低热固相化学反应合成了LaPO4纳米晶,用粉末X射线衍射(XRD)及电子衍射法(ED)分析了固相产物的物相,用透射电镜(TEM)观测粒子的大小、形貌、粒径及粒径分布.结果表明,产物为颗粒大小均匀、平均粒径约为30 nm的纳米晶,产率为92.6%.改变反应物、反应物配比、掺入惰性物质、加入微量溶剂或表面活性剂、研磨不同的时间等固相反应条件对合成LaPO4纳米晶的晶粒形貌、粒度和粒径分布有一定影响.用该方法合成纳米晶体,具有操作方便、合成工艺简单、产率高、选择性高、粒径均匀、且粒度可控、污染少,同时又可以避免或减少液相中易出现的硬团聚现象以及中间步骤和高温反应引起的粒子团聚现象等突出优点.Under ultrasonication, a LaPO4 nanometer crystal is synthesized through the solid -state chemical reaction. The solid phase is characterized by powder X-ray diffraction （XRD） and electron diffraction （ED）. The particle size, its distribution, and morphology of the prepared nanocrystallite are observed by transmission electron microscopy （TEM）. The results show that particle sizes are relatively uniform, the morphology of the crystal is spherical, the average particle diameter is about 30 nm, and the yield rate is approximately 92.6%. Furthermore, during the synthesis, the solid-state reaction conditions including raw materials, matching proportion of reactants, additions of inert substance, addition of trace solvents, surfactants and porphyrization time, etc, all have some influence on the morphology, particle size and size distribution of the final products. During the synthesis of the lanthanum oxalate nanocrystallines, the solid state reaction conditions such as changing reactant, matching proportion of reactant, adding inert substance, joining a little solvent or surface active solvent and grinding at different times may influence morphology, particle size and the size distribution of final products. The solid-state chemical reaction method can meet these needs and it is easy to operate with advantages of simple process such as synthesis, high yield, high selectivity, uniform particle size distribution, controllable size and less pollution. It can prevent or reduce the phenomenon of agglomeration of the liquid phase and the phenomenon of particle agglomeration caused by intermediate step and high-temperature reaction.

关 键 词：磷酸镧纳米晶 超声波 固相化学合成 结构表征 

分 类 号：O614[理学—无机化学] TQ13[理学—化学]