摘要
以磷钼酸和柠檬酸三铵为原料,分别采用固相法和液相法,制备了Keggin结构的(NH4)3PMo12O40.4H2O粒子。采用元素分析、FTIR、XRD、TG-DTA和SEM对制备的粒子的组成、结构和形貌进行了表征。固相法制备的粒子为不规则球形,平均粒径35nm左右;液相法制备的粒子为规则的菱形十二面体形状,粒子大小约500nm左右。热解性质表明,制备的粒子在400℃以下具有良好的热稳定性。对(NH4)3PMo12O40.4H2O粒子的形成机理进行了探讨,发现反应过程中的生成物柠檬酸对粒子的形貌控制起到关键作用。
The particles of (NH4)3 PMo12O40·4H2O with Keggin structure were synthesized using H3 PMo12O40·nH2O and (NH4)3C6H5O7 as the starting materials by solid-state and solution reactions. The as-prepared particles were characterized by elemental analysis, FTIR, XRD, TG-DTA and SEM. The particles prepared by solid-state reaction were irregular spherical shape, and the mean grain size was 35 nm. The morphology of the particles prepared by solution reaction was regular rhombic dodecahedral, and the mean grain size was 500 nm. Both of them showed good thermal stability up to 400℃. The formation mechanisms of the particles had been discussed, and the results indicated that the citric acid produced in the reaction process plays a key role for controlling of the particle morphology.
出处
《化学通报》
CAS
CSCD
北大核心
2008年第11期868-872,共5页
Chemistry
基金
江苏省高校自然科学基础研究项目(07KJD150050)资助
关键词
多金属氧酸盐
KEGGIN结构
机理
固相合成
粒子
Polyoxometalates, Keggin structure, Mechanism, Solid-state synthesis, Particles