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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 (NH4) 3 PMo12O40.4H2O particles with Keggin structure were prepared by solid state and liquid phase methods using phosphomolybdic acid and triammonium citrate as raw materials. The composition, structure and morphology of the prepared particles were characterized by elemental analysis, FTIR, XRD, TG-DTA and SEM. The particles prepared by the solid phase method are irregular spherical with an average particle diameter of about 35 nm. The particles prepared by the liquid phase method are regular rhombic dodecahedron shapes, and the particle size is about 500 nm. The pyrolytic properties indicate that the prepared particles have good thermal stability below 400 ° C. The formation mechanism of (NH4) 3 PMo12O40.4H2O particles was discussed. It was found that citric acid, which is the product of the reaction, plays a key role in controlling the particle morphology.