以SbCl3为试剂,通过醇盐水解,制备了单分散的纳米Sb4O5Cl2粒子,通过正交实验,系统地研究了各个因素和水平对制备单分散纳米Sb4O5Cl2的影响。用TEM观察了表面活性剂的种类对Sb4O5Cl2粒子形貌和粒径的影响,同时以云母作底材,研究了纳米Sb4O5Cl2在其表面上的分散性能。结果表明,制备单分散纳米Sb4O5Cl2的最佳制备条件为:反应温度45℃、水解20min、SbCl3浓度0.08g/mL、搅拌速度350d/min、加水40mL、醇化2.5h和异丙醇做醇解试剂。同时发现表面活性剂对Sb4O5Cl2形貌和粒度均有较大影响,而云母在MnCl2溶液内浸泡15min时静电引力达到最大,使得纳米Sb4O5Cl2在其表面上的吸附量达到最大值,并呈较好的单分散状态。
Monodispersed nano-Sb4O5Cl2 was prepared from SbCl3 as raw material via alkoxide hydrolysis. Various factors and levels in the preparation of monodispersed Sb4O5Cl2 nanoparticles were studied with orthogonal test. The effects of the type of surfactants as dispersant on the size and morphology were also studied with TEM. Meantime, the adsorption of Sb4O5Cl2 on the surface of mica was also studied. The results showed that the optimum conditions of preparing monodispersed Sb4O5Cl2 nanoparticles were reaction temperature 45℃, hydrolysis time 20 min, concentration of SbCl3 0.08 g/mL, stirring speed 350 r/min, water added volume 40 mL, alcoholysis time 2.5 h with isopropanol as alcoholysis reagent. And the surfactants, as shown in the experiments, had a significant effect on the dispersion and morphology of Sb4O5Cl2 nanoparticles. The result also showed that electrostatic attraction reached a maximum after mica was immersed in MnCl2 solution for 15 min so that the amount of Sb4O5Cl2 particles adsorbed on the surface of mica was the greatest. The final nano-Sb4O5Cl2 particles were uniformly well-dispersed.