Abstract: 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.