A new physical route for the production of monodispersed microsphere nanoparticle-polymer Composites utilizing a beads milling method, followed by an electrospray method, has been developed. Poly(methyl methacrylate) (PMMA)-TiO2 composites were used as a model to evaluate the performance of this route. SEM images showed that the products were monodispersed, spherical, and nonagglomerate. The mean diameter was in the range of 0.25- 1.87 mu m, with a standard deviation of 0.06-0.172. TEM images confirmed that nonagglomerated TiO2 nanoparticles were highly dispersed inside the polymer matrices. We found that, the concentration ratio of TiO2 to polymer in the precursor led to changes in precursor properties, such as permittivity and electrical conductivity, and resulted in changes in the produced particle size.