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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 μm, 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.