Three types of blends consisting of nano-Al2O3 particles, polyester, and epoxy resin were respectively prepared as suspended small balls in an acoustical levitator with a microgravity state. The microstructures of the blends were compared to those with identical composition prepared in a normal gravity field. The results showed that the nanoparticles was deposited at the bottom of blends, and the polyester possessed a sphere-crystalline-dispersed phase when the bends were prepared in the normal gravity field. However, the nanoparticles can be dispersed into epoxy resin at a nanoscale, and the polyester transformed to a highly dispersed amorphous phase when the blends were prepared by the acoustic levitation technique.