Nanocrystalline alumina particles coated with polyethylene have been prepared by a two-step chemical vapor synthesis (CVS) process using a hot-wall reactor to synthesize the nanocrystalline alumina core, and a RF plasma reactor for the subsequent polymer coating. The particle radius is about 4 nm, with the radius of the ceramic core being about 2.5 nm and the coating thickness about 1.5 nm. The powders have been characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Brunauer±Emmett±Teller (BET), small-angle neutron scattering (SANS), and high-resolution transmission electron microscopy (HRTEM).