Thin films of poly(3-hexadecyl pyrrole) (P3HDP) nanoparticles have been fabricated by using Langmuir-Blodgett film deposition technique. The structures and morphology of the films were studied by using infrared spectroscopy, scanning and transmission microscopes. The experimental results demonstrated that the nanoparticles were formed by self-assembling P3HDP at air-water surface. The water contact angles of these films with different deposition layers were measured to be as high as 110°.