Organic-inorganic hybrid films were prepared through layer-by-layer (LBL) deposition of poly(allylamine hydrochloride) (PAH) and ZrO2 nanoparticles coated with poly(acrylic acid) (PAA), allowing facile control. of surface roughness and hydrophobicity. Superhydrophobic behavior was observed after deposition of silica nanoparticles and a simple fluorination of the surface. The structure of films was controlled by the number of deposition cycles using PAA-coated 100 nm ZrO2 nanoparticles, the particle size, and the prelayer with PAH and PAA. The change in the apparent water contact angle of (PAH/PAA-coated ZrO2)(n) surfaces without fluorination of the surface agrees with Cassie and Baxter's model for nonwetted surfaces even though the outermost surface itself is hydrophilic. Superhydrophobic surfaces were then successfully developed by the deposition of hydrophilic silica nanoparticles on a 10 bilayer surface of PAH/PAA-coated ZrO2, and a simple fluorination. Moreover, the chemical stability of the film was greatly increased by heat-induced cross-linking of the film. The incorporation of ZrO2 nanoparticles in superhydropbobic films promises better mechanical properties than the organic film.