Coating films on glass substrate were prepared by sol-gel process using alkoxide solutions containing perfluoroalkylsilane (PFAS) and tetraethoxysilane (TEOS), The physical properties of the coating films were characterized by SEM, FT-IR, and XRD, And their surface properties were investigated by measuring contact angles and atomic compositions. Transparent coating films with smooth surface and uniform thickness could be obtained, The contact angles of the coating films for water and methylene iodide are extremely high, at 118 degrees and 97 degrees, respectively, and their surface free energies are about 9.7 dyn/cm, It was found that the water-repellent glass prepared is very hydrophobic and exhibits excellent water-repellency. Hydrophobic perfluoroalkyl groups are preferentially enriched to the outermost layer at the coating film-air interface, and two layers probably exist in the coating film. The upper layer oriented toward the air is composed of mainly perfluoroalkyl groups originating from PEAS, and the lower layer is composed of mainly -OSiO- groups originating from TEOS, The heat treatment after drying step cannot influence the surface enrichment of the perfluoroalkyl group. The hydrolysis reaction should be more completely done before the dip coating step to obtain lower surface free energy, The burning temperature should be less than 300 degreesC because the perfluoroalkyl group begins to decompose from this temperature.