Zirconia (ZrO2) thin films were prepared by metalorganic chemical vapor deposition (MOCVD) using ultrasonic nebulization with new source materials, Zr(OBu)(4), Zr(OBu)(3)(acac), Zr(OBu)2(acac)2, and Zr(OBu)(acac)(3). This process is a simple and economic method to prepare oxide thin films. Zr(OBu)(4) was successfully reacted with acetylacetone at a molar ratio of 1:3. Polycrystalline thin films were deposited at a substrate temperature range from 300 to 550 degrees C. The substitution of alkoxy radicals by acetylacetone made the deposition rate higher and insensitive to substrate temperature. The films deposited below 450 degrees C mostly had a monoclinic structure, and those deposited above 450 degrees C had a tetragonal structure. The measured optical energy band gap of zirconia film was 5.32 eV.