In the present thesis, a series of novel polymer nanocomposite (NC) films based on poly(vinyl chloride) (PVC) and poly(vinyl alcohol) (PVA) was prepared by solution mixing as well as facile and fast ultrasonic dispersion method. In the first and second projects, the zirconia , for having better dispersion and compatibility with organic media such as polymeric matrix, were modified with biosafe and biodegradable molecules including vitamin B 1 under ultrasonic irradiation conditions. The hydroxyl groups on the zirconia surfaces can interact with the modifiers functional groups. The grafting was confirmed by FT-IR spectroscopy, thermogravimetric analysis (TGA), XRD, field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) techniques. The TGA analysis has con?rmed the presence of about 7 wt% modifiers on the surface of zirconia. In the first part, the PVC/ ZrO 2 -VB 1 NC films were fabricated. For this aim, PVC has been selected as a polymeric matrix and its NCs with the different contents of modified zirconia (3, 5, 7 wt%) were prepared via ultrasonication. The obtained NCs were studied by FT-IR spectroscopy, TGA, X-ray diffraction, UV-Vis, water contact angle measurement, FE-SEM, TEM, and mechanical test. According to the UV-Vis spectrum, the absorption increased after the increase of zirconia as a high performance filler into the polymer matrix. The TGA results showed an increased thermal stability for the NC films compared with the pure polymer. Also, the morphological and curvature of normal distribution results showed a uniform dispersion of the particles in a nanoscale in the polymer matrix. In the second project, poly(vinyl alcohol) (PVA) was used as the polymer matrix and the PVA/ZrO 2 -VB 1 nanocomposite films were prepared by the addition of 3, 5, and 7 wt% of the modified zirconia to the PVA matrix under ultrasonic irradiation. The resulting nanocomposites were characterized using FT-IR,TGA and XRD,UV-Vis spectroscopy, FE-SEM, TEM, water contact angle measurement, and mechanical test. The water contact angle measurement showed an increase in the hydrophilicity of NCs compared wit the pure polymer. Also, the modified ZnO enhanced mechanical, thermal and optical properties of the prepared NC films.