In this study, double layer modification of ZrO 2 nanoparticle (NPs) was performed by citric acid and ascorbic acid as biodegradable and biocompatible modifiers for decreasing of agglomeration and improving of their compatibility with organic environments such as polymer matrix. The process was accomplished under ultrasonic method as a fast, low cost and green way. The modified ZrO 2 were studied with FT-IR, XRD, TEM, FE-SEM, and TGA techniques. In the first project, the poly(vinyl chloride)/ZrO 2 -CA-AA nanocomposites (NCs) films were successfully fabricated. For this purpose, different amount of the modified content (4, 8, 12 wt.%) incorporated to the PVC matrix by the ultrasonic technique. The properties of the synthesized NCs were studied by FT-IR, XRD, UV–Vis, FE-SEM, TEM, Mechanical test, and TGA techniques. The TGA analysis indicated that, T 5 and T 10 of the all NCs increased in compared with neat PVC. The UV absorption was changed by employing of ZrO 2 as an efficient filler in the polymer matrix. The FE-SEM images show that the modified were dispersed uniformely into the polymer matrix. In second part, different amount of content (4, 8, 12 wt.%) incorporated to the poly(vinyl chloride) matrix with ultrasonicated process and oly(vinyl alcohol)/ZrO 2 -CA-AA NC films were prepared. The NC films were studied by FT-IR, XRD, UV–Vis, FE-SEM, TEM, Mechanical test, and TGA techniques. The TGA analysis were confirmed the improvement of thermal stability of the NCs in comparison to the pure polymer. The TEM images show that the modified are core-shell in shape and a layer of PVA coated on the surface of ZrO 2 . The Mechanical analysis shows that the obtained NCs have higher mechanical properties in comparison to the pure polymer.