Incorporation of SiO 2 nanoparticles (NPs) into poly(vinyl chloride) (PVC) matrix to prepare PVC/SiO 2 nanocomposites (NCs) can enhance its properties. To achieve improved properties for the NCs, NPs should be dispersed properly and be compatible within the polymer matrix. Therefore, to prevent SiO 2 NPs from aggregation, surface modification of NPs was performed by citric acid (CA) and L(?)-ascorbic acid (AA) as biological and environmental friendly coating layers for the first time. This process was carried out under ultrasonic irradiation condition, which is an economical and eco-friendly tool. After that three different amounts of modified SiO 2 (SiO 2 -CA-AA) were inserted into PVC matrix and PVC/ SiO 2 -CA-AA NCs were prepared using solution casting method. The structures and morphology of the prepared NC films were verified by several techniques including Fourier transfer infrared, X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis, ultraviolet-visible (UV-Vis) spectroscopy and tensile testing. Thermogravimetric analysis confirmed the presence of about 13 wt% modifiers on the surface of SiO 2 . Microscopic observations showed good dispersity of SiO 2 -CA-AA NPs in the polymer matrix. Resulting NC films showed more flexibility than pure PVC.