In this work spherical SiO 2 nanoparticles were synthesized by sonochemical method using a new Schiff-base as a capping agent. The silica nanoparticles were obtained by hydrolysis of tetraethyl orthosilicate in aqueous alcohol solution. The effect of different parameters such as molar concentration of Schiffbase ligands and ultrasonic irradiation on the morphology and size of the products was examined. The results demonstrated that applying the appropriate amount of Schiff-base could be effective in control of particle size. The influence of SiO 2 nanostructures on the flame retardancy of the poly styrene, poly vinyl alcohol, cellulose acetate and ethyl cellulose was studied. In-situ and ex situ nanocomposites were investigated and results confirm that flame retardancy of in situ nanocomposites were better than ex situ samples. HOÁÁÁSi-O-SiÁÁÁOH barrier prevents reaching of flame, heat and oxygen to the polymeric nanocomposites.