In this paper we present the results of our patented (application filed in India) process for synthesizing a mixture of nanozirconia and nanosilica, obtained by the sol–gel method from commercially available zircon flour and hydrofluoric acid at low temperatures (∼ 100°C). Within the scope of this study, 99.2% dissolution of zircon was obtained by using 40% HF for a solid–liquid (S/L) ratio of 0.05 for a digestion period of 120 h. The nanoparticles, characterized by XRD, SEM and TEM techniques, were found to be largely spherical in shape and the average size of the particles was found to be less than 5 nm. Within the product, zirconiarich and silica-rich regions were found to exist.