In the present work, we have synthesized ZrO2 doped PbO2 nanocomposites by hydrothermal method using Zirconium nitrate hydrate [Zr(NO3)(4) center dot 5H(2)O] and lead nitrate [Pb(NO3)(2)] as a precursor. The results show that the amount of Iodine (I) and the NaOH concentration plays an important role in the formation of hexagonal structure. The quantum confinement regime (QCR), phase analysis, purity and morphology are investigated by X-ray diffraction (XRD), Ultraviolet-visible spectroscopy (UV-vis), Fourier transform infrared spectroscopy (FTIR), High resolution transmission electron microscopy (HRTEM), Energy dispersive X-ray spectroscopy (EDX), mu-Raman spectroscopy, The photocatalytic activity was evaluated by the degradation of methylene blue (MB) dye under UV and visible light solar irradiation. Due to the quantum confinement effect of nanocrystals, this nanocomposite could be potential building blocks to construct functional devices and for the main cladding materials for water-cooled reactors. (C) 2016 Elsevier B.V. All rights reserved.