Metal oxides play a very important role in many areas of chemistry, physics and materials science in the Nano metric scale. In the present work, the metal oxides of Vanadium and Zirconium and their composites are synthesized and characterized. Vanadium pentoxide nanoparticles prepared by Precipitation method. Zirconium oxide nanoparticles prepared by Chemical method are used to synthesize V2O5-ZrO2 Nano composites by Chemical method. All are characterized by UV-Vis studies, FTIR techniques; X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Atomic Force Microscope (AFM).The thermal behavior of the Nano composite is determined by Differential Scanning Calorimetry (DSC). From UV-visible spectrum of V2O5-ZrO2nanocomposite the peak intensity isobestic point at 400nm which indicates that the intercalation of ZrO2 in V2O5 lattices. XRD behavior of V2O5 nanoparticle, ZrO2 nanoparticle and V2O5-ZrO2nanocomposite exhibit the particle size distribution in the range of 7 to 85 nm. The structure of V2O5 nanoparticles, ZrO2 nanoparticle and V2O5-ZrO2nanocomposite are characterized using the SEM. Nano size of the V2O5 nanoparticle, ZrO2 nanoparticle and V2O5-ZrO2 nanocomposite are confirmed by AFM study.