Powder nanoparticles of vanadium oxide doped with titanium dioxide were successfully prepared by the chemical co-precipitation method. The sample was calcined at temperatures 150, 300, 450, and 600°C. As prepared and heat-treated samples were structurally characterized through X-ray diffraction. The crystal size, cell parameters, R-Factor, and structural properties of mixed nano oxide were investigated. The value of the goodness fit factor, R-Factor, and cell parameters were examined by Rietveld Refinement. XRD study reveals that V2O5 exhibits orthorhombic structure and this orthorhombic phase is fully developed at 600°C. By using XRD data crystallite size of V2O5 was estimated to be 33.98nm and the crystallite size of TiO2 was estimated to be 35.04nm.