The Ba 2 Zn 1-x Ni x WO 6 double perovskite oxides were synthesized using solid state reaction method. The effect of replacement of Zn 2+ with Ni 2+ cation on the structural properties was investigated by X-ray diffraction (XRD) at room temperature. From the X-ray diffraction and by means of standard Rietiveld method, the samples showed the same cubic crystal structure with (Fm-3m) space group and the crystallite size ranging from 71.91 nm to 148.71 nm. The unit cell volume was found to decrease as a result of the replacement, while there was no significant difference in the value of tolerance factor of the samples. This is may be due to the convergence of ionic radii of Ni 2+ and Zn 2+ cations. The Fourier Transform Infrared Spectroscopy (FTIR) was performed for the samples and the resultant characteristic absorption bands confirmed the double perovskite structure.