In the present study, the dopant effect of Zn on the crystal structure, thermal properties and morphology of magnesium aluminate (MgAl2O4) spinel (MAS) structure was investigated. A pure and two Zn-containing MASs (e.g. MgAl1.93Zn0.07O4 and MgAl1.86Zn0.14O4) were synthesized for this purpose via a wet chemical method, and the as-prepared samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, differential thermal analysis (DTA), thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy techniques. It was found that the crystal structure, thermal properties and morphology of the MAS system change with the increase in the amount of Zn. MgO phase formation was observed. The values of the lattice parameter, unit cell volume and crystallite size increased, and the crystallinity percentage decreased. The morphology was also affected by adding of Zn.