Using the sol-gel auto combustion method with diethanolamine (DEA) as fuel, a sequence of iron-substituted zinc aluminates, ZnFe x Al 2-x O 4 powders, including variable Fe 3+ ion concentrations (0 ≤ x ≤ 2) were effectively prepared. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), the Brunauer-Emmett-Teller (BET) method, UV-visible diffuse reflectance spectroscopy (UV-DRS), and vibrating sample magnetometer (VSM) were