MgAl2O4 was successfully used as a crystalline host network for the synthesis of nickel-based nano cyan refractory ceramic pigments. Different compositions of NixMg1xAl2O4 (0.1 6 x 6 0.8) powders have been prepared by using a low temperature combustion reaction (LTCR) of the corresponding metal nitrates with urea (U) as a fuel at 300 C in an open air furnace. The as-synthesized samples were characterized by thermal analysis (TG-DTG/DTA), X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM). UV–Vis and diffuse reflectance spectroscopy (DRS) using CIE- L⁄a⁄b⁄ parameters methods have been used for color measurements. The results show that the NixMg1xAl2O4 samples are the crystalline phase with a particle size of 8.85–43.66 nm in the temperature range 500–1200 C. The density, particle size, shape and color are determined for all the prepared samples with different calcination times and temperatures.