Nanoparticle doped Tb3+:MgAl2O4 synthesized by combustion method at 300◦C via ignited a stoichiometric mixture of aluminum nitrates, magnesium nitrates and Terbium nitrates with malonic acid dihydrazide as a fuel following by annealing at 800, 1000 and 1200oC. The obtained samples characterized by different tools as thermal analysis (TG-DTA), X-ray diffractions (XRD), UV–Vis spectroscopy, Transmission electron microscopy (TEM) and Infrared spectroscopy (IR). Particle sizes for 5%Tb3+:MgAl2O4 with a size of 10-12.5 nm and for 10%Tb3+:MgAl2O4 with a size of 10-12.5 nm were produced within the range of 800oC/2h -1200oC/2h compared by the particle size of MgAl2O4 with a size of 10-12.5 nm in the same condition.