This paper focuses on the synthesis and the photoluminescent properties of Ca 3−x Al 2 O 6 :xEu 3+ (0≤x≤0.1) nanophosphors prepared by microwave-assisted combustion method without any further heat treatment. X-ray diffraction, scanning electron microscopy and photoluminescence spectroscopy were used to characterize the produced samples. Nanosized particles smaller than 120nm were obtained as confirmed by SEM. When exposed to UV light radiation at 254nm, the europium-doped nanoparticles showed strong reddish-orange luminescence due to the characteristic transitions 5 D 0 → 7 F 1 (orange) and 5 D 0 → 7 F 2 , (red). The maximum emission intensity of the visible emission was obtained for x=0.05. It was also found that higher doping concentrations led to the luminescence quenching by a cross-relaxation mechanism between Eu 3+ ions in the lattice.