A simple combustion route was employed for the preparation of Eu 3+ -doped MgAl 1.8 Y 0.2− x O 4 nanocrystals using metal nitrates as precursors and urea as a fuel in a preheated furnace at 500°C. The powders thus obtained were then fired at 1000°C for 3h to get better luminescent properties. The incorporation of Eu 3+ activator in these nanocrystals was checked by luminescence characteristics. These nanocrystals displayed bright red color on excitation under 254nm UV source. The main emission peak was assigned to the transition [ 5 D 0 → 7 F 2 ] at 615nm. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) studies were carried out to understand surface morphological features and the particle size. Crystal structures of the nanocrystals were investigated by the X-ray diffraction (XRD) technique. The crystallite size of the as-prepared nanocrystals was around 29nm, which was evaluated from the broad XRD peaks. The crystallite size increased to ∼45nm on further heat treatment at 1000°C.