Nanopowders (NPs) of Eu doped MgAl2O4 were produced by laser evaporation of mixtures of micron sized powders of Al2O3, MgO and Eu2O3 with content of Eu 1, 2 and 4 mol%. The produced NPs were weak agglomerated and consisted of spherical particles with a mean diameter of 12–17 nm. The main phase of the NPs is defective spinel with a grain size 14 nm and content 91 wt.%. The produced powder contains additional phases of MgO and Eu2O3 as well. In order to form a structure of MgAl2O4:Eu3+ the NPs were annealed in air under a layer of coal at different temperatures from 800 C to 1300 C. Luminescent prop-erties of the annealed NPs were analyzed by the pulse cathode luminescence (PCL) method. The NP with the lowest Eu content had the highest emission intensity. The emission spectra of the NPs strongly depend on the annealing temperature. The maximum of emission intensity of the band 520 nm was observed at the annealing temperature of 1200 C.