Abstract-Multiphase nanopowder and amorphous/amorphous-nanocrystal coatings on the basis of Al 2 O 3 have been produced on a glass substrate by the method of pulsed electron beam evaporation in vacuum. Their characteristics are studied by XRD, BET, pulsed cathodoluminescence, and differential scanning calorimetry (DSC)/thermogravimetric analysis. The effect of the deposition time of nanoparticles (NPs) on the phase composition of coatings and nanopowders is established. The correlation of luminescent properties with the phase composition of coatings and nanopowders is detected. Amorphous-nanocrystal coatings and nanop owders containing an Al 2 O 3 γ phase with a defective cubic spinel structure are promising materials for the dosimetry of different types of ionizing radiation.