In the present work, nanocrystalline Gd2-xEuxO 3 phosphors have been synthesized by sol-gel method. The effect of Eu3+ concentration and annealing temperature on structural and luminescence properties of nanocrystalline powders were investigated. X-ray diffraction analyses showed that cubic Eu-doped Gd2O3 was formed and exhibited an average crystallite size ranging from 29nm to 41nm when the annealing temperature varied from 750 to 950°C, respectively. Photoluminescence (PL) measurements verified the presence of all transitions of Eu3+ dopant, being the 5D0 to 7F2 transition the most intense. It was also found that, on a common weight basis, the PL intensity was strongly dependent on both the annealing temperature and dopant concentration. The highest PL intensity was observed for 'x'=0.15. The observed quenching in luminescence would result from exchange interactions. Preliminary results on the PL characterization of nanocrystalline Gd2-xEuxO3 thin films are also presented.