In this study, monoclinic luminescent Gd2O3 nanocrystals doped with different concentrations of Er3+ (0.1, 1, and 10 mol%) were produced by propellant synthesis and flame spray pyrolysis (FSP). A comparison of their optical and morphological properties is reported. Following 980 nm excitation, an increase of the emission intensity from the H-2(11/2), S-4(3/2) -> I-4(15/2) and F-4(9/2) -> I-4(15/2) transitions was observed with increasing Er3+ concentration in the Gd2O3 nanocrystalline samples prepared via both techniques. However, the overall upconversion emission intensity was greater for the samples obtained by FSP. Furthermore, as the Er3+ concentration was increased, the intensity of the red (F-4(9/2) I-4(15/2)) emission was observed to increase more rapidly in comparison to the green (H-2(11/2), S-4(3/2) -> I-4(15/2)) emission resulting in an overall enhancement of the red component in the upconversion emission. Although both synthetic routes yield average crystallite sizes in the nanoscale, the TEM and SEM images confirm a more homogeneous morphology and lower particle aggregation for the nanocrystals produced by ESP. (C) 2010 Elsevier Ltd. All rights reserved.