A two-step strategy to the large-scale synthesis of sheet-like Y2O3:Eu3+ microcrystals is presented. XRD, TEM, SEM and photoluminescence spectroscopy have been employed to characterize the as-synthesized products. The results show that the sheet-like Y2O3:Eu3+ microcrystals are single-crystallite with a dense structure at relatively low calcination temperatures and transform into polycrystallites with a porous structure at high calcination temperatures. Furthermore, the single-crystallite material exhibits higher photoluminescence intensity in comparison with the polycrystallite product. (c) 2004 Elsevier B.V. All rights reserved.