Y2O3-H3BO3:Eu3+ powders were synthesized by the mechanical alloying (MA) method, and their structural and photoluminescent characteristics were investigated by X-ray diffractometry (XRD), scanning electron microscopy (SEM), thermogravimetric/differential thermal analysis (TG/DTA), and luminescence spectrophotometer. The crystallite size of the powder mixture milling for 30 minutes (min) by the Willaimson-Hall method was approximately 58.8 nm with strain of 0.00141; overall, the internal strain increased with the milling time (t(m)). The morphology of the powder mixture with t(m), as observed by SEM, divided into three different stages: agglomeration (0 < t(m) <= 30 min), disintegration (30min < t(m) <= 120 min), and homogenization (120min < t(m) <= 300 min). The transition temperature and the weight reduction rate of the sample powders were 645.58 degrees C and 2.851%, respectively. Furthermore, the photoluminescence of the powder mixture excited to 240 nm by a zenon discharge lamp (20 kW) was detected near 592 nm(D-5(0) -> F-7(1)), 613 nm, 628 (D-5(0) -> F-7(2)), and 650 nm (D-5(0) -> F-7(3)). (C) 2012 Elsevier B. V. All rights reserved.