AlSb nanocrystals were produced by the direct flow of electrons through powder mixture of 1: 1 M ratio Al:Sb. The phase, morphology, and vibration modes were characterized using XRD, TEM, and Raman spectroscopy. The optical property was also investigated using UV-Vis-NIR spectrophotometry. In the present research, the products were pure AlSb nanocrystals at 80 A for 10 min, and 110 A for 3 s, with the indirect energy band gaps of 1.647 eV and 1.688 eV, respectively. (C) 2011 Elsevier B. V. All rights reserved.