A ZnSe alloy was prepared by mechanical alloying and annealing at 520 degrees C for 6 h. Samples were analyzed using X-ray diffraction (XRD) and differential scanning calorimetry (DSC). The as-milled alloy had a dark brown color, which turned to the yellow color characteristic of commercial ZnSe products after annealing. After 10 h of milling the alloy exhibited a zincblende structure. The DSC spectrum showed a broad exothermic band related to structural relaxation and an incomplete endothermic peak associated with the sublimation of nanometric ZnSe. corroborated by a second DSC scanning measurement which indicated the presence of amorphous Se as a product of sublimation. XRD and DSC measurements confirmed that the annealing process led to the structural relaxation and sublimation of nanometric ZnSe. As products of sublimation, hexagonal Se and zincblende ZnSe phases were observed. (C) 2008 Elsevier B.V. All rights reserved.