Bi2Te3, Sb2Te3 and Bi8Sb32Te60 thermoelectric materials have been prepared by mechanical alloying using a high energy planetary ball milt. The alloy formation was followed by X-ray diffraction (XRD), the morphology by scanning electron microscopy (SEM) and the composition by electron microprobe. The samples of Bi8Sb32Te60 were prepared in a reasonable milling time (less than 8 h) by mechanical alloying of binary alloys (Bi2Te3 and Sb2Te3). The single phase Bi8Sb32Te60 solid solution obtained presents convenient stoichiometry and good homogeneity in composition.