Tin and bismuth powders were used to prepare the Sn40-Bi60 [wt%] mixture. The mixed powders were mechanically alloyed by processing in the high speed milling machine for 2, 4, and 6 h, respectively. When the milling process had been completed, all the resulting material was annealed and analyzed by XRD. The comparision of the results show, that the alloy is fully formed after 6 hours milling time. Differential scanning calorimeter was used to show the uniformity of the prepared alloy. SEM micrographs reflect the micro structure of the specimens. EDS analysis unveils that the alloy phase is very close to the assumed Sn40-Bi60 [wt%]. Mechanical properties evaluated by the micro hardness show the best results for 6 h milling time and 8 h annealing at 100 • C.