Fe50Se50 alloys has been produced from the elementary powders in a high-energy ball mill.The influence of milling times on the microstructures, structure and thermal proprieties have been studied by scanning electron microscopy (SEM) coupled with (EDS) microanalysis, X-Ray diffraction (XRD) and differential scanning calorimetry (DSC).The interaction hyperfine and magnetic proprieties are investigated by transmission Mössbauer spectroscopy (TMS) and thermomagnetic measurements (VSM) respectively. For milling times up to 6 h, the Rietveld refinement of the X-ray diffraction spectra shows the formation of the hexagonal β-FeSe phase, amorphous selenium and also nanocrystalline α-Fe, the (DSC) curves shows several exothermic and endothermic picks, such as the crystallization the selenium amorphous at 103°C For milling times 39 h; the XRD shows the emergence of new phase, also in nanometric scale, a typical of α-FeSe phase tetragonal which has technological interest because is a superconducting phase. The Mössbauer spectroscopy confirmed to formation the two phase's paramagnetic hexagonal β-FeSe and − FeSe tetragonal, in according the XRD and DSC. Measurement of 2 magnetization (VSM) shows that saturation magnetization (MS) decreases by increasing the time of milling.