Mixing and sintering aluminium and 20% mechanically alloyed Fe/B nanoparticles provokes the formation of intermetallics in the aluminium matrix when following a powder metallurgy route. Materials were sintered in a wide range of temperatures (from 600 to 1100 oC). Previous studies have shown that these materials present neither important dimensional changes during sintering nor significant differences in mechanical properties. However, sintering temperature strongly affects corrosion resistance and hot rolling capability. Low sintering temperature provides nanocomposites with lower corrosion properties and hot rolling capability. In this work the nanocomposites obtained at different temperatures were characterized by X-ray diffraction. This technique allows following the formation of different intermetallics at each temperature, since being non-equilibrium processes, the use of ternary phase diagram of these elements is not possible.