In this work shake milling were used to mechanically activate Nb – Al powder mixtures at different relative proportions (Nb80Al, Nb65Al, Nb54Al e Nb42Al). All milling process parameters were unchanged, e.g., powders mass, ball/powder mass ratio, balls diameter, quantity and kind of process control agent. Uniaxially compacted cylindrical pellets of milled powders were vacuum reacted. After a two-step degassing treatment (290°C for 0.5 h and 400°C for 4 h), samples were heated at 30°C/min. Ignition and combustion temperatures were measured by a thermocouple inserted in a hole drilled into the pellets. The microstructure of milled powders and reacted pellets were characterized by X-ray diffraction and SEM analysis. Bulk density of the pellets was measured by water immersion (Archimedes). The results showed a decrease of both ignition and combustion temperature with mechanical activation as seen by comparison with reacted pellets of the same composition not mechanically activated (simple mixtures). By increasing the heating hate the completeness of the reactions were improved. The lower the aluminum contents the lower the ignition and combustion temperatures and also the densification. The decrease on ignition temperature was caused by a more effective dispersion (and so more activation) attained by samples with lower aluminum content.