The new process in order to fabricate of Ni catalyst with high activity by the mechanochemical(MC) method which was combined the mechanical alloying(MA) and the chemical treatment process. The microstructure and characterization of mechanically alloyed Ni-5-wt% Al powder and Ni catalyst gained by alkali leaching were investigated byt he various analysis such as XRD, SEM-EDS, HRTEM and laser particle analyzer. The steady state powder with 1~2$mu extrm{m}$ mean particle size was obtained after 30hr milling with the PCA of 2 wt% stearic acid under the condition of grinding stainless steel ball to powder ratio of 60:1 and rotating speed fo 300rpm. According to result of HRTEM diffraction pattern, MA powder of the steady state was nanocrystalline $Al_3$$Ni_2$ intermetallic compound. Ni catalyst was obtained after KOH leaching of the steady state powder was about 20nm nanocrystalline which contained about 8 wt % Al.