The Raney Ni catalyst was fabricated by mechanochemically process(MC process) in the Al-Ni system. Intermetallic compound obtained by mechanical alloying was leached in an alkaline solution. The characteristics of the mechanically alloyed powder and Raney Ni catalyst were analyzed by XRD, ICP-AES and EXAFS. In Al-50wt.%Ni, the metastable intermetallic compound phase close to AlNi phase was obtained by mechanical alloying unlike Al-Ni equilibrium phase diagram. The metastable intermetallic compound was transformed into $Al_3$$Ni_2$phase via the annealing at $750^{circ}C$. The microstructure of Raney Ni fabricated by MC process was mainly bcc Ni including fcc Ni.