The Ni-Al alloy containing Cr,Fe additives were prepared as Raney Ni Catalyst by high energy milling.The size and surface state of Ni-Al alloy powder were studied by particle size analyzer and sanning electron microscopy.the Structure was analyzed by XRD and Moessbauer methods.The results showed that after a high-energy milling(HEM).the Ni-Al alloy transforms to a nano-scale NiAl structure with rich Al.By annealing the alloy,a metastable Ni2Al3 phase can be obtained.