The high energy ball-milling technique has been used to produce metastable Ni(Ru) alloys supported on alumina. This catalyst has potential application for the hydrogenation of the C=O bond. The active species are first formed by mechanical alloying pure Ni and Ru powders. The alumina support is ground independently until no structural transformation occurs. Finally, the supersaturated Ni(Ru) powder is milled with the alumina support to produce highly dispersed individual Ni(Ru) nanocrystals on the surface of Al2O3. This supported catalyst has been characterized by X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy and thermal desorption spectroscopy.