The textural and structural properties of a skeletal Ni catalyst prepared by alkali leaching of aluminum from the rapidly quenched Ni 50 Al 50 alloy have been investigated by elemental analysis (ICP-AES), nitrogen physisorption, powder X-ray diffraction (XRD), scanning electron microscopy (SEM), and H 2 thermal desorption techniques. As compared to Raney Ni, such a skeletal catalyst has a residual Ni 2 Al 3 phase, lower surface area, higher average pore diameter and porosity, larger mean crystallite size, and unit-cell parameter. These differences are attributable to the metastable character of the pristine rapidly quenched alloy and their relationship with the catalytic behavior is discussed and correlated.