The purpose of this work is to study the macrostructure, adsorption properties, and characteristics of reactivation of nonpyrophoric Raney Ni. It is shown that prevention of spontaneous combustion of Raney nickel by heat treatment in a controlled gaseous atomosphere leads to decrease of its specific surface, increase of the particle size of the catalyst, and increase of the relative content of strongly bonded hydrogen. According to the results of XPS spectroscopy (ESCA), a thin layer of nickel-aluminum spinel is formed on the catalyst surface.