Methods of making nanocrystalline materials, particularly ternary and quaternary nickel-iron alloys having a particle size of less than about 100 nm, such as nanocrystalline nickel and NiFeCr and NiFeCrMn alloys with an average overpressure of less than about 11 nanometers, are described. Nanocrystalline nickel is pulsed D.C. By application of an electric current it is deposited on the cathode in an aqueous acidic electrolyzer. Ternary and quaternary nickel-iron alloys and other binary, ternary and quaternary alloys are listed in D.C. Electroplating or Pulse D.C. It can be produced by electroplating. The electrolyte in the electrolytic cell also contains stress relieving agents, such as saccharin, which aid in particle size control. The novel products of the present invention can be used as wear resistant coatings, hydrogen storage materials, magnetic materials and catalysts for hydrogen evolution.
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