TECHNOLOGY FOCUS - INORGANIC CHEMISTRY - Preferred Method: The method comprises: adding an organic capping molecule to the mixture; reducing the mixture to form a many intermetallic metal alloy compound nanoparticles substantially capped by an organic shell, where the intermetallic metal alloy compound nanoparticles are characterized by the noble metal preferentially disposed proximate the surface of each of the noble metal nanoparticles; depositing the organic shell capped metal alloy nanoparticles on a high surface area carbon substrate powder, where the metal alloy nanoparticles are substantially free of platinum; and increasing the pH of the noble metal complex mixture and the base metal complex mixture; combining the noble metal complex mixture and the base metal complex mixture to form a complex salt solution; adding a carbon support to the complex salt solution to form a resulting mixture; heating the resulting mixture to reduce the resulting mixture to form a product including the metal alloy nanoparticles. The method further comprises: depositing the mixture on a carbon substrate to form a polymetallic catalyst substantially free of platinum, where the polymetallic catalyst is characterized by an oxygen reduction reaction (ORR) activity of at least about twice the ORR activity of a monometallic catalyst formed from the first noble metal; treating the polymetallic catalyst with an acid to remove at least a portion of an unwanted phase from the polymetallic catalyst; incorporating the polymetallic catalyst in a fuel cell; heating the mixture in an atmosphere of 600-800 degrees C while reducing the mixture; and removing the organic shell from the intermetallic metal alloy nanoparticles by one of a chemical treatment and a heat treatment. The method is conducted in a hydrogen containing atmosphere to form many polymetallic nanoparticles supported on a high surface area carbon support. The heat treatment comprised heating to a temperature of 600-800 degrees C. The noble metal and the base metal form an intermetallic compound when heat treated in a hydrogen reducing atmosphere. Preferred Components: The first noble metal is palladium (preferred), iridium, rhodium or gold. The first base metal is copper (preferred), iron, cobalt, nickel, zinc, tantalum, tungsten, rhenium or molybdenum. The nominal molar ratio of palladium to copper is 1:3-3:1. The first noble metal precursor comprises an acetoxy group. The noble metal comprises palladium. The base metal comprises a transition metal. EXAMPLE - Copper(II) acetate (0.0911 g) and palladium(II) acetate (0.0371 g) were added to 2-ethoxyethanol (130 ml) and oleic acid (1.3 ml) at 80 degrees C and the solution mixture was stirred for 30 minutes. Oleylamine (0.45 ml) was added and the reaction mixture was heated to 120 degrees C. The reaction was continued under reflux conditions for 2 hours. After the reaction mixture was allowed to cool to room temperature to obtain palladium-copper nanoparticle. The obtained precipitate was dried under nitrogen atmosphere to give purified palladium-copper nanoparticle (1:3).