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Bimetallic catalysts have been studied intensively because of their unique activity and selectivity. Unsupported alloy catalysts, however, are usually of limited value due to their very small surface areas. We have now developed a sonochemical synthesis of bimetallic alloys that provides both high surface areas and high catalytic activity. We have produced Fe-Co alloys by ultrasonic irradiation of mixed solutions of Fe(CO)5 and Co(CO)3(NO) in hydrocarbon solvents. The alloy composition can be controlled simply by changing the ratio of precursor concentrations. After treatment at 673K under H2 flow for 2 hours, we obtain nearly pure alloys. BET results show that the surface areas of these alloys are large (10-30 m2/g). TEM and SEM show that the alloy particles are porous agglomerates of particles with diameters of 10-20 nm. Sonochemically prepared Fe, Co, and Fe-Co powders have very high catalytic activity for dehydrogenation and hydrogenolysis of cyclohexane. Furthermore, sonochemically prepared Fe-Co alloys show high catalytic selectivity for dehydrogenation of cyclohexane to benzene; the 1:1 ratio alloy has much higher selectivity for dehydrogenation over hydrogenolysis than either pure metal.