RAMAZAN OG UZHAN APAYDIN, BURÇ AK EBIN, and SEBAHATTIN GÜ RMENNanostructured copper-nickel (CuNi) and copper-nickel-indium (CuNiIn) alloy particles were produced from aqueous solutions of copper, nickel nitrates and indium sulfate by hydrogen reduction-assisted ultrasonic spray pyrolysis. The effects of reduction temperatures, at 973 K, 1073 K, and 1173 K (700°C, 800°C, and 900°C), on the morphology and crystalline structure of the alloy particles were investigated under the conditions of 0.1 M total precursor concentration and 0.5 L/min H 2 volumetric flow rate. X-ray diffraction studies were performed to investigate the crystalline structure. Particle size and morphology were investigated by scanning electron microscope and energy-dispersive spectroscopy was applied to determine the chemical composition of the particles. Spherical nanocrystalline binary CuNi alloy particles were prepared in the particle size range from 74 to 455 nm, while ternary CuNiIn alloy particles were obtained in the particle size range from 80 to 570 nm at different precursor solution concentrations and reduction temperatures. Theoretical and experimental chemical compositions of all the particles are nearly the same. Results reveal that the precursor solution and reduction temperature strongly influence the particle size of the produced alloy particles.