A facile co-reduction and annealing synthesis route of nanospheric particles of Au-Ni bimetal with adjustable composition was developed. In a typical synthesis, a direct co-reduction of HAuCl4 center dot 4H(2)O and NiCl2 in aqueous solution was performed with the assistance of reductive NaBH4 and an anionic surfactant sodium dodecyl sulfate (SAS) functioned as the structure-directing agent. Ultrasonic mixing was used at the same time to control the size of the particles. The morphology, microstructure and the state of the surface atoms were analyzed in detail. These nanospheres showed enhanced electrocatalytic activity towards oxygen reduction reaction than that of pure Au nanoparticles, demonstrated in the low temperature SOFC as cathode. The maximum power density generated is 810 mW cm(-2) at 550 degrees C. This is a promising route of taking advantages the Phase Separation Mechanism to greatly reduce the use of noble metals in the ORR field without sacrificing the electrocatalytic activity. (C) 2014 Elsevier B.V. All rights reserved.