The fabrication of monocrystalline Ni5Sb2 nanowires array into porous anodic alumina membranes by using direct-current potentiostatic electrodeposition technique has been firstly reported. In this paper, the focus is on the effects of Sb content and the co-deposition voltage on the resultant. It was found that Ni5Sb2 nanowires array with a monoclinic structure could be successfully synthesized by regulating these two parameters. The analysis results displayed that the Ni5Sb2 nanowires array was highly filled and ordered, as well as around 80 nm in diameter. Structure analysis indicated that the as-deposited nanowires had a highly preferential orientation grown along [0 2 2] direction. (C) 2011 Elsevier B.V. All rights reserved.