A two-step anodic oxidation process was used to prepare porous anodic aluminum oxide (AAO) template in oxalic acid electrolyte. By adjusting technological parameters including current density, oxidation time and electrolyte concentration, the AAO template possessed of uniformly distributed holes, similar aperture and hexagonal orifice was obtained. Meanwhile, by removing the barrier layer without peeling the film, the residual aluminum became basement and functioned as electrode. In the non-aqueous system, the nanowire array of Gd-Co alloy was prepared by DC electrodeposition in the AAO template. Through the observation of SEM, the aperture of AAO template is approximately 60 nm, and it changes little before and after removing the barrier layer. The prepared Gd-Co alloy nanowire is orderly and in the similar size. EDS measurement shows that nanowires are of Gd-Co alloy and a few oxides, in which Gd-Co alloy content is 90.66wt%, and the mole ratio of Gd to Co is 1:7.5. XRD analysis displays that the nanowire of Gd-Co alloy is noncrystal.