Nanostructured NixCo100−x films were deposited on Cu substrates by reducing the constituent metal salts in refluxing ethylene glycol at 194 °C. The average crystallite size increased with x, and reached a maximum of 64 nm when x = 100. The coercivity Hc of the films measured in the direction perpendicular (⊥) to the plane of the film was higher than that in the parallel (∥) direction. For the sample of x = 50, Hc⊥ was 379 Oe, which was six times that of Hc∥. Saturation magnetization Ms in the film plane was 1016 emu/cm3, and the remanent magnetization Mr 636 emu/cm3, giving a squareness ratio of 0.63. This film also had a Vickers hardness of 193. © 1999 American Institute of Physics.