Nanostructured Ni films were deposited on Cu by reducing nickel acetate tetrahydrate in refluxing ethylene glycol at about 194 °C. The effects of deposition time (t) and Pt as nucleating aid were investigated in this polyol process. The solution chemistry varied with t. At longer t, corrosive attack of the solvent on deposited films led to dissolution and re-deposition of Ni. Saturation magnetization increased with t and decreased with increasing Pt precursors. The deposited Ni films were magnetically saturated. They showed in-plane magnetization anisotropy and perpendicular coercivity anisotropy. The use of Pt caused rapid powder precipitation but did not enhance film deposition. The Pt-catalyzed Ni films showed a (200) texture and a higher squareness ratio.