Nanocrystalline silver-nickel deposits were prepared by pulsed electrolysis at different current densities from nontoxic complex electrolytes of two compositions containing silver nitrate and nickel sulphate. The structural and magnetic properties of these deposits have been analyzed in comparison with those of pure Ag and pure Ni deposited under similar conditions. The morphological and the microstructural studies have been carried out for these samples using SEM and HRTEM. The results suggest that the as deposited materials consist of Ag-Ni in the metastable alloy form. Heating the sample beyond Curie temperature leads to grain growth and long range ordering. The hysteresis curves and the magneto-thermograms reveal that the deposits exhibit room temperature ferromagnetism. (C) 2011 Elsevier B. V. All rights reserved.