Thin Cu/Ni multilayers were deposited on a rotating disk electrode by square-wave galvanostatic pulses in one-third and full strength Watts nickel baths with 50 to 1000 ppm CU2+. A theoretical model. was developed to predict the copper content in the Ni layer. Factors affecting the deposition which include the mass-transfer rate, copper ion concentration, temperature, and applied current density were studied. The copper content in the Ni layer was analyzed experimentally by x-ray diffraction and potentiodynamic stripping. Theoretical predictions are in good agreement with experimental results.