Nanocrystalline coatings have become an essential component of single and multilayer electronic packaging, ship building, mining, magnetorestrictive applications, etc. In the current work, nanocrystalline Ni-Cu films were synthesized by pulsed electrode-position using a citrate bath. Cathodic polarization experiments were carried out for optimization of bath composition to co-deposit nanocrystalline Ni-Cu films. Depositions were optimized between the current density range of 0.05-0.25 Acmr2to achieve a uniform equiaxed coating with a target Ni content of greater than 70% owing to their superior corrosion resistance and enhanced hardness.