Ni-Fe alloys ranging in composition of Fe rich invar (Ni100-xFeX, where x ~ 64), have a variety of high technology applications due to their wide spectrum of physical properties. In this paper, the effects of the applied potential (-1.20V, -1.35V) and the bath composition (0.1M, 0.01M) of the Ni-Fe alloy thin films are studied. Ni100-xFeX layers were electrodeposited onto Copper substrates with a pH of about 2.5. The experiments were performed at room temperature and the deposition time was equal to 10mn for all deposited samples. The experiments were performed using electrochemical techniques, by means of cyclic voltammetry (CV) and chronoamperometry (CA). The morphology and elemental composition of the deposited films were studied by means of electron microscopy coupled to EDS analysis.