The influence of process parameters on formation of thin films of NiCoP is explained by evoking the reaction mechanism. Experimental work involved a systematic study of the mass transfer effects, the applied current density, the solution pH and temperature, and bath composition on the alloy composition, faradic efficiency and morphology of the deposit obtained. The surface morphology of NiCoP alloys was obtained by scanning electron microscopy (SEM). The films were characterized by x-ray diffraction spectroscopy (XRD) and were found to be generally amorphous with small amounts of crystalline phases dispersed depending upon the phosphor content. The corrosion resistance of the deposits in a chloride medium was observed to increase with the phosphor content. The presence of phosphorous in deposits yields higher corrosion resistance. The recrystallization of NiCoP alloys at elevated temperatures was examined by differential scanning calorimetry (DSC).