NiFeCr nanoparticles with a Ni-rich composition were synthesized using a wet chemical synthesis technique. As-synthesized nanoparticles were crystalline with an average size of 6.8 ± 2.5 nm. For electrochemical analysis, as-synthesized nanoparticles were mixed with epoxy and coated over a mild steel substrate. Electrochemical measurements exhibited a very high polarization resistance and very low corrosion current for the nanoparticle-epoxy coated sample illustrating high resistance of the NiFeCr nanoparticle-epoxy coating towards highly corrosive media.