Mechanical Alloying is a solid state powder processing technique, used for developing a wide variety of conventional as well as novel materials, having unique microstructures and properties. It involves milling of powders in a desired weight ratio in an inert atmosphere, during which repeated welding, fracturing and rewelding of powder results in a homogenous mixture of powders with very fine structure. This process is used to prepare variety of materials including alloys and intermetallics. Nickel-based alloys are commonly used as soft magnetic materials, which possess high permeability, high saturation magnetization and low coercivity. Generally, Ni-Fe-Cr alloys have high relative permeability and low eddy current losses. Alloys of the miscible Nickel-Iron-Chromium system prepared by MA materials find applications in Magnetic devices, Transformers, Audio coils, Motors, A.C, D.C applications and other antifriction components in automotive, electrical and electronic industries. The present work deals about the mechanical alloying of Nickel-15wt%Iron-5wt%Chromium system using elemental powders and the milling has been carried out for varying time durations.