MoNiAl-WC reinforced Fe matrix composites were obtained by mechanical alloying. The effect of various reinforcement ratios on microstructure change, elemental characterization and phase transformation were examined by using optical microscopy, scanning electron microscopy, energy dispersion spectroscopy, X-ray diffraction, elemental surface mapping and a microhardness test. Fe and MoNiAl-WC compound and powder mixtures were synthesized by MA and nanocrystalline solid solution was obtained. The increase in the reinforcement ratio reduced grain size in the structure and increased the carbide ratio. The composite demonstrated excellent metallurgical qualities and interface bonding. Moreover, it was found that the amount of porosities increased with increasing reinforcement. X-Ray analysis showed the formation of NiAl, Al3Ni and WC phases.