This study investigated the effects of sintering at 700 °C and compositional variations on the structural and mechanical properties of (Ni-Cr-Fe) alloys prepared by powder metallurgy. X-ray diffraction (XRD) revealed no new phase formation, while sharper peaks and reduced full width at half maximum (FWHM) indicated improved crystallinity and increased crystallite size. Optical microscopy showed a grain-size reduction in sample (A) from 145 μm to 95 nm, whereas grain growth occurred in samples (B) and (C). Vickers hardness increased in sample (A) from 243.9 to 263.7 HV, decreased slightly in sample (B), and remained nearly constant in sample (C). The wear rate decreased in samples (A) and (B) but increased in sample (C). Overall, sample (A) exhibited the highest hardness, while sample (B) demonstrated superior wear resistance due to its balanced properties.