The aim of this study is to determine the nanocrystalline size by using Williamson-Hall method of Fe80Cr20 powder which prepared by mechanical alloying process. X-rays diffraction line profile analysis was adopted to analyze the crystallite size and microstrains of Fe80Cr20 alloys powder. Transmission Electron Microscopy (TEM) was used to examine the microstructure morphology of the nanosized of Fe80Cr20 alloys. The crystallite size, microstrain, and lattice parameters were estimated by Williamson–Hall plot. The results showed that the mechanical alloying processes resulted the final product in nanocrystalline size range (below 12 nm) which confirmed by TEM observation and XRD line profile analysis.