The solid solution variation of Fe and Cr mixed powder with balling time during mechanical attrition were detected using X -ray diffraction. The balled powder is observed using TEM (Transmission Electronic Microscopy ). It has been shown that the solution of Fe and Cr elements increases with increasing balling time and the Fe -Cr alloy completely alloyed can be obtained after balling 40 hours. Balling ran produce nanocrystalline grains in the samples, whose sizes are in the range from 20 to 80 nm after balling 20 hours. Also, Balling can lead to lattice strain, making lattice constants enlarge and diffraction angle shift to higher angle location. The lattice strain can be partly eliminated though annealing.