Abstract. -Fe-Cr phase was investigated using formula Fe 80 Cr 20 . Ball milling process and ultrasonic technique is successfully done to develop solid solubility and improve homogenous, respectively. However, the effect of the Cr to Fe powder is not complete investigated using combination of its process. Ball milling is conducted by milling time of 60 hours and ultrasonic technique were carried out at ultrasonic time of 3 h, 3.5 h, 4 h, 4.5 h and 5 h. From the strain effect analysis is obtained that the strain increased with crystallite size decreased and broad peaks due to the micro strain that is obtained from the increasing d-spacing. The solid solubility and lattice parameter of the material relatively increased from the untreated sample to treated samples with the highest solid solubility of 62.1% and highest lattice parameter of 3.091 nm which is located at the milled and UB 4.5 hours. It is caused the temperature increased that effect to the higher diffusion of the atom. Therefore, the combination treatment is highest promote to improve the properties of the metallic materials.