In this work, Fe-Cr alloys were coated via Aluminum (Al) pack cementation, followed by Nickel (Ni) electrodeposition. The process of pack cementation was done with mixing powders of Al, Al(2)0(3) and NH4Cl with weight percentage of 15%, 85%, and 5% respectively. To control successful Al diffusion to the substrate, pack cementation was conducted for 7 hours with two holding temperatures treatment at 400 degrees C for 4 hours, and 800 degrees C hours for 2 hours. Subsequently, the electrodeposition of Ni was applied with the solution consisting of NiSO4, H3BO3, and NiCl2. The samples were placed in the cathode, and then dipped in the solutions, while Ni plate used as anode. Successfully the samples were coated by dual Al-Ni layers, the samples were slowly heat treated at 900 degrees C for 10 hours. The interdiffusion of Al and Ni were characterized with SEM/EDX to investigate the distribution of the elements. Mechanical properties of the coated substrates were analyzed with Hardness Vickers (HV). It was found the hardness of the substrate increased significantly, from originally 255 HV to the 1177 HV after pack cementation. The hardness of the substrates has decreased to 641 HV after Ni plating, but subsequent heat treatment has been able to increase the hardness to 842 HV. This phenomenon can be correlated to the inward Al diffusion, and outward Fe, Cr diffusion. The formation of intermetallic compounds due to Al inward and Fe, Cr outward diffusion were discussed in details.