The corrosion of carbon steel is major infrastructure degradation problem in practically all industries, including chemical materials, mineral, and petrochemical industries. Coating on carbon steel is one of the techniques which required improving corrosion resistance in extreme environments. In present work, NiCoCrAl was diffusion-coated onto low carbon steel by electrodeposition for NiCo and pack cementation for Cr and Al. The cross section of coated specimen was observed and analyzed using SEM and TEM. Two types of coating processes have been challenging the formation of bond-coat layer on carbon steel substrate with different temperature coating process. SEM and EDS results show that the coating comprises three layers: intermetallics zone of Ni (Al) and Al (Cr), interdiffusion zone of Ni (Co), and there is the substrate. By XTEM observation, it was found that γ (Ni,Fe) and ζ hexagonal structure were identified in all specimens. Orthorhombic structure with the Al3Ni was identified in specimen developed at temperature of 800OC. Further, the top surface of a 1000OC specimen has two phases of β-NiAl and ζ hexagonal structure. In order to understand the performance of two types coating system with different temperature process, oxidation test at temperature of 800OC for 100 hours has been carried out and the result shows that coating system which was developed at 800OC has better oxidation resistance compare to 1000OC coating system.