In order to protect Niobium material from oxidation, MoSi2 coating was prepared on the Niobium substrate by spark plasma sintering. Oxidation behavior of MoSi2 coating was investigated in air over the temperature range of 1200-1500 degrees C. The interfacial diffusion between MoSi2 coating and Niobium substrate was also examined. Dense MoSi2 coating was successfully prepared using spark plasma sintering. The porosities of top and side coatings are about 5.5% and 6.4%, respectively. No cracks were present in the MoSi2 coating. Cracking and spallation of the SiO2 scale did not occur at test temperatures. Two intermediate phases (Nb,Mo)(5)Si-3 and Nb5Si3 phases, were detected in the boundary of MoSi2 coating and Nb substrate. The growth of the reaction layer was dominated by the diffusion of Si toward the Nb substrate and obeyed a parabolic rate law. A multi-layered structural coating formed on Nb substrate, which consisted of MoSi2, (Mo,Nb)(5)Si-3 and Nb5Si3 in turn. (C) 2014 Elsevier B.V. All rights reserved.