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In order to improve the oxidation resistance properties of 30 at.% Mo5Si3/MoSi2 composite at high temperature in air, a molybdenum disili-tide coating was prepared on its surface by a molten salt technology. XRD and SEM analysis showed that only tetragonal MoSi2 phase ex-isted in the coating after being siliconized for 5 h at 900℃. The oxidation film formed on the uncoated sample was not dense, so that oxygen diffused easily through it. The volatilization of MoO3 resulted in the oxidation film separating from the substrate. The MoSi2coating was proved to be an effective method to prevent 30 at.% MosSi3/MoSi2 composites from being oxidized at 1200℃. A dense glassy SiO2 film was formed on the MoSi2 coating surface, which acted as a barrier layer for the diffusion of oxygen atoms to the substrate. The 30at.% Mo5Si3/MoSi2 composites with a MoSi2 coating showed much better oxidation resistance at high temperature.