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MoSi 2 and Mo(Si, Al) 2 coatings were prepared on Mo–0.5Ti–0.1Zr–0.02C alloy using pack cementation process. Oxidation studies revealed that Mo(Si, Al) 2 coating had a much superior oxidation resistance in the temperature range from 400 to 900 °C, where pest disintegration of MoSi 2 occurs due to internal oxidation. The growth kinetics of Al 2 O 3 layer formed on Mo(Si, Al) 2 coating was much slower than that of SiO 2 layer formed on MoSi 2 coatings during oxidation.