The application of molybdenum was limited as a candidate material for working at a high temperature because molybdenum has a poor oxidation resistance. MoSi2 is typically selected to solve the problem since it can form a dense SiO2 coating to protect the substrate molybdenum. MoSi2 coating on the surface of the Mo was prepared by pack cementation process in this paper. The silicide coating was formed by controlling the weight ratio of Si/MoSi2 powders and the pack cementation time. The results showed that the Si is mainly involved in the formation of a silicide layer on the surface of Mo. The MoSi2 is little participation in the coating formed. Two silicide layers have formed on the surface of Mo, outer layer of MoSi2 and inner layer of Mo5Si3. With the extension of time, the thickness of the MoSi2 layer and the Mo5Si3 layer increases, but the increasing rate slows down. Introduction High melting point and high temperature strength of refractory metals has attracted the attention of many researchers, Refractory materials play an important role in national defence industry, aviation, nuclear industry[1,2]. Metals with melting point above 1800 °C, such as tungsten, molybdenum, niobium, vanadium and chromium, have lower prices and wide range of practical applications. Molybdenum has been attended as high temperature performance, high thermal conductivity, specific heat capacity low, and has good thermal shock and thermal fatigue ability. Molybdenum antioxidant performance is poor, because they begin to form oxide above 400°C, and volatilization of the oxide with the increase of temperature rapidly speed up[3], resulting in the failure of materials, but the high temperature anti-oxidation coating can effectively resolve the refractory metals oxidation problem. The development of high temperature anti-oxidation coating has attracted the attention of many researchers at home and abroad. Ryosuke, etc. [4] using the Molten-salt Growth Method in a pure Nb matrix prepared NbSi2 coating. Tatsuo, etc. [5] has prepared Mo(Si,A1)2 coating by hot pressing coated niobium alloys. The lack of the antioxidant capacity of these coating systems or service temperature is low (≤1400°C), and difficult to meet the high temperature (≥ l 600°C) for a long time anti-oxidant requirements. Excellent high temperature properties of MoSi2 caused the concern of researchers recently. The glassy SiO2 phase generated at high temperatures can prevent the further oxidation of the coating, and effectively play a role in filling the crack. As for the formation of MoSi2 coating, Mo layer was firstly deposited using plasma or arc[6], and then silicified to the MoSi2 coatings. This MoSi2 coating has more pores or cracks and it is easy to peel off. Suzuki etc [7] prepared MoSi2 coatings on the Mo substrate and alloy steel by a molten salt method, the laser cladding method and CVD method, but the cost is high. The MoSi2 coatings were prepared by dipping slurry on a molybdenum substrate, and then using the pack cementation method in this study. The coating density, thickness and other factors were analyzed. International Conference on Materials, Environmental and Biological Engineering (MEBE 2015) © 2015. The authors Published by Atlantis Press 347 Experimental 1mm thick molybdenum plates were cut into 30mm×15 mm samples and the samples surface was ground with sandpaper, and was cleaned by ultrasonic instrument filled with acetone, and then dried. The Si powder, MoSi2 powder and activator powder were mixed by a certain proportion, and then mixed with organic binder into the slurry on the molybdenum surface. After dried, the mixed powder was covered in a crucible. Lastly, the sample was put into a vacuum furnace for heat treatment at the temperature of 1320°C for 7 hours. The sample was cut and polished the cross-section after the heat treatment. The organization and structure of the coating were analyzed by using the scanning electron microscope (JSM-5600LV type) and the spectrum analyzer (IE 300 X-type). Results and Discussion The effect on the ratio of Si powder and MoSi2 powder. Si powder is a silicon atom source. MoSi2 powder could be a diluent and NaF powder plays the role of the activator. The Si atoms spread to Mo atoms vicinity to react with Mo for formation a silicide. The different Si, MoSi2 weight ratio was designed, and to study the formation of the silicide layer. The total weight of these two materials is 30g. Fig. 1 is the morphology of samples cross section with heat treatment at the different ratio of Si/MoSi2. It shows that the molybdenum surface have formed two layers of the darker outer layer and lighter inner layer. Through energy dispersive spectroscopy analysis, the outer layer of Mo / Si atomic ratio close to 1:2, formed the MoSi2 layer and the inner Mo / Si atomic ratio close to 5:3 formed the Mo5Si3 layer. Observed the morphology of the coatings, the outer layer of MoSi2 prone to cracks, while inner Mo5Si3 coating almost no cracks. It shows that the coating have good thermal expansion match between Mo5Si3 layer and Mo substrate. The coatings cracks were leaded by a large internal stress cooling to room temperature. Fig.1. The different Si/MoSi2 proportion of cross-section diagram (a)0:30; (b)1:4; (c)1:2; (d)30:0 A Mo5Si3 transition layer has formed between the MoSi2 layer and Mo substrate, but it was impossible to reach significant buffering effect because the thickness is too small, and the MoSi2 layer still have cracks because of the large internal stress. a b