Oxidation protective MoSi 2 -Mo 5 Si 3 /SiC multi-coatings for carbon/carbon composites were prepared by chemical vapor reaction and slurry-sintering method. The influence of preparation technology on the structure and phase composition of the coating was investigated by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) analyses, and then their relationship was discussed. The results indicate that the Si/Mo ratio of the slurry and sintering processing were two main factors that significantly affected the structure and phase composition of the multi-coating. Appropriate sintering process and relatively high Si/Mo ratio were essential for preparing the multi-coating with dense structure and favorable phase composition. After being sintered at 1723 K for 2 h and with the Si/Mo ratio of the slurry being 4.5 (weight ratio), a dense structure accompanied by favorable phase composition of the coating can be obtained. When heat treated at 2373 K for 1 h, this coating became more compact and continuous. Oxidation tests (performed at 1623 and 1823 K) demonstrated that both of these two obtained multi-coatings exhibited better anti-oxidation property than single layer SiC coating. Oxidation protective MoSi 2 -Mo 5 Si 3 / SiC multi-coatings for carbon / carbon composites were prepared by chemical vapor reaction and slurry-sintering method. The influence of preparation technology on the structure and phase composition of the coating was investigated by scanning electron Microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) analyzes, and then their relationship was discussed. The results indicate that the Si / Mo ratio of the slurry and sintering processing were two main factors that significantly affected the structure and phase composition of the multi-coating. Appropriate sintering process and relatively high Si / Mo ratio were essential for preparing the multi-coating with dense structure and favorable phase composition. After being sintered at 1723 K for 2 h and with the Si / Mo ratio of the slurry being 4.5 (weight ratio), a dense structure accompanied by favorable phase composition of the coating can be obtained. When heat treated at 2373 K for 1 h, this coating became more compact and continuous. Oxidation tests (performed at 1623 and 1823 K) demonstrated that both of these two obtained multi-coatings for rendering better anti-oxidation property than single layer SiC coating.