用初始Ｍｏ粉和Ｓｉ粉通过自蔓延高温合成方法（ＳＨＳ）制取不同Ｍｏ５Ｓｉ３含量的ＭｏＳｉ２／Ｍｏ５Ｓｉ３复合材料．用Ｘ射线衍射仪、扫描电镜对产物进行组织结构分析．实验结果表明，在自蔓延高温合成中，ＭｏＳｉ２是一步生成，无中间相形成．随着样品中Ｓｉ含量的减少，产物中Ｍｏ５Ｓｉ３的含量增多，颗粒度变小 MoSi2 / Mo5Si3 composites with different Mo5Si3 contents were prepared by SHS method with the initial Mo powder and Si powder. The structure of the product was analyzed by X-ray diffraction and scanning electron microscopy. The experimental results show that in the SHS synthesis, MoSi2 is formed in one step, and no mesophase is formed. With the decrease of Si content in the sample, the content of Mo5Si3 in the product increases and the particle size becomes smaller