MoSi2 is presently regarded as the most important material for electrical heating and as one with huge potential for high temperature structural uses. MoSi2 and MoSi2 matrix composites were prepared by self-propagating high tempera-ture synthesis (SHS). Pure MoSi2 was obtained and a compound of MoSi2 and WSi2 was synthesized in the form of pre-dominant solid solution (Mo,W)Si2. By adding aluminum of 5.5 at.% to Mo-Si, the crystal structure of MoSi2 changed into a mixture of tetragonal Cllb MoSi2 and hexagonal C40 Mo(Si,Al)2. The (Mo,W)Si2-Mo(Si,Al)2-W(Si,Al)2 composite mate-rials were synthesized by adding aluminum of 5.5 at.% to Mo-W-Si. However, if the amount of the added aluminum was not larger than 2.5 at.%, it did not have any significant effect. SHS is an effective technology for synthesis of MoSi2 and MoSi2 matrix composites. MoSi2 is presently regarded as the most important material for electrical heating and as one with huge potential for high temperature structural uses. MoSi2 and MoSi2 matrix composites were prepared by self-propagating high temperaure synthesis (SHS). Pure MoSi2 was obtained and a compound of MoSi2 and WSi2 was synthesized in the form of pre-dominant solid solution (Mo, W) Si2. By adding aluminum of 5.5 at.% to Mo-Si, the crystal structure of MoSi2 changed into a mixture of tetragonal Cllb MoSi2 and The (Mo, W) Si2-Mo (Si, Al) 2-W (Si, Al) 2 composite mate- rials were synthesized by adding aluminum of 5.5 at.% to Mo- W-Si. However, if the amount of the added aluminum was not larger than 2.5 at.%, It did not have any significant effect. SHS is an effective technology for synthesis of MoSi2 and MoSi2 matrix composites.