In this thesis,the bulk samples SiMoS1+x (0≦x≦1), the polycrystalline structure reveals a poorly-crystalline MoS2 phase with several unknown reflections. However in SiMoS1.4 all of the unknown reflections could be identified to be alloy MoSi2 structure, and it is the only sample which doesn’t show diamagnetic transitions. While in the XRD of the rest samples most of the unknown reflections may be assigned to alloy Mo3Si3 structure. The electrical transitions in resistivity of bulk sample SiMoS1+x with x = 0, 0.2, 0.8, and 1, are observed at 4.25K, 4.41K, 3.32K, and 3.75K, respectively. And the samples with x = 0 and 1, reveal diamagnetic transitions at 4.54K and 3.51K, and find out pure phase of MoSi2, MoS2 and Mo3Si3 .