In order to reveal the effect of vacuum treatment and Ti content on the properties and microstructure of Mo-0.1Zr alloy, Mo-0.1Zr and Mo-0.1Zr-nTi (n=0.4, 0.55, 0.7 and 0.9) alloys were prepared via powder metallurgy processes and final vacuum treatment was adopted. The result shows that the mechanical properties of Mo-0.1Zr alloy were enhanced greatly by the vacuum treatment, especially the elongation of the alloy (25.6%), much higher than that of the forged Mo alloys. Simultaneously, obvious transgranular fracture was observed on the fracture surface after vacuum treatment instead of the intergranular fracture. It induces the generation of (Mo,Ti)xOy second-phase particles by adding element Ti into the Mo-0.1Zr alloy, which exists in the grain boundaries. With the increase of Ti content, the amount of second-phase particles increases and leads to the reduction of mechanical properties of the alloys