In present study, production of Al/(Al2O3+AlxVy+AlaNib) composite in Al-V2O5-NiO system with thermomechanical activation method has been investigated. For this purpose, the mixing of Al, V2O5 and NiO powders with two different weight fraction (P0: Al-18.9 V2O5-7.9NiO, P1: Al-13.3V2O5-5.6NiO) were grinded and densification was occurred. Differential thermal analysis method was used to investigation of phase transitions. Heat treatments was conducted on the raw comperest silenderical samples due to the peak temperature of the reactions, P0 raw samples heated at temperatures of 725,770 and 950oC and P1 raw samples at temperatures of 725, 830 and 960oC. XRD analysis and the microstructure of the sintered samples at temperature of 960 showed that the phases Al3V, Al23V4, a-Al2O3, Al2V3 in both sample as reinforcement is formed.in this temperature. The difference between P0 and P1 samples is that in the P0, AlNi phase and in P1 Al4Ni3 phase formed. Studies also show that by increasing temperature we have increase in the hardness and density. In P0, hardness and density values in this sample where much more than of P1.