The mechanical alloying behavior of elemetal powders in the V-Al and V-Al-Zr systems was examined. The effects of milling time on the phase and particle size of powder has been thoroughly studied. For mechanical alloying, SPEX mixed/mill has been used. The milling time of V-Al and additional Zr are varied to find the optimum condition of forming amorphous phase. The X-ray diffraction pattern, microstructure detection and microhardness test are carried out to analyze the MA products. The procedure of mechanical alloying is as follows ; initial state-welding-equiaxed particle formation-random welding orientation-steady state. When the final step is reached, no lamellar-structures detected. The steady state condition is observed after 10 hours and 12 hours milling for V-Al and V-Al-Zr alloy, respectively. The microhardness continuosly increase up to 10 hours and 12 hours after then it remains constant. At 48 hours milling for V-Al alloy, the forms of amorphous phase is observed from X-ray diffraction pattern and transmission electron micrograph.