Ti-Mo-(0~9) Fe alloys were processed by mechanical alloying and subsequent spark plasma sintering (SPS) from elemental powders, and the influences of preparation parameters on the performance of milled powders and sintered alloys were studied. The results show that at the Fe content range of 3~9wt.% titanium based alloys with high density and ultra-fine grain structure can be produced by SPS at 900℃ from the powders milled for 10h. The microstructure of the titanium alloys mainly consists of β-Ti phase matrix and FCC-Ti particles, and the average grain size is in the range of 130~490nm. It is the first time that titanium based alloys with face-centered cubic structure are produced. During mechanical alloying process, the addition of Fe element greatly improves the glass forming ability of the alloy system, and the ability and the volume fraction of amorphous phase in the powders are obviously enhanced as increasing Fe content. After high-energy ball-milling for 10h, amorphous/nanocrystalline Ti-Mo-Fe composite powders are found to exhibit favorable thermostability.