Nanostructured metals and alloys have been the subject of considerable scientific and technological interest, as a result of their potential in structural and other applications. However, inspection of the scientific literature reveals that only limited work has been reported on nanocrystalline Ti Alloys. The objective of this research is to study the synthesis and characterization of nanocrystalline Ti alloys using a cryomilling technique. The effects of cryomilling parameters, such as milling time and ball to powder ratio, on the synthesis and structure of cryomilled Ti powders were investigated using XRD, DSC, and SEM. The experiment results show that nanocrystalline Ti powders with a grain size of about 16-20nm can be prepared using the cryomilling technique. The grain size and particle size of cryomilled Ti powders decrease with increasing cryomilling time. Compared to the ball milling using a SPEX mill at room temperature, the cryomilling technique leads to less contamination of oxygen, nitrogen and iron in the cryomilled Ti powder.