A novel biocomposite Ti-35wt%Nb-2.5wt%Sn-15wt%HA powders was synthesized by high energy ball mill(HEBM) for various periods of time. The microstructure and characteristics of the milled powder particles were investigated. Results showed that in the composite powders milled for 4h, Ti was still exhibited primary α phase, with the increase of ball milling time up to 8h, Ti transformed into primary β phase and a little α phase, after ball milling for 12h, Ti transformed into β phase fully. the transform temperature was 380.06°C. And TEM and PSD results indicated that nanostructure was obtained after 12h milling..