Al-42wt%Nb powder was prepared by high-energy mechanical milling(HEMM). The particle size, phase transformation and microstructure of the as-milled powder were investigated by particle size distribution (PSD) analyzer, scanning electron microscopy (SEM), X-ray diffractometery (XRD), transmission electron microscopy (TEM)and differential thermal analysis (DTA). The milled powders were heated to a sintering temperature at 1000C with under vaccum with vaccum tube furnace. Microstructural examination of sintered Ti-42wt%Nb alloy using 4h-milled powder showed Ti-rich phases (α-Ti) which are fine and homogeneously distributed in the matrix (Nb-rich phase: β-Ti). The sintered Ti-42wt%Nb alloy with milled powder showed higher hardness. The microstructure of the as quenched specimens fabricated by sintering using mixed and milled powder almost are same, but the hardness of as quenched specimen fabricated by using mixed powder increased due to solution hardening of Nb in Ti matrix. The aging effect of these specimens on microstructural change and hardening is not prominent.