Nb, Al, Ti, C and B powders were mechanically alloyed(MA) in an Ar gas atmosphere. The results of X-ray diffraction indicated that for the starting composition of Nb₃Al, Nb solid solution was obtained in the early stage of MA process, thereafter it became to be amorphous. Nb₃Al compound was obtained by vacuum heating of 72.0ks MA powders. Nb₃Al and TiC were obtained in the system of the composition of Nb₃Al-30vol%TiC by vacuum heating of 72.0ks MA powders. Furthermore, fine TiC particle dispersed Nb₃Al composite was obtained by HIP processing of MA powders. TEM observation of the HIPed compacts revealed that TiC, which was more less than 0.1μm, precipitated on fine grained Nb₃Al matrix.