An Al-5vol%Ti3SiC2 nanocomposite has been prepared by ball milling technique. Steel ball, agate ball and zirconia ball were selected during the ball milling process and then the microstructure evolution of the powder mixture was investigated. The homogenous fine mixed powder can be obtained with zirconia ball, whereas the conglomeration will be formed in the case of steel ball and agate ball. The bulk Al/Ti3SiC2 nanocomposite was fabricated by hot pressing technique. The effects of the particle size and agglomerate state of Ti3SiC2, as well as the microstructure of Al/Ti3SiC2 nanocomposite were studied by SEM and TEM. It was found that the nanosized Ti3SiC2 particle could be obtained during the ball milling process and distributed in aluminium homogenously.