Nano-sized was in situ synthesized in copper matrix through self-propagating high temperature synthesis (SHS) with high-energy ball milled Ti-B-Cu elemental mixtures as powder precursors. The size of particles in the product of SHS reaction decreases with time of preliminary mechanical treatment ranging from 1 in untreated mixture to 0.1 in mixtures milled for 3 min. Subsequent mechanical treatment of the product of SHS reaction allowed the particles to be reduced down to 30-50 nm. Microstructural change of -Cu nanocomposite during spark plasma sintering (SPS) was also investigated. Under simultaneous action of pressure, temperature and electric current, titanium diboride nanoparticles distributed in copper matrix move, agglomerate and form a interpenetrating phase composite with a fine-grained skeleton.