Mixed micron-sized Cu/Ti3SiC2 (vol5%) powder was mechanically milled using agate balls and zirconia balls separately. Then followed an examination of it with the FEI-SEM. The experimental results show that, distributed homogenously in Cu matrix, the Ti3SiC2 particles have a size of about 30-50 nm after milled with agate balls for 8 h, while it remains approximately unchanged after milled with zirconia balls. The microstructure of the mixture at different ball-milling stages was also studied. Bulks of Cu/Ti3SiC2 nano-composite were fabricated by hot pressing nano-sized Cu/Ti3SiC2 powder at the temperature of 1 073 K under 100 MPa. Then came an investigation of the effects of the particle size and agglomerate state of Ti3SiC2 as well as the microstructure of Cu/Ti3SiC2 nano-composite. It was found that the nano-sized Ti3SiC2 particles distribute evenly in copper.