In the present investigation on the preparation of CuO doped Al2O3 nanoparticles using high energy ball-milling. Copper oxide (CuO) belongs to the monoclinic crystal system, aluminium oxide (Al₂O₃) belongs to the trigonal crystal system. Copper oxide is low melting and boiling point to compare aluminium oxide. CuO 90%- Al₂O₃ 10% doped new alloy prepared by ball milling technique and heat treatment for furnace in 500°c. The CuO-Al₂O₃ doped nano-materials characterized by UV-visible spectroscopy for optical band gap, SEM for the surface and X-RD to calculate the crystalline size and the lattice distortion.