Cu-(2.5 or 5.0vol.%)Al2O3 nanocomposite balls and granules and Cu-(2.5vol.% or 5.0vol.%)Pb alloy powder were prepared by high energy mechanical milling (HEMM) of mixtures of Cu and either Al2O3 or Pb powders. It was observed that with the increase of the content of Al2O3 nanoparticles from 2.5vol.% to 5vol.% in the powder mixture, the product of HEMM changed from hollow balls into granules and the average grain size and microhardness changed from approximately 130nm and 185HV to 100nm and 224HV, respectively. On the other hand, HEMM of Cu–(2.5 or 5.0vol.%) Pb powder mixtures under the same milling conditions failed to consolidate the powder in-situ. Instead, it led to formation of nanostructured fine powders with an average grain size of less than 50nm. Energy dispersive X-ray mapping showed homogenous distribution of Pb in the powder particles in Cu–5vol.%Pb alloy powder produced after 12 hours of milling. With the increase of the Pb content from 2.5 to 5.0 vol.%, the average microhardness of the Cu-Pb alloy powder particles increases from 270 to 285 HV. The mechanisms of the effects are briefly discussed.