Effects of type and concentration of process control agent on characteristics of the nanocrystalline Cu-1Ta nanocomposite during milling and subsequent sintering were investigated. Microstructural analyses showed that addition of stearic acid (SA) into Cu-1Ta mixture was more effective compared to toluene. The results revealed that application of 2% SA provided a significant dissolution of Ta in Cu lattice after milling for 32 h; however, the extended milling encouraged Ta rejection and increased the crystallite size. Reduction of SA to 1% resulted in a narrower crystallite size distribution with mean size of 18.5 nm. The mechanical and physical tests also indicated that addition of 1% SA rather than 2% toluene caused an increase of 33% in electrical conductivity with nearly no change in micro-hardness.