Aluminum powder with different C and C–Cu mixtures powders were fabricated by powder metallurgy, using high-energy mechanical milling as a pre-treatment of powders. To evaluate the combined effect of the C–Cu mixture and the process conditions, such as sintering temperature/time and milling time, on the yield stress and hardness, two experimental designs were carried out. The results were analyzed with Minitab Statistical Software using contour plots. From the results, better mechanical properties were found at a Cu/C ratio of 0.33 and samples with high C content (3 wt. %). In samples subject to long sintering time (3 h), the mechanism of precipitation of the second phase was mainly present, resulting in an improvement in mechanical properties. From the difference found between the elastic limit and the microhardness tests, it was found that there was an inefficient sintering process affecting the elastic limit test results. Additionally, X-ray analyses using the Rietveld program, were used for microstructural characterization and mechanical parameters of yield strength and ultimate tensile strength.