In this study, a nanocrystallite Cu-20Zn-10Al prealloyed powder was produced by mechanical alloying method from elemental powders and nanostructured samples prepared via liquid phase sintering process. The different milling times and process control agents were considered as milling parameters to determine of optimum conditions. The milled powder was investigated by means of X-ray diffraction measurements, scanning electron microscopy, particle size analysis by means of laser technique and simultaneous thermal analysis. Then the milled powder at various milling times was cold compacted at 600 MPa and sintered at different temperatures ranging from 760 to 790 °C according to liquid phase temperature measuring by diffraction thermal analysis. Microstructural characterization, compaction and densification, micro-hardness measurement and X-ray diffraction measurements were conducted from consolidated samples at different sintering temperature and milling times. The results show that a Cu-Zn-Al homogenous supersaturated solid solution with a crystallite size of 2.4 nm (by Stearic acid as PCA) was obtained after 56 h of milling time. Furthermore, the maximum densification occurred at 775 °C with a milling time of 56 h.