Pure Al particles reinforced with amorphous-nanocrystalline Cu36Zr48Ag8Al8 particles composite powders were prepared by high-energy milling without and with ethanol. The mechanical milling procedures were compared so that in the case of dry milling the particle size increased owing to cold welding, but the crystallite size decreased below 113 nm. The amorphous phase disappeared and was not developed until 30 h of milling time. Using ethanol as a process control agent, the particle size did not increase, while the amorphous fraction increased to 15 wt.%. Ethanol decomposed to carbon dioxide, water, and ethane. Its addition was necessary to increase the amount of the amorphous structure.