In this study, an Al-10 wt-%Al2O3 composite powder prepared by mechanical alloying was investigated at different milling times. To evaluate the effects of the amount of methanol as a process control agent on the characteristics of mechanical alloyed Al-Al2O3 composite powder and the properties of the composite materials, the composite powders and the composite materials have been successfully produced with different amounts of methanol, namely, 1, 2 and 3 wt-%. The composite powders were characterised using scanning electron microscope (SEM), laser particle size analyser, X-ray diffraction analysis and Vickers microhardness test. The milled powders were pressed and sintered under argon gas control. The microstructure of the produced composite was investigated by SEM. The results show that varying amounts of methanol produce considerable effects on the morphology, particle size and structural behaviour of the as milled composite powders. Moreover, different microhardness values were obtained for different amounts of methanol at the same milling time.