Abstract In this research, the effect of aluminothermic reaction on the progress of carbothermic reaction in simultaneous mechanochemical reduction of CuO and ZnO has been studied. A mixture of CuO and ZnO powders along with different amounts of aluminum and graphite was milled in a planetary ball-milling machine. The adiabatic temperature and overall reaction enthalpy were varied by changing the aluminum/carbon ratio. The results showed that by increasing the amount of aluminum, the exothermic aluminothermic reaction provided the required heat for the endothermic carbothermic reactions. Consequently the oxide powders were entirely reduced during ball-milling process and α-brass–Al2O3 nanostructured composites were obtained. X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used to characterize the final products. By utilizing the Scherrer\\\\\\\'s method, the mean grain size of the products was calculated to be in the nanometer range, further confirmed by TEM observations.

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