Aluminium-based alloys have wide applications but little is known about the thermalchemical kinetics of nanoalloys. This work investigated the thermal oxidation of Zn and Al nanoalloys (nAlZn) with a BET equivalent diameter of 141 nm through the simultaneous TGA/DSC method. The thermal analysis was combined with elemental, morphology and crystalline structure analysis to elucidate the reaction mechanisms. It was found that the complete oxidation of nAlZn in air can be characterised by a three-stage process, including two endothermic and three exothermic reactions. With the help of ex-situ XRD, different reaction pathways were proposed for different stages, forming the end products of ZnO and ZnAl 2 O 4 . The reactivity comparison between Al and nAlZn suggested that different criteria should be used for different applications.