In this paper,thermogravimetry/differential scanning calorimetry(TG/DSC) and XPS were used to characterize the thermo-reaction properties of nanometer aluminum powders and micro-aluminum under air,Ar and O2.The different oxidation conditions of these two kinds of powders were studied.The experimental results confirm the difference of thermo-reaction properties between nanometer aluminum powders and micrometer aluminum.Nanometer aluminum powders would not be oxidized under 550℃,and micrometer aluminum would not be oxidized markedly till 1000℃ at atmosphere.