Al/CuO multilayer films were deposited with magnetron sputtering process and analysed with differential scanning calorimetry (DSC). Results show that the reduction-oxidation may happen. The chemical reaction heat is about 1197.5 kJ·mol-¹. The activation energy of the second reaction calculated by Kissinger equation is about 565.146 kJ·mol-¹. Because of the high activation energy, Al/CuO multilayer films can be conserved for a long time. The process of the reaction between films is composed of two steps and the highest temperature of the reaction is 2573 ℃.temperature of the reaction is 2573 ℃.