In this study, in-situ Al2O3p/Al composite was prepared by the exothermic dispersion method from Al-calcined kaolin system. Thermodynamic analysis was carried out by calculating Gibbs free energy. The reaction kinetics of the system was studied by differential scanning calorimetry and Kissinger equation. The effects of heating temperature and holding time on the microstructure of the composites were analysed. The results showed that the reaction activation energy of the system continued to increase with the progress of the reaction. With the extension of the reaction time at 800°C, the particle size of Al2O3 increased slowly. When the holding time was 50 min, the density and hardness of the composite material were 2.7 g cm−3 and 64HV respectively.