In this study, the mechanical activation process of the Al-TiO2-H3BO3 thermite mixture was modeled and optimized before self-propagation high-temperature synthesis of Al2O3-TiB2 ceramic composite powders. For this purpose, response surface method in conjunction with full factorial design was conducted for evaluating the experiments and modeling the process. The milling speed and milling time were considered as the process input parameters. In addition, the intensity and temperature of the last exothermic peaks in DSC curves, which correspond to the occurrence of self-propagation high-temperature synthesis process, were chosen as the responses. Analysis of variance was employed for checking the accuracy of the developed models. Furthermore, the effects of milling speed and time on the responses were explored using the developed methods, in detail. The results showed that the models were significant and they predicted the responses accurately. Moreover, the milling time was obtained to be more effective parameter on the responses. The optimized condition for the mechanical activation was 340 rpm and of 17.63 h for milling speed and milling time, respectively.