In this work, the experimental results obtained during the preparation of Al-Ni and Al-Ni-Mg alloys using the aluminothermic reduction of NiO by submerged powder injection, assisted with mechanical agitation are presented and discussed. The analyzed variables were melt temperature, agitation speed, and initial magnesium concentration in the molten alloy. For some of the experiments performed, it was found that the Ni concentration increased from 0 to about 3 wt-% after 90 min of treatment at constant temperature and constant agitation speed. In order to determine the values of the kinetic parameters of interest, such as the activation energy and the rate constants, the values of the results obtained were fitted to the kinetic formulae available. Moreover, the kinetics of the reaction were found to be governed by the diffusion of Al and Mg to the NiO boundary layer, where MgAl2O4 or Al2O3 were formed as the main reaction products. Finally, from a thermodynamic study of the system, the main reactions that took place are explained.