The feasibility of synthesizing MgSiN2 powders through combustion synthesis process is demonstrated. A self-sustained combustion wave can be initiated with or without the addition of active diluent. The wave propagation resulted in a product with several secondary phases in addition to the main phase MgSiN2 when the combustion reaction was initiated without the addition of active diluent. As the active diluent was used in the reactant mixtures, the amounts of the secondary phases were decreased. The effect of active diluent addition on the phase composition and morphology of the final product was discussed. Furthermore, the use of MgSiN2 crystal seeds in the reactant mixtures was also investigated. It is found that the active diluent can facilitate the nitridation reaction. The experimental results showed that changing the experimental parameters such as the amount of active diluent and the MgSiN2 crystal seeds could optimize the fabrication of MgSiN2 powders through combustion synthesis process.