Aluminium nitride (AlN) powder has been produced through carbothermal synthesis of alumina (Al2O3) powder acid carbon. TEM is used to identify the nano-sized AlN grains that initiate on the surface of the Al2O3 grains during the first stage of the carbothermal synthesis cycle and to characterize the final product. Magic Angle Spinning NMR is coupled with TEM to identify the reaction sequence for the formation of the AlN.