Fine, pure gamma-AlON powders have been synthesized by a combinational method. The method was based on the weight change between the reactant (Al2O3) and the resultant (AlN) in a carbothermal reduction (CR) reaction. It combined the advantages of CR method and solid-state reaction method, and overcame their disadvantages. Sucrose was used as the reducer instead of carbon black. Compared with carbon black, sucrose was more effective in nitridation and hindering the agglomeration of powders.