Gamma aluminum oxynitride (γ-AlON) with a cubic spinel structure is a stable solid solution of Al 2 O 3 -AlN system, which has been attracted much attention in recent decades. 1,2 Transparency of AlON fully dense specimen is in the wavelength range of about 0.2-5 μm. 3 AlON is appropriate for phosphor-converted white LED, light-emitting devices, load-bearing orthopedic, and ceramic semiconductors because of its excellent optical properties besides high hardness and strength. AlON can be used instead of sapphire with a lower price, for applications that excellent mechanical and optical properties are needed. [4][5][6] Carbothermal reduction and nitridation (CRN) method is the most applied technique for AlON fabrication comparing to the other methods. The first report of using the CRN method was published by Yamaguchi et al. in 1959. 6,7 This method needs simple equipment, cheaper raw materials compared to the solid phase reaction, and the final product of this technique has a uniform chemical composition in terms of stoichiometry. 6,8 Remained carbon content in the final product and various effective factors, which can hardly be controlled, are disadvantages of this method. When the CRN method uses as a single-step process, before producing enough amounts of AlN beside α-Al 2 O 3 , a large part of the AlO 2 gaseous species exists because of the high temperature (more than 1800°C) of synthesis. This results in an excessive reduction of Al 2 O 3 phase amount, and consequently, the AlN phase presents in the final product. 9,10 The main reaction of twostep CRN technique corresponds to reaction (1):This main reaction consists of two sub-reactions, which in the first step, γ-Al 2 O 3 reacts with carbon and nitrogen; accordingly, AlN is produced. In the second step, α-Al 2 O 3 reacts with AlN and AlON is fabricated as the final product. 6,11 (1) 64 + x 3 Al 2 O 3 + 3xC + xN 2 → 2Al 64+x 3 O 32−x N x + 3xCO