β-Sialon/ZrN/ZrON composites were successfully fabricated by an in-situ carbothermal reduction？nitridation process with fly ash, zircon and active carbon as raw materials. The effects of raw materials composition and holding time on synthesis process were investigated, and the formation process of the composites was also discussed. The phase composition and microstructure of the composites were characterized by means of XRD and SEM. It was found that increasing carbon content in a sample and holding time could promote the formation of β-Sialon, ZrN and ZrON. The proper processing parameters to synthesize β-Sialon/ZrN/ZrON composites were mass ratio of zircon to fly ash to active carbon of 49：100：100, synthesis temperature of 1550 °C and holding time of 15 h. The average grain size ofβ-Sialon and ZrN（ZrON） synthesized at 1550 °C for 15 h reached about 2 and 1μm, respectively. The fabrication process ofβ-Sialon/ZrN/ZrON composites included the formation ofβ-Sialon and ZrO2 as well as the conversion of ZrO2 to ZrN and ZrON.
