Synthesized β-SiAlON based on bauxite (Al2O3 in 68wt%) by using combined reduction agents aluminum/carbon, aluminum/silicon were studied. Calculated mass change ratio of the specimens after firing, Examined Phase composition and microstructure of the specimens by using XRD, SEM and EDS, Examined the relative content by using chemical analysis.The results show that: the synthesis mechanism of two combined reduction agents specimens are different, the formation amount of β-SiAlON are different, crystal morphology are not the same, the production costs are different; the end of the reaction temperature are 1500°C, the column β–SiAlONˊz are about 3.