were synthesised from high aluminium fly ash by using a carbothermal reduction-nitridation process. The effects of temperature and the addition of carbon black on the phase compositions and morphologies have been investigated using X-ray diffraction (XRD) and scanning electron microscopy (SEM). Thermodynamic analysis has been used to study phase transformations. For the sample with the stoichiometric carbon black content, the product formed at 1500uC was single phase short prismatic Si 3 Al 3 O 3 N 5 . The products at 1600uC were Ca-a-Sialon accompanied by AlN, whereas at 1700uC, Si 4 Al 2 O 2 N 6 and SiAl 4 O 2 N 4 formed. Increasing the carbon black at 1500uC, Si 3 Al 3 O 3 N 5 , b-SiC, 15R and Fe x Si were produced as reaction products.