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A simple method for synthesis of β-SiAlON powder by nitridation of alumina–silica gel in ammonia was provided. Precursor was obtained from a mixture of nanosized alumina and colloidal silica. Nitridation reactions took place at 1100°C and conversion to β-SiAlON was achieved at 1300°C for 2–3 h. The synthesized β-SiAlON powder was nanocrystalline in size (<100 nm).