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β‐Sialon materials are synthesized by nitriding reduction reaction using secondary aluminum dross and Si powder as the raw materials. The results indicate that the phases of products are stratified, in which the lower layer is pure β‐Sialon and the upper layer is mainly β‐Sialon, Al2O3 and spinel. This is caused by the transformation of the Si powder from solid to liquid phase and the metal oxide...