β-Sialon based composites were produced using a vertical reactor by carbothermal reduction reaction under nitrogen using fly ash and lignite chars to examine the effects of mixing, carbon content, reaction temperature and sintering time. The influences of chars as a reductant were further investigated in comparison with graphite. The evolution of phase and morphology in samples were analyzed by X-ray diffraction (XRD) and scanning electron microscope (SEM). Mechanical stirring was favored to mix fly ash and chars, while ball-milling shove the chars with porous structure due to collisions of agate balls, preventing N₂ penetration to the inner parts of reactants. When excess carbon was increased to 100%, a higher combustion reactivity of low-temperature chars resulted in the production of SiC phase. The evolution of β-Sialon with increasing reaction temperature showed the samples mixed with chars were more sensitive to reaction temperature than that with graphite. β-Sialon phase increased gradually with increasing sintering time to 6 h and decreased thereafter due to the decomposition or conversion of β-Sialon. These changes were more significantly for samples adding lignite chars. The optimal operation has been determined and rod-like β-Sialon whiskers with high aspect ratio appeared after performing the operation. In the growth process of whiskers, bead-shape whiskers were observed, suggesting that the growth mechanism was different from the conventional vaporliquidsolid (VLS) mechanism.
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