This paper describes the spark plasma sintering (SPS) of Y-and Ca-α/β-SiAlON powders synthesized by salt-assisted combustion at temperatures of 1600 °C with different holding times. X-ray diffraction reveals that with increasing holding time, the α to β transformation ratio of Y-α-SiAlON becomes greater than that of Ca-α-SiAlON.Nevertheless, all samples effectively reach their theoretical density after sintering. The Vickers hardness measured with an applied load of 19.614 (2.0 kg) decreases with a decreasing amount of α-SiAlON, with a maximum value of 19.4 GPa being achieved in Ca-α/β-SiAlON with an α-SiAlON content of 55%.