? 2022 Elsevier Ltd and Techna Group S.r.l.Si3N4 ceramics were prepared using novel two-step sintering method by mixing α-Si3N4 as raw material with nanoscale Y2O3–MgO via Y(NO3)3 and Mg(NO3)2 solutions. Si3N4 composite powders with in situ uniformly distributed Y2O3–MgO were obtained through solid–liquid (SL) mixing route. Two-step sintering method consisted of pre-deoxidization at low temperature via volatilization of in situ-formed MgSiO3 and densification at high temperature. Variations in O, Y, and Mg contents in Si3N4–Y2O3–MgO during first sintering step are discussed. O and Mg contents decreased with increasing temperature because SiO2 on Si3N4 surface reacted with MgO to form low-melting-point MgSiO3 compound, which is prone to volatilize at high temperature. By contrast, Y content hardly changed due to high-temperature stability of Y–Si–O–N quaternary compound. In the second sintering step, skeleton body was densified, and the formation of Y2Si3O3N4 secondary phase occurred simultaneously. Two-step sintered Si3N4 ceramics had lower total oxygen content (1.85 wt) than one-step sintered Si3N4 ceramics (2.51 wt). Therefore, flexural strength (812 MPa), thermal conductivity (92.1 W/m·K), and fracture toughness (7.6 MPa?m1/2) of Si3N4 ceramics prepared via two-step sintering increased by 28.7, 16.9, and 31.6, respectively, compared with those of one-step sintered Si3N4 ceramics.
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