Microstructures of 3 mol% yttria‐stabilized zirconia (3YSZ) with different content of TiN were investigated in this study by XRD, SEM, and TEM. The specimens were hot‐pressing sintered at 1450°C for 2.5 h under 50 MPa in vacuum, and then further characterized on microstructure change and phase distribution. The TiN added to 3YSZ can suppress tetragonal (t) to monoclinic (m)‐3YSZ phase transformations, reduce 3YSZ grain size, and improve its mechanical properties. The ceramic was formed of homogeneously dispersed 3YSZ and TiN grains with average size of 0.7 and 1 μm, respectively. The coexistence of t‐ and m‐phases was observed in one grain, and the nucleation of m‐phase with acicular twin occurred preferentially at grain boundaries of t‐phase. The TEM analysis was focused on the 3YSZ–30 wt% TiN specimens in order to identify the relationships between t‐ and m‐structures, and twin structures of m‐phase. Two crystallographic relations of t‐ to m‐transformation are (100)m//(110)t, [010]m//[001]t in type I, and (100)m//(110)t, [001]m//[001]t in the type II. The acicular (100)m and lathlike (110)m twins in m‐phase were also observed.
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