Effect of fatigue on fracture toughness and phase transformation of Y-TZP ceramics by X-ray diffraction and Raman spectroscopy.

The aim of this study was to evaluate the effect of fatigue on fracture toughness and phase transformation of yttria-stabilized zirconia polycrystal materials (Cercon and Lava). The specimens were tested for indentation fracture toughness either with or without being subjected to fatigue (20,000 cycles, 2 Hz, 200 N load). X-ray diffraction (XRD) analysis was used to examine the phase composition of specimens. The indentation images were analyzed using Raman spectroscopy at indentation center (p1), indentation corner (p2), points on crack 100 μm (p3), and 200 μm (p4) away from the corner and a point ∼80 μm away from the crack (p5). Fracture toughness results were statistically analyzed by two-way analysis of variance (ANOVA); XRD and Raman spectroscopy results were analyzed by three-way ANOVA. Fracture toughness of Cercon control (CC) and fatigue (CF) groups were 6.8 and 6.9 MPa√m, respectively, with no significant difference (p > 0.01). Fracture toughness of Lava fatigue (LF; 7.3 MPa√m) was significantly higher than Lava control (LC; p < 0.01). XRD analyses showed CC and LC consisted of tetragonal zirconia, monoclinic zirconia detected after fatigue. After indentation, relative amount of monoclinic phase significantly increased in CC, CF, and LC; decreased in LF. The Raman spectroscopy results indicated that monoclinic fraction was the highest at p2, subsequently at p1 and decreased at p3, p4, and p5 for all groups. Mechanical cycling increased fracture toughness of Cercon and Lava, the second being significant. Phase transformation was also detected after fatigue, which is higher in Lava. Analysis of indentations showed that transformation was highest was at the corner, second at center.