Pre-sintering pigmentation techniques do not affect the fatigue behavior of adhesively luted 4YSZ restorations

This study aims to characterize the effect of shading techniques on the fatigue behavior of a 4YSZ ceramic (4 mol% yttrium stabilized zirconia) adhesively bonded to a dentin analogue (fiber-reinforced epoxy resin). 4YSZ ceramic discs (IPS e.max ZirCAD, Ø = 10 mm and 1 mm of thickness) were allocated according to the factor 'shading technique' into 4 groups: Brush- unshaded ceramic disc (IPS e.max ZirCAD BL) pigmented at the pre-sintered stage with pigment solution applied manually using a round liner brush; Immersion- unshaded ceramic disc pigmented through immersion in the solution for 1 s on only one side of the ceramic disc; Manufacturer- specimens already shaded by the manufacturer (IPS e.max ZirCAD MT A2 - Manufacturer group); Control- a control condition with absence of pigment (i.e. non-pigmented specimens). The specimens were sintered and a spectrophotometer (SP60, EX- Rite) was used to ensure that the same perceived color (i.e. pigment saturation) was achieved in the different shading strategies (Manufacturer, Brush or Immersion groups). To do so, the color differences (ΔE₀₀) were calculated using the CIEDE 2000 equation; and an ΔE₀₀ of up to 1.77 was considered as an acceptability threshold. Dentin analogue discs were obtained (Ø = 10 mm and 2.5 mm of thickness) and randomly allocated into pairs with the 4YSZ ceramic discs. Next, the pairs were adhesively bonded using a resin cement (Multilink N). The bonded assemblies (n = 15) were tested for fatigue using the step-stress test method (frequency of 20 Hz; 10,000 cycles per step, initial load 200 N; step-size of 100 N, up to 700 N; and after, step-size of 50 N, until specimen failure/fracture or radial cracks). Fatigue failure load (FFL) and number of cycles for failure (CFF) were recorded for statistical analysis. Fractographic features were accessed, and complementary roughness, topography, grain size and phase content analyses were performed. No statistical differences were observed in the fatigue behavior among the non-shaded condition (Control group - 880 N) and the shaded specimens (Manufacturer - 887 N, Brush - 820 N, and Immersion - 850 N groups; p > 0.05). However, the use of a brush shading technique induced slightly inferior fatigue mechanical behavior of the restorative set compared to the specimens already shaded by the manufacturer (p = 0.027). No differences in Weibull modulus were observed among the tested groups. The specimens pigmented by the brush technique demonstrated a rougher surface, with statistically higher Rz values, in addition to a larger grain size in comparison to all other conditions (p< 0.05). No m-phase content was identified (only t and c phases were detected). Thus, the shading techniques used to provide a Vita classic A2 shade does not negatively affect the mechanical fatigue properties of a bonded 4YSZ ceramic. However, the brush technique has detrimental effect on the fatigue behavior compared to when the ceramic was already provided in a shaded format by its manufacturer.