Characteristic fatigue strength and reliability of dental glass-ceramics: Effect of distinct surface treatments – Hydrofluoric acid etching and silane treatment vs one-step self-etching ceramic primer

Abstract

The aim of this study was to mechanically characterize through flexural fatigue test two CAD-CAM glass-ceramics according to distinct surface etching protocols. To do so, feldspathic (FELD) and lithium disilicate (LD) glass ceramics were subjected to different surface treatments: (1) control – no treatment (Ctrl); (2) conventional protocol etching with 5% hydrofluoric acid followed by silane coupling agent application (HF + SIL; Monobond N, Ivoclar); or (3) using a self-etching ceramic primer (E&P; Monobond Etch & Prime, Ivoclar). Ceramic discs (N = 120; Ø = 12 mm; thickness = 1.2 mm) were produced from CAD-CAM blocks, with 60 being from FELD (VITABLOCS Mark II, Vita Zahnfabrik) and 60 from LD (IPS e.max CAD, Ivoclar). Next, 20 disks of each ceramic were allocated into three groups: Ctrl, HF + SIL, or E&P. Surface roughness data were collected on all samples before and after surface treatments (except for Ctrl). Cyclic fatigue (n = 15) biaxial flexural strength tests were performed by the piston-on-three-balls geometry (ISO 6872) considering the test parameters established from a monotonic test (n = 5). The monotonic test was carried out at a 1 mm/min loading rate and 500 kgf loading cell until fracture to obtain the failure data. The cyclic fatigue test was executed underwater at a frequency up to 20 Hz, with the first stress being 25% of the monotonic test for 5000 cycles, followed by increments of 5% of the monotonic test at each step of 10,000 cycles until failure (fracture). Complementary fractography, topography and Atomic Force Microscopy (AFM) analyses were performed. Characteristic Fatigue Strength (CFS) and Weibull modulus were analyzed by Weibull analysis using the fatigue test data. Roughness and complementary analysis data were analyzed by one-way ANOVA. The statistical results exhibited similar CFS among Ctrl, HF + SIL and E&P for both glass-ceramics. The survival analysis corroborates the findings, however the Weibull modulus pointed out superior structural reliability of FELD treated with the E&P group compared to HF + SIL. According to the complementary analyses, HF + SIL exhibited a higher surface area than E&P and Ctrl for FELD (p = 0.001). Roughness showed statistically significant differences among conditions for FELD (E&P < Ctrl = HF + SIL; p < 0.05) and no difference for LD (p > 0.05). Therefore, the CFS were not influenced by any condition evaluated for FELD and LD glass-ceramics; however, superior structural reliability (higher Weibull modulus) for the feldspathic ceramic treated with the E&P was observed.