Surface characterization of indirect restorative materials submitted to different etching protocols

Abstract

Objectives: This in vitro study aimed to evaluate the effect of different times and concentrations of hydrofluoric acid etching on the surface of indirect restorative materials obtained from blocks used in CAD-CAM technology.

Methods: Specimens (4 mm × 4 mm × 0.8 mm) were obtained for each indirect restorative material: zirconia-reinforced lithium monosilicate ceramic (Celtra Duo), nanoceramic resin (Lava Ultimate), and polymer-infiltrated ceramic network material (Vita Enamic). The materials were submitted to etching with 5% or 10% hydrofluoric acid for 20, 40, 60, or 90 s. A control group for each material was evaluated without any surface treatment, totaling nine experimental groups for each material (n = 10). The specimens were evaluated for surface roughness (R_a and R_z), confocal optical microscopy, the contact angle (θ), surface free energy (γs), total free interaction energy (∆G) using a goniometer, and microshear bond strength to resin cement. Specimen images were obtained using scanning electron microscopy, confocal optical microscopy, and atomic force microscopy. Data on the surface roughness, the contact angle, surface free energy, total free interaction energy, and bond strength were subjected to two-way ANOVA and Tukey´s test (α=0.05).

Results: In general, Celtra Duo showed better results after etching with 10% hydrofluoric acid for 40 or 60 s. Lava Ultimate showed better performance after etching with 10% hydrofluoric acid for 20 or 40 s, whereas Vita Enamic showed better results after etching with 5% hydrofluoric acid for 90 s.

Conclusion: Each material showed different characteristics after etching with hydrofluoric acid. Knowledge of the proper protocol for each material is essential to ensure improvements in the adhesion process and durability of indirect restorations. In general, Celtra Duo presented mechanical properties superior to those of Lava Ultimate and Vita Enamic.

Clinical significance: Specific etching protocols must be recommended for each indirect material because longer exposure to hydrofluoric acid can jeopardize the surface, thus affecting the mechanical and bond strength properties.

Keywords: Bond strength; Hydrofluoric acid; Microscopy atomic force; Microscopy electron scanning; Surface properties.