Optimal Hydrofluoric Acid Etching Duration and Impact of Silane/Adhesive on Profilometric Properties and Bonding to Lithium Disilicate Glass Ceramics.

Objectives: This study aimed to assess the surface roughness, surface free energy (SFE), and shear bond strength (SBS) on a lithium disilicate glass-ceramic surface following varying etching protocols (time variation) and application of silane either with or without adhesive material.

Methods and materials: Lithium disilicate glassceramic (LDGC) computer-aided design and computer-aided manufacture (CAD/CAM) blocks were cut using a slow-speed cutting mechanism. CAD/CAM blocks were then evaluated for surface roughness, 6 groups (n=20); SFE,12 groups (n=5); and SBS, 10 groups (n=10). The cut CAD/CAM blocks were randomly allocated to 28 groups. Groups were based on the following: 30 or 90 seconds of etching with 9% hydrofluoric acid (HF); application or absence of silane coupling agent (Sil); and application or absence of adhesive (Adh).The control group (Cont) had untreated surfaces. Unetched surfaces were surveyed with only silane (Sil), only adhesive (Adh), or silane+adhesive (SilAdh). Further etched groups were HF30 with HF for 30 seconds, HF30-Sil, HF30-Adh, and HF30-SilAdh. Alternative 90-second etching times produced similar groups: HF90, HF90-Sil, HF90-Adh, and HF90-SilAdh. A digital profilometer was used to assess the surface roughness of specimens, and two readings were recorded. Sessile drop analysis was used to examine SFE specimens, and the OWRK model was modified to measure liquid surface tension. A universal testing machine (UltraTester, Ultradent Products, Inc, South Jordan, UT, USA) was utilized for the SBS test, with the crosshead speed set at 0.5 mm/min until failure. Representative treated specimens from each group were submitted to surface morphological evaluation and chemical analysis using scanning electron microscopy/energy dispersive x-ray spectroscopy (SEM/EDXS) (n=3). After data collection, evaluation using one- or two-way analysis of variance and the post-hoc Tukey test (α=5%) was conducted.

Results: A longer etching time of 90 seconds produced a rougher surface. After the 90-second etching process, SFE displayed the greatest values; nevertheless, the use of silane did not affect SFE. For every group examined, the application of silane followed by adhesive resulted in an increase in SBS and more stable bonding over time. SEM/EDXS showed that etching times did affect the amount of cerium on the surface and altered surface morphology.

Conclusions: Higher and more consistent bond strengths have been observed with longer etching periods. Silane and adhesive application on the ceramic surface showed stronger and enhanced bond strength, specifically when longer etching times were employed.