Silane reactivity and resin bond strength to lithium disilicate ceramic surfaces

Abstract

Objective: To evaluate the silane status in commercially available products and their bonding capacity with polished glass-ceramic surfaces before and after hydrofluoric (HF) acid-etching.

Methods: The products tested were Calibra Silane Coupling Agent/CS, G-Multi Primer/GM, Kerr Silane Primer/KS, Monobond Plus/MB and Scotchbond Universal Adhesive/SB. The silane status was studied by ¹³C nuclear magnetic resonance spectroscopy (¹³C-NMR). The roughness parameters of polished (group A) and HF acid-etched (group B) lithium disilicate glass-ceramic surfaces were measured by optical profilometry (n = 5/group). The interaction of the products with group A and B ceramic surfaces was examined by attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR). The shear strength (SBS) of a flowable composite bonded to the ceramic surfaces (groups A, B) was assessed before (NS) and after silane treatment (n = 20/group, product).

Results: The NMR analysis showed the presence of silanol monomers only in CS. Methoxylated-siloxane adducts were found in GM, silanol-siloxane adducts in MB, SB, and siloxane polymers in KS. Acid-etching greatly increased Sa, Sz, Sdr, Sc and Sv parameters (p < 0.001) and ATR-FTIR analysis demonstrated evidence of bonding with the substrate in CS. Weibull analysis of SBS revealed the following rankings in characteristic life (p < 0.05): CS > SB,KS,MB > GM > NS (group A) and CS > GM > SB,KS,MB,NS (group B). The most reliable treatment in both groups was CS. For the same silane treatment, the SBS of group B were significantly higher from group A. Failures were mainly of adhesive type, except of several partial resin cohesive failures found in group B.

Significance: The chemical bonding capacity of the silanes was highest in products with silanol monomers. Acid-etching increased bond strength to a level that neutralized the silane contribution in products with silanol-siloxane adducts and siloxane polymers, providing thus bond strength values similar to silane-free treatments.

Keywords: Ceramic roughness; Glass ceramic; IR; NMR; Resin bonding; Silane reactivity.