OBJECTIVE

To investigate the effect of silane contents on their chemical interaction with 10-methacryloyloxydecyl-dihydrogen phosphate (MDP), and affecting the bonding of MDP to zirconia by time-of-flight secondary ion mass spectrometry (TOF-SIMS) and solid-state nuclear magnetic resonance (SSNMR) spectroscopy.

METHODS

Zirconia (Cercon ht, Dentsply) slabs were prepared and fully sintered. Experimental primers SE-5 and SE-10 were formulated by adding 5 wt% and 10 wt% γ-methacryloxypropyltrimethoxysilane to an MDP-based primer SE BOND (SE), respectively. SE, SE-5, and SE-10 were applied on the assigned zirconia slabs. The chemical compositions on the surface and adhesive interfaces were examined by TOF-SIMS in a depth-profiling mode. Hydrophilicity and resin affinity of treated zirconia were analyzed. The bond strengths to resin cylinder were examined either after 24-h storage or thermocycles. In addition, zirconia powders treated with three primers were assessed by SSNMR spectrometry for the adsorption of MDP.

RESULTS

TOF-SIMS analysis showed that SE treatment generated the greatest amount of P-O-Zr related ions, which reduced in SE-5 and SE-10 groups. The 3D ion-images illustrated the generation of ZrO(OH) ions with silane contents. The SSNMR analysis revealed that the chemical bonding was mainly P-O-Zr ionic bonds in SE but shifted to P-OH-Zr hydrogen bonds in SE-5 and SE-10. SE-5 and SE-10 treated zirconia presented higher hydrophilicity and affinity to resin compared to Zr did. SE showed the highest initial bond strength which significantly decreased after thermocycling.

SIGNIFICANCE

MDP adsorption onto zirconia via P-O-Zr ionic bond promotes bonding with resin. The silane enhances the hydroxylation of zirconia and impairs the adsorption of MDP, but does not adversely affect the bond durability.