Effects of some chemical surface modifications on resin zirconia adhesion

Objectives To evaluate the effects of various chemical surface modifications on adhesion between zirconia and resin adhesive. Material and methods Pre-sintered zirconia discs were sectioned from commercial cylindrical blocks and polished with abrasive papers under running tap water. All the discs were randomly divided into five study groups according to the methods of surface treatment, including: the control group (fully sintered, without any modification), group S (fully sintered and sandblasted with silica coated alumina particles), group HN (fully sintered and etched with a blend of mineral acid solution at 100 °C for 25 min), group HF (fully sintered and etched with 48% hydrofluoric acid solution at 100 °C for 25 min), and group Si (coated with silica particles and then fully sintered). The mean value of surface roughness was evaluated before further treatment. Resin stubs (3.6mm in diameter and 3mm in height) were adhered and light cured on each zirconia disc after the application of a silane coupling agent. In each group, all the samples were further divided into three subgroups with each n=12, one for the measurement of initial adhesion strength (shear bond) value and the other two were tested after thermal cycling for 10,000 and 20,000 cycles, respectively. The results were analyzed with two-way ANOVA and Turkey HSD (p<0.05). XRD technique was utilized in the examination of zirconia surface crystallinity. The morphological appearance of zirconia surface after surface treatment was observed with SEM. Results The control group showed the lowest initial shear bond strength (SBS) value (16.8 ± 2.4 MPa) and did not survive the aging treatments. All the investigated surface treatments improved resin zirconia bond strength significantly, the group S displaying the highest initial value of 25.1 ± 2.7 MPa. However, the highest resistance to the aging effects of thermal cycling was found in group Si. It was further shown in the XRD examination that only the grit-blasting caused the crystalline transformation from tetragonal phase to monoclinic phase (T → M). On the other hand, such a phase transformation could not be detected in all the other four groups. Significance Resin zirconia adhesion could be effectively improved by both HF etching and silica coating on zirconia surface, without leading to a T → M crystalline phase transformation.