METHODS: Silanated, titanated and pure NBT at 5% were incorporated in PMMA matrix. Neat PMMA matrix served as a control. NBT was sonicated in MMA prior to mixing with the PMMA. Curing was carried out using a water bath at 75°C for 1.5h and then at 100°C for 30min. NBT was characterised via Fourier transform-infrared spectroscopy (FTIR), Transmission Electron Microscopy (TEM) and Brunauer-Emmett-Teller (BET) analysis before and after surface modification. The porosity and fracture toughness of the PMMA nanocomposites (n=6, for each formulation and test) were also evaluated.
RESULTS: NBT was successfully functionalised by the coupling agents. The TCA exhibited the lowest percentage of porosity (0.09%), whereas silane revealed 0.53% porosity. Statistically significant differences in fracture toughness were observed among the fracture toughness values of the tested samples (p<0.05). While the fracture toughness of untreated samples was reduced by 8%, an enhancement of 25% was achieved after titanation. In addition, the fracture toughness of the titanated samples was higher than the silanated ones by 10%.
CONCLUSION: Formation of a monolayer on the surface of TCA enhanced the NBT dispersion, however agglomeration of silanated NBT was observed due to insufficient coverage of NBT surface. Such behaviour led to reducing the porosity level and improving fracture toughness of titanated NBT/PMMA composites. Thus, TCA seemed to be more effective than silane.
CLINICAL SIGNIFICANCE: Minimising the porosity level could have the potential to reduce fungus growth on denture base resin to be hygienically accepTable Such enhancements obtained with Ti-NBT could lead to promotion of the composites' longevity.
METHODS: Different volume percentages of HEMA were tested in four experimental silane-based primer solutions (additions of HEMA: 0, 5.0 vol%, 25.0 vol% and 50.0 vol%). An experimental silane blend (primer) of 1.0 vol% 3-isocyanatopropyltrimethoxysilane (ICMS) + 0.5% bis-1,2-(triethoxysilyl) ethane (BTSE) was prepared and used. The experimental primers together with the control group were applied onto acid-etched premolars for attachment of orthodontic brackets. After artificial aging by thermocycling the shear-bond strength was measured. The fractured surfaces of all specimens were examined under scanning electron microscopy (SEM) to evaluate the failure mode on the enamel surface.
RESULTS: The experimental primers showed the highest shear-bond strength of 21.15 MPa (SD ± 2.70 MPa) and with 25 vol% showed a highly significant increase (P < 0.05) in bond strength. The SEM images showed full penetration of adhesive agents when using silane-based primers. In addition, the SEM images suggested that the predominant failure type was not necessarily the same as for the failure propagation.
CONCLUSIONS: This preliminary study suggested that nonacidic silane-based primers with HEMA addition might be an alternative to for use as adhesion promoting primers.