Fiber post bonding with beta-tricalcium phosphate incorporated root dentin adhesive. SEM, EDX, FTIR, rheometric and bond strength study.

The aim was to formulate an experimental adhesive (EA) and added nanoparticles (NPs) of beta-tricalcium phosphate (ß-TCP) to see the impact on pushout bond strength (PBS) and other mechanical properties. Three adhesives were prepared, including EA (control, without ß-TCP NPs), 2.5%-ß-TCP NPs containing adhesive (2.5%-NPA), and 5% ß-TCP NPs containing adhesive (5%-NPA). For the characterization of the NPs, scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy was accomplished. For the adhesive's characterization, rheological assessment, and degree of conversion (DC) analysis were performed. PBS of these adhesives against resin fiber post to root dentin, interfacial failure categories, and resin dentin interface analysis were also assessed. The ß-TCP NPs were seen as agglomerated asymmetrical particles on SEM. These NPs were composed primarily of calcium (Ca), and phosphorus (P). Rheological evaluation of the adhesive's showed a drop in the viscosity of all adhesives at greater angular frequencies. The greatest DC was detected for the EA group (67.54 ± 7.9) followed by 2.5%-NPA group (45.32 ± 5.1), whereas the lowest DC values were seen for the 5%-NPA group (38.97 ± 6.5). Concerning PBS, the 2.5%-NPA revealed the highest values at the coronal (12.81 ± 3.0) and middle (8.50 ± 2.3) sections, whereas, for the apical section, the highest PBS values were seen for the 5%-NPA (4.9 ± 1.6). Most of the failures for all adhesive groups were seen at the adhesive-dentin interface (cohesive type failures) for all root segments (coronal, middle, and apical). The resin-dentin interface analysis verified hybrid layer and resin tag formation for all adhesives, but the presence of dispersed ß-TCP NPs was only seen in the two NP-reinforced adhesives. The adding of ß-TCP NPs in the adhesive could be beneficial as it could improve its PBS. Suitable rheological properties and dentin interaction were also observed for NP-reinforced adhesives. A reduced DC was seen for both ß-TCP NP-containing adhesives as compared to the EA. RESEARCH HIGHLIGHTS: Experimental adhesives were reinforced with beta-tricalcium phosphate (ß-TCP) nanocrystals. The ß-TCP NPs were seen as agglomerated asymmetrical particles on SEM. These NPs were composed primarily of calcium (Ca), and phosphorus (P). ß-TCP adhesives demonstrated superior pushout bond strength and a drop in the adhesive viscosity at greater angular frequencies compared to control adhesive. The greatest DC was detected for the EA group followed by 2.5%- ß-TCP group, whereas the lowest DC values were for the 5%- ß-TCP group.

Adhesive Bond Integrity of Experimental Zinc Oxide Nanoparticles Incorporated Dentin Adhesive: An SEM, EDX, µTBS, and Rheometric Analysis.

Objective: Our study is aimed at preparing an experimental adhesive (EA) and assessing the influence of adding 5-10 wt.% concentrations of zinc oxide (ZnO) nanoparticles on the adhesive's mechanical properties. Methods: Field emission scanning electron microscopy (FESEM) and energy dispersive X-ray (EDX) spectroscopy were employed to investigate the morphology and elemental distribution of the filler nanoparticles. To examine the adhesive properties, microtensile bond strength (µTBS) testing, an investigation of the rheological properties, degree of conversion (DC), and analysis of the interface between the adhesive and dentin were carried out. Results: The SEM micrographs of ZnO nanoparticles demonstrated spherical agglomerates. The EDX plotting confirmed the incidence of Zn and oxygen (O) in the ZnO nanoparticles. The highest µTBS was observed for nonthermocycled (NTC) 5 wt.% ZnO group (32.11 ± 3.60 MPa), followed by the NTC-10 wt.% ZnO group (30.04 ± 3.24 MPa). Most of the failures observed were adhesive in nature. A gradual reduction in the viscosity was observed at higher angular frequencies, and the addition of 5 and 10 wt.% ZnO to the composition of the EA lowered its viscosity. The 5 wt.% ZnO group demonstrated suitable dentin interaction by showing the formation of resin tags, while for the 10 wt.% ZnO group, compromised resin tag formation was detected. DC was significantly higher in the 0% ZnO (EA) group. Conclusion: The reinforcement of the EA with 5 and 10 wt.% concentrations of ZnO nanoparticles produced an improvement in the adhesive's µTBS. However, a reduced viscosity was observed for both nanoparticle-reinforced adhesives, and a negotiated dentin interaction was seen for 10 wt.% ZnO adhesive group. Further research exploring the influence of more filler concentrations on diverse adhesive properties is recommended.