Characterization of Experimental Nanoparticulated Dental Adhesive Resins with Long-Term Antibacterial Properties

Experimental adhesives with functional nitrogen-doped titanium dioxide nanoparticles (N_TiO2) have been shown to display improved properties. However, these materials have not been characterized regarding their degree of conversion (DC), biaxial flexure strength (BFS), surface roughness (SR), elastic modulus (EM), and long-term antibacterial functionalities. Experimental adhesives were synthesized by dispersing N_TiO2 (10%, 20%, or 30%, v/v%) into OptiBond Solo Plus (OPTB, Kerr Corp., USA). Unpolymerized adhesives (volume = 50 μL/drop, n = 3/group) were individually placed onto a heated (37 °C) attenuated total reflectance (ATR) monolithic diamond crystal (Golden Gate, Specac). The spectra of composites were obtained with a Fourier-transform infrared (FTIR) spectrometer (Nicolet IS50; 500–4500 cm−1; resolution = 4 cm−1, 10 internal scans/spectrum) before and after polymerization. Disk-shaped specimens (diameter = 6.0 mm, thickness = 0.5 mm) for BFS (n = 12/group), SR and EM (n = 3/group), and for antibacterial testing (n = 18/group/time-point) were fabricated and photopolymerized (1 min each; 385–515 nm, 1000 mW/cm2; VALO). DC values (%) were calculated from pre- and post-polymerization spectra using the two-frequency method and tangent-baseline technique. BFS was assessed using a universal testing machine (Instron 68TM-5, crosshead speed = 1.27 mm/min, 25 °C). SR and EM were investigated using an atomic force microscope (Multimode 8) with aluminum-coated silicon probes (8 nm pyramidal tip, spring constant 40 N/m, Bruker). Antibacterial testing was performed by growing Streptococcus mutans biofilms (UA159-ldh, 37 °C, microaerophilic) on the surfaces of specimens for 24 h and then measuring the relative luminescence units (RLU) with a Biotek Synergy HT multi-well plate reader. Results demonstrate that experimental materials containing 10%, 20%, and 30% of N_TiO2 displayed higher levels of DC, had better mechanical properties, and were able to exert strong and durable antibacterial properties without visible light irradiation and after extended periods of simulated shelf-life and aging in PBS. The reported experimental materials are expected to increase the service lives of polymer-based bonded restorations by decreasing the incidence of secondary caries

The Applicability of a Drop Penetration Method to Measure Contact Angles on TiO2 and ZnO Nanoparticles

In this study, six solvents (water, diiodomethane, bromonaphthalene, formamide, ethanol and ethylene glycol) were examined for three nanoparticle substrates, zinc oxide and titanium dioxide (21 nm and 100 nm), with the goal of assessing the suitability of a modified drop penetration method (DPM) for orders of magnitude smaller particles. Nanoparticles were compressed into flat discs and the solvent dropped on the surface while the image with time was recorded. Contact angles were in reasonable agreement with literature over the range of 20–80°, but failed to provide acceptable results for surface energy components. It was necessary to eliminate certain solvents and substrates not meeting the selection criteria