Mechanical and antibacterial properties of an experimental flowable composite containing Nb₂O₅ and NF_TiO₂ nanoparticles.

Abstract

This study developed an experimental flowable composite incorporated with niobium pentoxide (Nb₂O₅) combined or not with titanium dioxide co-doped with fluorine and nitrogen (NF_TiO₂) and evaluated the mechanical and antibacterial properties. The experimental flowable composite (TEGDMA + BisGMA 1:1 + 60%wt - inorganic filler - borosilicate 0.7 μm) was formulated according to the type and concentration of Nb₂O₅ and NF_TiO₂ (0.5, 1, 1.5 and 2 wt%) or NF_TiO₂ + Nb₂O₅ (0.25, 0.5, 0.75 and 1 wt% - 1:1). The control groups were formed by the experimental composite without the incorporation of Nb₂O₅ and/or NF_TiO₂ (GC-E) and by a commercial flowable composite (GC). The characterization of the surface of the composite and its particles was carried out using scanning electron microscopy (SEM) and energy dispersive x-rays (EDX). Specimens were manufactured and subjected to mechanical tests of flexural strength (FS) (n = 12), flexural modulus (FM) (n = 12), roughness (Ra) (n = 10), microhardness (n = 10), and contact angle (n = 10); and, to evaluate the antibacterial activity, they were submitted to tests of biofilm formation against S. mutans (CFU/mL) (n = 5), biofilm biomass by dry weight (n = 5) and confocal laser microscopy (%LIVE/DEAD) (n = 5). Data were submitted to one-way ANOVA and Tukey's post-hoc and, those that were not homoscedastic, but with normality, were submitted to Welch's ANOVA and Games-Howell's post-hoc. Dunnet's test was used to compare the controls with the other experimental groups (α = 5). The Nb₂O₅ particles had an average size of 32.4 μm and the nanoparticles (NPs) of NF_TiO₂, 10 nm. EDX analysis identified isolated peaks of N, F, Ti, and Nb confirming the presence of these particles in the resin matrix. The 1.5% NF_TiO₂ group had a higher FS and FM than the controls (p < 0.05). GC showed higher microhardness between groups (p < 0.05). There was no difference between the experimental groups regarding contact angle and roughness (p > 0.05), except for GC, which had the highest Ra values and the lowest contact angle between groups (p < 0.05). Composites containing 0.5%, 1%, 1.5%, and 2% Nb₂O₅, 1%, 1.5%, and 2% NF_TiO₂ and 2% Nb₂O₅ + NF_TiO₂ showed lower biofilm formation (p < 0.05), lower total biofilm biomass (p < 0.05), and a higher percentage of dead cells (44%, 52%, 52%, 79%, 42% 43%, 62%, 65%, respectively) than GC and GC-E (5% and 1%, respectively). It is concluded that the incorporation of 1.5% NF_TiO₂ promoted a greater FS and FM among the experimental composites and that the addition of Nb₂O₅ particles (0.5%, 1%, 1.5%, and 2%), NF_TiO₂ (1%, 1.5% and 2%) and the combination Nb₂O₅ + NF_TiO₂ (2%) showed significant antibacterial effects.