Dental Materials Department, School of Dentistry, Federal University of Rio Grande do Sul. Ramiro Barcelos Street, 2492, Rio Branco, 90035-003, Porto Alegre, RS, Brazil.
Laboratory of Molecular Catalysis, Institute of Chemistry, Federal University of Rio Grande do Sul. Bento Gonçalves Avenue, 9500, Agronomia, 91501-970, Porto Alegre, RS, Brazil.
Dent Mater. 2021 Feb;37(2):223-235. doi: 10.1016/j.dental.2020.11.004. Epub 2020 Nov 24.
Formulate experimental adhesives containing titanium dioxide nanotubes (nt-TiO) or titanium dioxide nanotubes with a triazine-methacrylate monomer (nt-TiO:TAT) and evaluate the effect of these fillers on the physical, chemical, and biological properties of the adhesives.
First, nt-TiO were synthesized via a hydrothermal method. The nt-TiO were mixed with a triazine-methacrylate monomer (TAT) to formulate nt-TiO:TAT, which were characterized by transmission electron microscopy (TEM). The nt-TiO, TAT, and nt-TiO:TAT were evaluated via Fourier Transform Infrared, Ultraviolet-visible, and micro-Raman spectroscopies. An experimental adhesive resin was formulated with bisphenol A glycerolate dimethacrylates, 2-hydroxyethyl methacrylate, and photoinitiator/co-initiator system. nt-TiO or nt-TiO:TAT were incorporated at 2.5 wt.% and 5 wt.% in the adhesive. The base resin without nt-TiO or nt-TiO:TAT was used as a control group. The adhesives were evaluated for antibacterial activity, cytotoxicity, polymerization kinetics, degree of conversion (DC), Knoop hardness, softening in solvent (ΔKHN%), ultimate tensile strength (UTS), 24 h- and 1 year- microtensile bond strength (μ-TBS).
TEM confirmed the nanotubular morphology of TiO. FTIR, UV-vis, and micro-Raman analyses showed the characteristic peaks of each material, indicating the impregnation of TAT in the nt-TiO. Adhesives with nt-TiO:TAT showed antimicrobial activity against biofilm formation compared to control (p < 0.05), without differences in the viability of planktonic bacteria (p > 0.05). All groups showed high percentages of pulp cell viability. The polymerization kinetics varied among groups, but all presented DC above 50%. The addition of 5 wt.% of nt-TiO and both groups containing nt-TiO:TAT showed higher values of Knoop hardness compared to the control (p < 0.05). The groups with nt-TiO:TAT presented lower ΔKHN% (p < 0.05) and higher UTS (p < 0.05) than the control group. After one year, the group with 5 wt.% of nt-TiO, as well as both groups containing nt-TiO:TAT, showed higher μ-TBS than the control (p < 0.05).
The mixing of a triazine-methacrylate monomer with the nt-TiO generated a filler that improved the physicochemical properties of the adhesive resins and provided antibacterial activity, which could assist in preventing carious lesions around tooth-resin interfaces. The set of physical, chemical, and biological properties of the formulated polymer, together with the greater stability of the bond strength over time, make nt-TiO:TAT a promising filler for dental adhesive resins.
制备含有二氧化钛纳米管(nt-TiO)或含有三嗪-甲基丙烯酸酯单体的二氧化钛纳米管(nt-TiO:TAT)的实验性胶粘剂,并评估这些填料对胶粘剂的物理、化学和生物性能的影响。
首先,通过水热法合成 nt-TiO。将 nt-TiO 与三嗪-甲基丙烯酸酯单体(TAT)混合以制备 nt-TiO:TAT,并通过透射电子显微镜(TEM)进行表征。通过傅里叶变换红外光谱、紫外-可见光谱和微拉曼光谱对 nt-TiO、TAT 和 nt-TiO:TAT 进行了评价。用双酚 A 甘油二甲基丙烯酸酯、2-羟乙基甲基丙烯酸酯和光引发剂/共引发剂体系配制实验性胶粘剂树脂。将 2.5wt.%和 5wt.%的 nt-TiO 或 nt-TiO:TAT 掺入胶粘剂中。不含 nt-TiO 或 nt-TiO:TAT 的基础树脂用作对照组。评估了抗菌活性、细胞毒性、聚合动力学、转化率(DC)、努普硬度、溶剂软化(ΔKHN%)、极限拉伸强度(UTS)、24 小时和 1 年微拉伸结合强度(μ-TBS)。
TEM 证实了 TiO 的纳米管形态。FTIR、UV-vis 和微拉曼分析显示了每种材料的特征峰,表明 TAT 浸渍在 nt-TiO 中。与对照组相比,含有 nt-TiO:TAT 的胶粘剂对生物膜形成具有抗菌活性(p < 0.05),但对浮游细菌的活力没有差异(p > 0.05)。所有组的牙髓细胞存活率均较高。聚合动力学在各组之间有所不同,但所有组的 DC 均高于 50%。与对照组相比,添加 5wt.%nt-TiO 和含有 nt-TiO:TAT 的两组的努普硬度值更高(p < 0.05)。含有 nt-TiO:TAT 的组的 ΔKHN%(p < 0.05)较低,UTS 较高(p < 0.05)。1 年后,添加 5wt.%nt-TiO 和含有 nt-TiO:TAT 的两组的 μ-TBS 均高于对照组(p < 0.05)。
将三嗪-甲基丙烯酸酯单体与 nt-TiO 混合生成了一种填料,改善了胶粘剂树脂的物理化学性能,并提供了抗菌活性,有助于防止牙-树脂界面周围的龋齿病变。所制备的聚合物的一系列物理、化学和生物学特性,以及随着时间的推移结合强度的稳定性增加,使 nt-TiO:TAT 成为一种有前途的牙科胶粘剂树脂填料。