Puppin-Rontani J, Fugolin A P P, Costa A R, Correr-Sobrinho L, Pfeifer C S
Int J Adhes Adhes. 2020 Dec;103. doi: 10.1016/j.ijadhadh.2020.102688. Epub 2020 Aug 2.
Thio-urethane oligomeric additives have been shown to improve the mechanical properties of dental composites and resin cements. To try to harness those same properties in dental adhesives, in this study, these oligomers (TU) were added to the matrix and/or as filler functionalization of experimental adhesives, and the effects on conversion and mechanical properties were analyzed.
BisGMA and HEMA (60/40 wt%) were used as the monomer matrix, made polymerizable by the addition of 0.2 wt% 2,2-dimethoxy-2- phenylacetophenone. 2,6-di--butyl-4-methylphenol was added at 0.5 wt% as the inhibitor. This material was used as the unfilled control (BH). TU oligomers were added at 20 wt % to the matrix (BH+20%TU, unfilled) and/or used as filler functionalization (TF, 10 wt%). Fillers functionalized with methacrylate (MF, 10 wt%) served as the control. The experimental adhesives groups containing fillers were: BH+10%MF; BH+10%TF; BH+20%TU+10%MF; BH+20%TU+10%TF. Flexural properties were tested in three-point bending (wet and dry). Polymerization kinetics was followed in real-time in near-IR. Water Sorption/Solubility (WS/SL, ISO 4049) and Viscosity (rotational rheometry) were also evaluated. For Microtensile bond strength 40 vol% ethanol was added to adhesives, which was applied onto sound dentin from third human molars. The data were analyzed with one-way ANOVA and Tukey post-hoc test, and test t for the comparison between storage time of the microtensile bond strength test (alpha = 0.05).
There was no significant difference between groups when yield strength (YS) and flexural modulus (FM) were evaluated in dry conditions. After water storage, all the groups containing TU in the matrix showed statistically lower YS/FM values. This was true in spite of the statistically higher conversion for those same groups. The maximum rate of polymerization (Rpmax) was higher for BH+10%TF and no significant difference was found for the groups BH and BH+10% MF. The lowest Rpmax values were found for BH+20%TU+10%TF and BH+20%TU. BH+20%TU+10%TF showed the highest viscosity values followed by BH+20%TU+10%MF and BH+20%TU, with statistically significant difference between them. For the microtensile bond strength test at 24h (p = 0.13) and 6 months (p = 0.11) and WS/SL (p 0.05), no significant difference was found among groups. The storage time (24 h and 6 months) did not affect the microtensile bond strength results.
In spite of improving the conversion, the addition of TU in the matrix reduced the mechanical properties of the adhesives tested after water storage. This did not affect the bond strength at 24 h or 6 months.
硫代聚氨酯低聚物添加剂已被证明可改善牙科复合材料和树脂水门汀的机械性能。为了在牙科粘合剂中利用这些相同的性能,在本研究中,将这些低聚物(TU)添加到实验性粘合剂的基质中并/或用作填料功能化,分析其对转化率和机械性能的影响。
使用BisGMA和HEMA(60/40 wt%)作为单体基质,通过添加0.2 wt%的2,2 - 二甲氧基 - 2 - 苯基苯乙酮使其可聚合。添加0.5 wt%的2,6 - 二叔丁基 - 4 - 甲基苯酚作为抑制剂。该材料用作未填充对照(BH)。将TU低聚物以20 wt%添加到基质中(BH + 20%TU,未填充)并/或用作填料功能化(TF,10 wt%)。用甲基丙烯酸酯官能化的填料(MF,10 wt%)用作对照。含有填料的实验性粘合剂组为:BH + 10%MF;BH + 10%TF;BH + 20%TU + 10%MF;BH + 20%TU + 10%TF。在三点弯曲(湿态和干态)下测试弯曲性能。在近红外光下实时跟踪聚合动力学。还评估了吸水性/溶解性(WS/SL,ISO 4049)和粘度(旋转流变学)。对于微拉伸粘结强度,向粘合剂中添加40 vol%的乙醇,将其应用于第三恒磨牙的健康牙本质上。数据采用单因素方差分析和Tukey事后检验进行分析,并对微拉伸粘结强度测试的储存时间之间的比较进行t检验(α = 0.05)。
在干燥条件下评估屈服强度(YS)和弯曲模量(FM)时,各实验组之间无显著差异。水储存后,基质中含有TU的所有组的YS/FM值在统计学上均较低。尽管这些组的转化率在统计学上较高,但情况依然如此。BH + 10%TF的最大聚合速率(Rpmax)较高,BH组和BH + 10%MF组之间未发现显著差异。BH + 20%TU + 10%TF和BH + 20%TU的Rpmax值最低。BH + 20%TU + 10%TF的粘度值最高,其次是BH + 20%TU + 10%MF和BH + 20%TU,它们之间存在统计学上的显著差异。对于24小时(p = 0.13)和6个月(p = 0.11)的微拉伸粘结强度测试以及WS/SL(p > 0.05),各实验组之间未发现显著差异。储存时间(24小时和6个月)不影响微拉伸粘结强度结果。
尽管提高了转化率,但在基质中添加TU会降低水储存后测试的粘合剂的机械性能。这在24小时或6个月时不影响粘结强度。