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Influence of the organic matrix composition on the polymerization behavior and bulk properties of resin composites containing thiourethane-functionalized fillers
European Polymer Journal ( IF 6 ) Pub Date : 2020-05-01 , DOI: 10.1016/j.eurpolymj.2020.109664
Ana Paula Fugolin 1 , Ana Rosa Costa 2 , Emilie Kono 1 , Eleanor Quirk 1 , Jack L Ferracane 1 , Carmem S Pfeifer 1
Affiliation  

Objectives The incorporation of thiourethane-based oligomeric additives into resin composite formulations leads to improvement in mechanical properties and reduction in polymerization stress, but may increase viscosity. The objective of this study was to functionalize filler particle surfaces with thiourethane silane molecules and determine the impact of the inorganic filler loading and surface treatment on the behavior of experimental resin composites with systematically-varied organic matrices. Methods Thiourethane oligomer was synthesized de novo, and grafted to the surface of 0.7um barium glass. BisGMA and TEGDMA (BT) were combined (at 30:70, 50:50 or 70:30 wt%) to 50 or 75 wt% of methacrylate (MA-Sil - control) or thiourethane-silanized (TU-Sil) particles. Composites were made polymerizable by the addition of 0.2 wt% BAPO and 0.05 wt% BHT was added as inhibitor. A mercury arc lamp (320-500 nm) at 800 mW/cm2 was used for all curing procedures. Kinetics of polymerization was assessed by near-IR spectroscopy in real time. Polymerization stress was determined with a cantilever system in real time (Bioman). Flexural modulus and strength were determined in 3-point bending (25x2x2 mm). Water sorption and solubility and film thickness were tested according to ISO 4049. Polymeric network characteristics were analyzed by dynamic mechanical analysis (DMA). Data was analyzed with two-way ANOVA/Tukey's test (95%). Results Viscosity increased with the increase in BisGMA and/or filler amounts. Overall, TU-Sil containing composites showed delayed vitrification and higher final DC. Filler concentration did not affect DC neither flexural strength. DC decreased with increasing BisGMA content. Polymerization stress reduced and flexural modulus increased for higher filler content, especially for formulations containing TU-Sil particles. The water stability was positively affected by the increase in amount of BisGMA and inorganic filler particles. In terms of polymeric network, the addition of TU-Sil particles increased the Tg and decreased the E' and cross-link density. Conclusions With the exception of flexural modulus, all tested properties were significantly impacted by the matrix viscosity and/or the addition of TU-Sil filler particles. In general, the use of thiourethane oligomers as a silane coupling agent was able to reinforce the materials and reduce the polymerization stress without negatively affecting the viscosity of the system.

中文翻译:

有机基体组成对含硫代氨基甲酸酯功能化填料的树脂复合材料聚合行为和整体性能的影响

目的 将基于硫代氨基甲酸酯的低聚添加剂加入树脂复合材料配方可改善机械性能并降低聚合应力,但可能会增加粘度。本研究的目的是用硫代氨基甲酸酯硅烷分子对填料颗粒表面进行功能化,并确定无机填料负载和表面处理对具有系统变化有机基体的实验树脂复合材料行为的影响。方法从头合成硫氨酯低聚物,接枝到0.7um钡玻璃表面。BisGMA 和 TEGDMA (BT) 结合(以 30:70、50:50 或 70:30 wt%)到 50 或 75 wt% 的甲基丙烯酸酯(MA-Sil - 对照)或硫代氨基甲酸酯硅烷化 (TU-Sil) 颗粒。通过添加 0.2 wt% BAPO 和 0.0 使复合材料可聚合。添加05 wt% BHT作为抑制剂。所有固化程序均使用 800 mW/cm2 的汞弧灯 (320-500 nm)。通过近红外光谱实时评估聚合动力学。用悬臂系统实时测定聚合应力(Bioman)。弯曲模量和强度在 3 点弯曲 (25x2x2 mm) 中测定。根据 ISO 4049 测试吸水性和溶解度以及膜厚度。通过动态机械分析 (DMA) 分析聚合物网络特性。使用双向 ANOVA/Tukey 检验 (95%) 分析数据。结果粘度随着 BisGMA 和/或填料量的增加而增加。总体而言,含有 TU-Sil 的复合材料显示延迟玻璃化和更高的最终 DC。填料浓度不影响 DC 也不影响弯曲强度。DC随着BisGMA含量的增加而降低。对于较高的填料含量,特别是对于含有 TU-Sil 颗粒的配方,聚合应力降低,弯曲模量增加。BisGMA 和无机填料颗粒量的增加对水稳定性有积极影响。就聚合物网络而言,TU-Sil 颗粒的添加提高了 Tg 并降低了 E' 和交联密度。结论 除了弯曲模量外,所有测试的性能都受到基体粘度和/或添加 TU-Sil 填料颗粒的显着影响。一般来说,使用硫代氨基甲酸酯低聚物作为硅烷偶联剂能够增强材料并降低聚合应力,而不会对体系的粘度产生负面影响。对于较高的填料含量,特别是对于含有 TU-Sil 颗粒的配方,聚合应力降低,弯曲模量增加。BisGMA 和无机填料颗粒量的增加对水稳定性有积极影响。就聚合物网络而言,TU-Sil 颗粒的添加提高了 Tg 并降低了 E' 和交联密度。结论 除了弯曲模量外,所有测试的性能都受到基体粘度和/或添加 TU-Sil 填料颗粒的显着影响。一般来说,使用硫代氨基甲酸酯低聚物作为硅烷偶联剂能够增强材料并降低聚合应力,而不会对体系的粘度产生负面影响。对于较高的填料含量,特别是对于含有 TU-Sil 颗粒的配方,聚合应力降低,弯曲模量增加。BisGMA 和无机填料颗粒量的增加对水稳定性有积极影响。就聚合物网络而言,TU-Sil 颗粒的添加提高了 Tg 并降低了 E' 和交联密度。结论 除了弯曲模量外,所有测试的性能都受到基体粘度和/或添加 TU-Sil 填料颗粒的显着影响。一般来说,使用硫代氨基甲酸酯低聚物作为硅烷偶联剂能够增强材料并降低聚合应力,而不会对体系的粘度产生负面影响。特别适用于含有 TU-Sil 颗粒的配方。BisGMA 和无机填料颗粒量的增加对水稳定性有积极影响。就聚合物网络而言,TU-Sil 颗粒的添加提高了 Tg 并降低了 E' 和交联密度。结论 除了弯曲模量外,所有测试的性能都受到基体粘度和/或添加 TU-Sil 填料颗粒的显着影响。一般来说,使用硫代氨基甲酸酯低聚物作为硅烷偶联剂能够增强材料并降低聚合应力,而不会对体系的粘度产生负面影响。特别适用于含有 TU-Sil 颗粒的配方。BisGMA 和无机填料颗粒量的增加对水稳定性有积极影响。就聚合物网络而言,TU-Sil 颗粒的添加提高了 Tg 并降低了 E' 和交联密度。结论 除了弯曲模量外,所有测试的性能都受到基体粘度和/或添加 TU-Sil 填料颗粒的显着影响。一般来说,使用硫代氨基甲酸酯低聚物作为硅烷偶联剂能够增强材料并降低聚合应力,而不会对体系的粘度产生负面影响。TU-Sil 颗粒的添加提高了 Tg 并降低了 E' 和交联密度。结论 除了弯曲模量外,所有测试的性能都受到基体粘度和/或添加 TU-Sil 填料颗粒的显着影响。一般来说,使用硫代氨基甲酸酯低聚物作为硅烷偶联剂能够增强材料并降低聚合应力,而不会对体系的粘度产生负面影响。TU-Sil 颗粒的添加提高了 Tg 并降低了 E' 和交联密度。结论 除了弯曲模量外,所有测试的性能都受到基体粘度和/或添加 TU-Sil 填料颗粒的显着影响。一般来说,使用硫代氨基甲酸酯低聚物作为硅烷偶联剂能够增强材料并降低聚合应力,而不会对体系的粘度产生负面影响。
更新日期:2020-05-01
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