Thadathil Varghese Jerrin, Cho Kiho, Farrar Paul, Prentice Leon, Prusty B Gangadhara
School of Mechanical and Manufacturing Engineering, University of New South Wales, NSW 2052, Australia.
School of Mechanical and Manufacturing Engineering, University of New South Wales, NSW 2052, Australia; Division of Applied Oral Sciences & Community Dental Care, Faculty of Dentistry, University of Hong Kong, Hong Kong, China.
Dent Mater. 2022 Jul;38(7):1173-1183. doi: 10.1016/j.dental.2022.06.002. Epub 2022 Jun 9.
This experimental investigation explored the optimisation of silane treatment of surface-modified S-2 Glass fibres in restorative dental composites for improved mechanical performance. The influence of optimum amount of silane to improve the interfacial adhesion at the fibre-matrix interfaces and its effect on the mechanical properties of the restorative composites were explored.
S-2 Glass fibres of 5 μm diameter and 250 μm length were surface modified using the acid etching technique. The etched fibres were then treated with either 3-methacryloxypropyltrimethoxysilane (3-MPS), 3-Glycidoxipropyltrimethoxysilane (3-GPS) or 8-methacryloxyoctyltrimethoxysilane (8-MOTS) at varying molar % / wt% concentrations. Fibres that were not silanised with any silane coupling agents were used as the control sample. The silanol content of each mixed silane was observed using Fourier transform infrared (FT-IR) spectroscopy analysis. Fibres (5 wt%) with optimised molar% / wt% silane coupling concentration were added to UDMA/TEGDMA dental resin. Mechanical properties such as flexural strength, flexural modulus, and the breaking energy of the materials were evaluated using a comprehensive experimental programme.
FTIR spectrum of glass fibre silanised with each silane coupling agent revealed many peaks from 3800 to 1400 cm, indicative of -CH, -CH and CO bonding, suggesting the proper silanization of the fibre. The contact angle test revealed that optimum wt% concentration of 3-MPS, 3-GPS and 8-MOTS were 0.5%, 0.8% and 1.4% respectively. The flexural strength of the fibre-reinforced with optimum concentration of 3-MPS (DC-3-MPS_0.5%) increased by 7.0% compared to those of the 2 wt% concentration of 3-MPS fibre-reinforced composite (DC-3-MPS_2.0%). While the flexural strength of optimum concentration 8-MOTS grafted dental resin composites (DC-8-MOTS_1.4%) were 9.9% higher than that of 2 wt% concentration 8-MOTS grafted dental resin composite (DC-8-MOTS_2.0%) and the flexural strength of optimum concentration of 3-GPS (DC-3-GPS_0.8%) was 7.5% higher when compared to that of 2 wt% concentration 3-GPS grafted dental resin composites (DC-3-GPS_2.0%). A concurrent trend was found while investigating the fracture behaviour of the dental composite with optimum wt% concentration of each silane coupling agent against its corresponding higher wt% concentrations. The ANOVA results showed that the optimum fibre-reinforced dental composites grafted with 8-MOTS showed better mechanical behaviour when compared to 3-GPS and 3-MPS.
The interfacial adhesion between the fibre and the resin due to silane coupling agents has helped to improve the mechanical properties of the fibre-reinforced dental composite. This is the first experimental study to provide a thorough investigation into the significance of the optimal use of silane coupling agents to treat the S-2 Glass fibres and subsequently the influence on the mechanical performance of the fibre-reinforced flowable dental composites.
本实验研究探索了用于修复性牙科复合材料的表面改性S-2玻璃纤维硅烷处理的优化方法,以提高其机械性能。研究了硅烷最佳用量对改善纤维-基体界面间粘结力的影响及其对修复性复合材料机械性能的作用。
采用酸蚀技术对直径5μm、长度250μm的S-2玻璃纤维进行表面改性。然后,将蚀刻后的纤维用3-甲基丙烯酰氧基丙基三甲氧基硅烷(3-MPS)、3-缩水甘油醚氧基丙基三甲氧基硅烷(3-GPS)或8-甲基丙烯酰氧基辛基三甲氧基硅烷(8-MOTS)在不同的摩尔百分比/重量百分比浓度下进行处理。未用任何硅烷偶联剂进行硅烷化处理的纤维用作对照样品。使用傅里叶变换红外(FT-IR)光谱分析观察每种混合硅烷的硅醇含量。将具有优化摩尔百分比/重量百分比硅烷偶联浓度的纤维(5重量%)添加到UDMA/TEGDMA牙科树脂中。使用综合实验方案评估材料的弯曲强度、弯曲模量和断裂能等机械性能。
用每种硅烷偶联剂进行硅烷化处理的玻璃纤维的FTIR光谱在3800至1400cm处显示出许多峰,表明存在-CH、-CH和CO键,这表明纤维已成功进行了硅烷化处理。接触角测试表明,3-MPS、3-GPS和8-MOTS的最佳重量百分比浓度分别为0.5%、0.8%和1.4%。与2重量%浓度的3-MPS纤维增强复合材料(DC-3-MPS_2.0%)相比,最佳浓度3-MPS(DC-3-MPS_0.5%)增强的纤维的弯曲强度提高了7.0%。最佳浓度8-MOTS接枝的牙科树脂复合材料(DC-8-MOTS_1.4%)的弯曲强度比2重量%浓度8-MOTS接枝的牙科树脂复合材料(DC-8-MOTS_2.0%)高9.9%,最佳浓度3-GPS(DC-3-GPS_0.8%)的弯曲强度比2重量%浓度3-GPS接枝的牙科树脂复合材料(DC-3-GPS_2.0%)高7.5%。在研究每种硅烷偶联剂最佳重量百分比浓度的牙科复合材料相对于其相应较高重量百分比浓度的断裂行为时发现了类似趋势。方差分析结果表明,与3-GPS和3-MPS相比,最佳浓度8-MOTS接枝的纤维增强牙科复合材料表现出更好的机械性能。
硅烷偶联剂使纤维与树脂之间的界面粘结力得到改善,有助于提高纤维增强牙科复合材料的机械性能。这是第一项对硅烷偶联剂最佳用量处理S-2玻璃纤维的重要性以及随后对纤维增强可流动牙科复合材料机械性能的影响进行全面研究的实验性研究。