Objective

To evaluate the influence of the addition of functionalized and non-functionalized TiO₂ nanostructures on properties of a resin composite.

Methods

TiO₂ nanostructures were synthesized and functionalized, using 3-(aminopropyl)triethoxysilane (APTMS) and 3-(trimethoxysilyl)propyl methacrylate (TSMPM). Characterizations were performed with XRD, EDS, TEM, and TGA. Resin composites containing Bis-GMA/TEGDMA, CQ, DABE, and barium-aluminum silicate glass were produced according to TiO₂ nanostructure (nanotube or nanoparticle), concentration (0.3 or 0.9 wt%), and functionalization (APTMS or TSMPM). The resin composite without nanostructures was used as control. The amount of fillers was kept constant at 78.3 wt% for all materials. The degree of conversion (DC - at 0 h and 24 h), maximum polymerization rate (Rp_max), and Knoop microhardness (KHN before and after ethanol softening) were evaluated. Data were analyzed with two-way ANOVA with repeated measures and Tukey's HSD (α = 0.05).

Results

TGA results demonstrated that functionalizations were effective for both nanostructures. For DC, resin composites, time and interaction effect were significant (p < 0.001). Higher DC was found for 0.3-wt%-functionalized-nanotubes at 24 h. For nanoparticles, only 0.9-wt%-non-functionalized and 0.3-wt%-APTMS-functionalized showed DC similar to the control and all other groups showed higher DC (p < 0.05). Rp_max was higher for 0.3-wt%-APTMS-nanotubes, which corresponded to higher DC after 24 h. The lowest Rp_max occurred for 0.9-wt%-TSMPM-nanotubes, which showed smaller DC at 0 h. For KHN, resin composites, ethanol softening and interaction effect were significant (p < 0.001). KHN decreased after ethanol softening all groups, except for 0.3-wt%-TSMPM-nanotubes, 0.9-wt%-TSMPM-nanotubes, and 0.3-wt%-non-functionalized-nanoparticles.

Conclusion

The resin with 0.3-wt%-TSMPM-nanotubes showed higher DC after 24 h, while being the most stable material after the ethanol softening.

Significance

The addition of functionalized TiO₂ nanostructures in resin-based materials may improve the properties of the material.

中文翻译：

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功能化TiO ₂纳米管和纳米粒子的添加对实验树脂复合材料性能的影响

目的

为了评估添加功能化和非功能化TiO ₂纳米结构对树脂复合材料性能的影响。

方法

使用3-（氨基丙基）三乙氧基硅烷（APTMS）和甲基丙烯酸3-（三甲氧基甲硅烷基）丙酯（TSMPM）合成并官能化TiO ₂纳米结构。用XRD，EDS，TEM和TGA进行表征。根据TiO ₂纳米结构（纳米管或纳米颗粒），浓度（0.3或0.9 wt％）和功能化（APTMS或TSMPM），生产包含Bis-GMA / TEGDMA，CQ，DABE和钡铝硅酸盐玻璃的树脂复合材料。没有纳米结构的树脂复合物用作对照。对于所有材料，填料的量保持恒定在78.3重量％。转化率（DC-在0 h和24 h时），最大聚合速率（Rp _max））和努氏显微硬度（乙醇软化前后的KHN）进行了评估。数据采用重复测量和Tukey HSD（α= 0.05）的双向方差分析进行分析。

结果

TGA结果表明，官能化对于两种纳米结构均有效。对于DC，树脂复合材料的时间和相互作用效果显着（p <0.001）。发现在24 h时0.3-wt％的功能化纳米管的DC更高。对于纳米颗粒，仅0.9-wt％的未官能化和0.3-wt％的APTMS-官能化显示出与对照相似的DC，并且所有其他组均显示出更高的DC（p <0.05）。0.3％（重量）-APTMS-纳米管的Rp _max更高，这对应于24小时后更高的DC。最低Rp_最大值0.9-wt％-TSMPM-纳米管发生过，在0 h时DC较小。对于KHN，树脂复合材料，乙醇软化和相互作用效果显着（p <0.001）。乙醇软化所有组后，KHN降低，除了0.3-wt％-TSMPM-纳米管，0.9-wt％-TSMPM-纳米管和0.3-wt％-非官能化的纳米颗粒。

结论

具有0.3 wt％-TSMPM纳米管的树脂在24 h后显示出较高的DC，而在乙醇软化后却是最稳定的材料。

意义

在树脂基材料中添加功能化的TiO ₂纳米结构可以改善材料的性能。