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热循环对新型低收缩树脂胶粘剂粘结性能的影响。

Effects of thermal cycling on bonding properties of novel low-shrinkage resin adhesive.

机构信息

Dept. of Prosthodontics, School and Hospital of Stomatology, Cheeloo College of Medicine, Shandong University & Shandong Key Laboratory of Oral Tissue Regeneration & Shandong Engineering Laboratory for Dental Materials and Oral Tissue Regeneration & Shandong Provincial Clinical Research Center for Oral Diseases, Jinan 250012, China.

Research Institute of Polymer Materials, School of Materials Science and Engineering, Shandong University, Jinan 250061, China.

出版信息

Hua Xi Kou Qiang Yi Xue Za Zhi. 2023 Jun 1;41(3):276-283. doi: 10.7518/hxkq.2023.2022459.

Abstract

OBJECTIVES

The current study aimed to investigate the bonding properties of a novel low-shrinkage resin adhesive containing expanding monomer and epoxy resin monomer after thermal cycling aging treatment.

METHODS

Expanding monomer of 3,9-diethyl-3,9-dimethylol-1,5,7,11-tetraoxaspiro-[5,5] undecane (DDTU) as an anti-shrinkage additive and unsaturated epoxy monomer of diallyl bisphenol A diglycidyl ether (DBDE) as a coupling agent were synthesized. A blend of DDTU and DBDE at a mass ratio of 1∶1, referred to as "UE", was added into the resin matrix at the mass fraction of 20% to prepare a novel low-shrinkage resin adhesive.Then, the methacrylate resin adhesive without UE was used as the blank control group, and a commercial resin adhesive system was selected as the commercial control group. Moreover, the resin-dentin bonding and micro-leakage testing specimens were prepared for the thermal cycling aging treatment. The bonding strength was tested, the fracture modes were calculated, the bonding fracture surface was observed by scanning electron microscope (SEM), and the dye penetration was used to evaluate the tooth-restoration marginal interface micro-leakage. All the data were analyzed statistically.

RESULTS

After aging, the dentin bonding strength of the experimental group was (19.20±1.03) MPa without a significant decrease (>0.05), that of the blank control group was (11.22±1.48) MPa with a significant decrease (<0.05) and that of the commercial control group was (19.16±1.68) MPa without a significant decrease (>0.05). The interface fracture was observed as the main fracture mode in each group after thermal cycling by SEM. The fractured bonding surfaces of the experimental group often occurred on the top of the hybrid layer, whereas those of the blank and commercial control groups mostly occurred on the bottom of the hybrid layer. Micro-leakage rating counts of specimens before and after thermal cycling were as follows: the experimental group was primarily 0 grade, thereby indicating that a relatively ideal marginal sealing effect could be achieved (>0.05); meanwhile, the blank control group was primarily 1 grade, and the penetration depth of dye significantly increased after thermal cycling (<0.05); the commercial control group was primarily 0 grade without statistical difference before and after thermal cycling (>0.05), while a significant difference was observed between the commercial control group and experimental group after thermal cycling (<0.05).

CONCLUSIONS

The novel low-shrinkage resin adhesive containing 20%UE exhibited excellent bonding properties even after thermal cycling aging treatment, thereby showing a promising prospect for dental application.

摘要

目的

本研究旨在探讨含有膨胀单体和环氧树脂单体的新型低收缩树脂胶粘剂在热循环老化处理后的粘结性能。

方法

合成了 3,9-二乙基-3,9-二羟甲基-1,5,7,11-四氧杂螺[5.5]十一烷(DDTU)作为抗收缩添加剂的膨胀单体和作为偶联剂的双烯丙基双酚 A 二缩水甘油醚(DBDE)不饱和环氧树脂单体。将 DDTU 和 DBDE 以质量比 1∶1 混合,称为“UE”,以 20%的质量分数添加到树脂基质中,制备新型低收缩树脂胶粘剂。然后,将不含 UE 的甲基丙烯酸树脂胶粘剂作为空白对照组,选择商业树脂胶系统作为商业对照组。此外,还制备了用于热循环老化处理的树脂-牙本质粘结和微渗漏测试标本。测试粘结强度,计算断裂模式,用扫描电子显微镜(SEM)观察粘结断裂表面,并使用染料渗透评估牙修复边缘界面微渗漏。对所有数据进行统计学分析。

结果

老化后,实验组牙本质粘结强度为(19.20±1.03)MPa,无明显下降(>0.05),空白对照组为(11.22±1.48)MPa,明显下降(<0.05),商业对照组为(19.16±1.68)MPa,无明显下降(>0.05)。热循环后,SEM 观察到各组的主要断裂模式为界面断裂。实验组的断裂粘结面常发生在混合层的顶部,而空白组和商业对照组的断裂粘结面大多发生在混合层的底部。热循环前后标本的微渗漏评分计数如下:实验组主要为 0 级,表明可获得相对理想的边缘密封效果(>0.05);同时,空白对照组主要为 1 级,热循环后染料渗透深度明显增加(<0.05);商业对照组热循环前后均为 0 级,无统计学差异(>0.05),但热循环后商业对照组与实验组差异有统计学意义(<0.05)。

结论

含 20%UE 的新型低收缩树脂胶粘剂即使经过热循环老化处理,仍具有优异的粘结性能,在口腔应用方面具有广阔的前景。

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本文引用的文献

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Development of low-shrinkage dental adhesives via blending with spiroorthocarbonate expanding monomer and unsaturated epoxy resin monomer.
J Mech Behav Biomed Mater. 2022 Sep;133:105308. doi: 10.1016/j.jmbbm.2022.105308. Epub 2022 Jun 9.
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Enhancing resin-dentin bond durability using a novel mussel-inspired monomer.
Mater Today Bio. 2021 Nov 29;12:100174. doi: 10.1016/j.mtbio.2021.100174. eCollection 2021 Sep.
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Hua Xi Kou Qiang Yi Xue Za Zhi. 2020 Jun 1;38(3):256-262. doi: 10.7518/hxkq.2020.03.005.
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