AIM The study aimed to assess graphene oxide (GO) adhesive and its dentin interaction using scanning electron microscopy (SEM), MicroRaman spectroscopy and Microtensile bond strength (μTBS). MATERIALS AND METHODS Experimental GOA and control adhesives (CA) were fabricated. Presence of GO within the experimental adhesive resin was assessed using SEM and Micro-Raman spectroscopy. Ninety specimens were prepared, sixty teeth were utilized for μTBS, twenty for SEM analysis of interface for CA and GOA and ten were assessed using microRaman spectroscopy. Each specimen was sectioned and exposed dentine was conditioned (35% phosphoric acid) for 10 s. The surface was coated twice with adhesive (15 s) and photopolymerized (20 s). Composite build-up on specimen was photo-polymerized. Among the bonded specimens, thirty specimen were assessed using Micro-Raman spectrometer, SEM and energy dispersive X-ray spectroscopy (EDX), whereas remaining specimens were divided in to three sub-groups (n = 10) based on the storage of 24 h, 8 weeks and 16 weeks. μTBS testing was performed at a crosshead speed of 0.5 mm/min using a microtensile tester. The means of μ-tbs were analyzed using ANOVA and post hoc Tukey multiple comparisons test. RESULTS No significant difference in μTBS of CA and GOA was observed. Storage time presented a significant interaction on the μTBS (p < 0.01). The highest and lowest μTBS was evident in CA (30.47 (3.55)) at 24 h and CA (22.88 (3.61)) at 18 weeks. Micro-Raman analysis identified peaks of 1200 cm-1 to 1800 cm1, D and G bands of GO nanoparticles in the resin. Uniform distribution of graphene oxide nanoparticles was present at the adhesive and hybrid layer. CONCLUSION GO showed interaction within adhesive and tooth dentin similar to CA, along with formation of hybrid layer. In ideal conditions (absence of nanoleakage), graphene oxide modified adhesive shows comparable bond strength and durability of resin dentine bond.

中文翻译：

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基于氧化石墨烯纳米填料的实验性牙本质粘合剂。A SEM / EDX、Micro-Raman 和微拉伸粘合强度分析

目的 该研究旨在使用扫描电子显微镜 (SEM)、显微拉曼光谱和微拉伸粘合强度 (μTBS) 评估氧化石墨烯 (GO) 粘合剂及其牙本质相互作用。材料和方法实验性GOA和控制粘合剂（CA）被制造出来。使用 SEM 和显微拉曼光谱评估实验粘合剂树脂中 GO 的存在。制备了 90 个样品，60 个牙齿用于 μTBS，20 个用于 CA 和 GOA 界面的 SEM 分析，10 个使用显微拉曼光谱进行评估。每个样本都被切片，暴露的牙本质被调理（35% 磷酸）10 秒。用粘合剂（15 秒）和光聚合（20 秒）将表面涂敷两次。样品上的复合材料堆积是光聚合的。在粘合试样中，使用显微拉曼光谱仪、SEM 和能量色散 X 射线光谱仪 (EDX) 评估了 30 个样本，而剩余的样本根据 24 小时、8 周和 16 小时的储存分为三个亚组 (n = 10)周。μTBS 测试使用微拉伸测试仪以 0.5 mm/min 的十字头速度进行。使用 ANOVA 和事后 Tukey 多重比较检验分析 μ-tbs 的平均值。结果CA和GOA的μTBS没有显着差异。存储时间对 μTBS 有显着的交互作用（p < 0.01）。最高和最低的 μTBS 在 24 小时时 CA（30.47（3.55））和 18 周时 CA（22.88（3.61））是明显的。显微拉曼分析确定了树脂中 GO 纳米颗粒的 1200 cm-1 至 1800 cm1 峰、D 和 G 带。氧化石墨烯纳米粒子的均匀分布存在于粘合剂和混合层中。结论 GO 显示了与 CA 类似的粘合剂和牙本质的相互作用，以及混合层的形成。在理想条件下（没有纳米泄漏），氧化石墨烯改性粘合剂显示出与树脂牙本质粘合相当的粘合强度和耐久性。