Graphene oxide nano-filler based experimental dentine adhesive. A SEM / EDX, Micro-Raman and microtensile bond strength analysis

Abstract

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.