Dentin Bond Integrity of Hydroxyapatite Containing Resin Adhesive Enhanced with Graphene Oxide Nano-Particles-An SEM, EDX, Micro-Raman, and Microtensile Bond Strength Study

含羟基磷灰石树脂粘接剂经氧化石墨烯纳米颗粒增强后与牙本质的粘接完整性——扫描电镜、能谱分析、显微拉曼光谱和微拉伸粘接强度研究

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Abstract

The aim was to synthesize and characterize an adhesive incorporating HA and GO nanoparticles. Techniques including scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX), micro-tensile bond strength (μTBS), and micro-Raman spectroscopy were employed to investigate bond durability, presence of nanoparticles inside adhesive, and dentin interaction. Control experimental adhesive (CEA) was synthesized with 5 wt% HA. GO particles were fabricated and added to CEA at 0.5 wt% (HA-GO-0.5%) and 2 wt% GO (HA-GO-2%). Teeth were prepared to produce bonded specimens using the three adhesive bonding agents for assessment of μTBS, with and without thermocycling (TC). The adhesives were applied twice on the dentin with a micro-brush followed by air thinning and photo-polymerization. The HA and GO nanoparticles demonstrated uniform dispersion inside adhesive. Resin tags with varying depths were observed on SEM micrographs. The EDX mapping revealed the presence of carbon (C), calcium (Ca), and phosphorus (P) in the two GO adhesives. For both TC and NTC samples, HA-GO-2% had higher μTBS and durability, followed by HA-GO-0.5%. The representative micro-Raman spectra demonstrated D and G bands for nano-GO particles containing adhesives. HA-GO-2% group demonstrated uniform diffusion in adhesive, higher μTBS, adequate durability, and comparable resin tag development to controls.

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