Abstract

Experimental two-step universal adhesives (2-UAs) providing a particle-filled hydrophobic adhesive resin with a significant film thickness to hydrophobically seal the adhesive interface were designed and synthesized. This study aimed to characterize their interfacial interaction with dentin, to determine whether the 2-UA formulations achieve durable bonding to low C-factor flat dentin and to measure their water sorption. Bonding effectiveness of 2-UAs that combine a 10-MDP-based primer with hydrophobic adhesive resins differing only for filler (BZF-21, BZF-29, and BZF-29_hv) were comparatively investigated with the commercial adhesive Clearfil SE Bond 2 (C-SE2, Kuraray Noritake). Adhesive-dentin interfaces were characterized with TEM. Adhesive-resin disks were immersed in distilled water at 37°C for 1 week, 6 months and 1 year to measure water sorption and solubility. 'Immediate' and 'aged' micro-tensile bond strength (μTBS) of the adhesives applied in etch-and-rinse (E&R) and self-etch (SE) bonding mode to low C-factor flat dentin were measured. Statistical analyses involved linear mixed-effects (LME) modelling and Kruskal-Wallis testing (p<0.05). TEM revealed that E&R hybrid layers were more sensitive to aging than SE hybrid layers. Lower water sorption was recorded for all UAs compared with C-SE2. The immediate μTBS of BZF-21 and BZF-29 was not significantly different from that of C-SE2. The 1-year aged μTBS of all 2-UAs was significantly lower than that of C-SE2, except for BZF-29 applied in E&R mode. A significant reduction in μTBS upon 1-year aging was recorded for BZF-21 and BZF-29 applied in E&R mode. A significant difference in μTBS between E&R and SE bonding modes was recorded for all adhesives except BZF-21. Experimental 2-UAs with a hydrophobic adhesive-resin design produced±20-μm thick adhesive-resin layers, absorbed less water and resulted in bonding performance that was more aging-resistant when applied in SE than in E&R bonding mode. The silica-filled BZF-29 2-UA revealed the most comparable bonding performance with C-SE2 in a low C-factor condition (flat dentin).

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