Characterization of Micro- and Nanophase Separation of Dentin Bonding Agents by Stereoscopy and Atomic Force Microscopy

The aim was to study the effect of solvents on the phase separation of four commercial dental adhesives. Four materials were tested: Clearfil (TM) SE Bond (CSE), Clearfil Protect Bond (CPB), Clearfil S3 Bond (CS3), and One-Up Bond F Plus (OUB). Distilled water or ethanol was used as a solvent (30 vol%) for microphase separation studies, by stereoscopy. For nanophase images, the mixtures were formulated with two different solvent concentrations (2.5 versus 5 vol%) and observed by atomic force microscopy. Images were analyzed by using MacBiophotonics ImageJ to measure the area of bright domains. Macrophase separations, identified as a loss of clarity, were only observed after mixing the adhesives with water. Nanophase separations were detected with all adhesive combinations. The area of bright domains ranged from 132 to 1,145 nm(2) for CSE, from 15 to 285 nm(2) for CPB, from 149 to 380 nm(2) for CS3, and from 26 to 157 nm(2) for OUB. In water-resins mixtures, CPB was the most homogeneous and OUB showed the most heterogeneous phase formation. In ethanol-resin mixtures, CSE attained the most homogeneous structure and OUB showed the most heterogeneous phase. Addition of 5 vol% ethanol to resins decreased the nanophase separation when compared with the control materials.