This work aimed at characterizing the interface between dentin and the resin-infiltrated dentin made following the etching procedure that prepares for the bonding of tooth-colored restorations. The non-destructive measurement of fluid flow through the dentin-self-etch resin interface was followed repeatedly during a two year aging period. Two self-etch adhesive systems were selected for experiments on the evolution of permeability and evaluation of infrared spectral changes following the 24 month aging period. The adhesives contained water and a co-solvent, namely acetone for iBond, and t-butanol for Xeno V. For both adhesive systems, the permeability decreased during the first 3 months after etching, reaching values of -66.9 and -70.5% for iBond and Xeno V, respectively. Afterwards, the fluid flow slowly increased but still remained below 50% of the initial value following the 2-year aging period. The slow degradation of the resin-dentin interface, attributed to water impregnated collagen hydrolysis, is evidenced by these variations in fluid flow, and is also noted by the increase in water-related infrared absorption bands at 3300 cm(-1) and at 1600 cm(-1). The results are discussed in terms of co-solvent hydrophobicity, evaporation rate and viscosity together with resin infiltration depth and affinity for water.

The treatment of demineralized dentin with ethanol has been proposed as a way to improve hydrophobic monomer penetration into otherwise water saturated collagen fibrils. The ethanol rinse is expected to preserve the fibrils from collapsing while optimizing resin constituent infiltration for better long term adhesion. The physico-chemical investigations of demineralized dentin confirmed objectively these working hypotheses. Namely, Differential Scanning Calorimetry (DSC) measurements of the melting point of water molecules pointed to the presence of free and bound water states. Unfreezable water was the main type of water remaining following a rinsing step with absolute ethanol. Two different liquid water phases were also observed by Magic Angle Spinning (MAS) solid state Nuclear magnetic Resonance (NMR) spectroscopy. Infrared spectra of ethanol treated specimens illustrated differences with the fully hydrated specimens concerning the polar carbonyl vibrations. Optical microscopy observations as well as scanning electron microscopy showed an improved dentin-adhesive interface with ethanol wet bonding. The results indicate that water can be confined to strongly bound structural molecules when excess water is removed with ethanol prior to adhesive application. This should preserve collagen from hydrolysis upon aging of the hybrid layer.

Objectives: Our aim was to investigate the reaction mechanism of formation of the hybrid layer by a HEMA-containing self-etch adhesive and to study fluid filtration, contact angle and interfacial ultrastructure by SEM following a 1 year ageing period.Methods: Acidic behaviour and chemical interactions between Silorane System Adhesive and dentine were studied by potentiometric titrations, atomic absorption spectroscopy and infrared spectroscopy. The hydrophilicity of the adhesive was evaluated using the sessile drop method and dentine permeability by hydraulic conductance. The morphological study of the dentine/adhesive system interface was conducted using SEM.Results: The Silorane System Adhesive behaved as a multi-acid with several different pK(a) values. When the adhesive was in contact with dentine, the acid was progressively consumed and calcium ions were released. The acrylate substituted phosphonate bound strongly to apatite crystals. The polyacrylic acid copolymer reacted with calcium ions and formed an interpenetrating polymer network (IPN). Water contact angle measurements showed rapid spreading on primer (angles reached 15 degrees at 30 s) and larger contact angles when the Silorane bonding layer was added (from over 60 degrees to 44 degrees). A thick, homogeneous hybrid layer was observed both initially and after 1 year of ageing, with a corresponding hydraulic conductance of -48.50% initially and -52.07% at 12 months.Conclusion: The Silorane System Adhesive is capable of both dissolving calcium ions and binding to apatite surfaces. The results showed the hydrophilicity of the adhesive, which formed an IPN-like hybrid layer that conserved adequate impermeability over a 1-year period. (C) 2010 Elsevier Ltd. All rights reserved.