Search

X-ray photoelectron spectroscopy (XPS) is used to analyze 4-META resin and enamel that are debonded at an adhesive interface. The XPS spectra showed two chemical states for Ca: one resulted from Ca of hydroxyapatite and the other, an unknown chemical state, suggested that Ca was chemically bonded with 4-META. We postulate that for a chemical reaction of 4-META and hydroxyapatite, the chemical structure of carboxyl groups will resemble that of calcium phthalate. Hence, calcium phthalate was used as a reference material. Additionally, the spectra obtained from the adhesive interface and the mixture of calcium phthalate with hydroxyapatite particles were compared using peak deconvolution analysis. XPS analysis revealed that the chemical bond of 4-META with enamel resembled the chemical state of Ca in calcium phthalate. Consequently, we suggest that Ca of the enamel and the carboxyl group of 4-META were chelate-bonded at the interface.

The purpose of this study was to evaluate the durability of resin-dentin bonds in 10-yr water-storage testing. Resin-dentin bonded bulk specimens were prepared using six commercially available resin adhesives. The resin-dentin bonded specimens were stored in water for 24 h (control group) or for 10 yr (experimental groups). After each storage period, the specimens were sectioned to make specimen beams and then subjected to a microtensile bond test. After the bond test, fractured surfaces were examined by scanning electron microscopy (SEM). In addition, interfacial observation of silver nanoleakage was performed using the backscatter electron mode of SEM. The bond strengths of four of the six adhesive systems tested decreased significantly after 10 yr. However, no significant bond-strength reduction was recorded for the other two systems. The interfacial observations showed water tree propagation in the bonding resin layer as a typical morphological change after aging for five of the six adhesives tested. Water tree propagation may be a symptom of degradation in the resin bonding layer of resin-dentin bonds., ((c) 2010 The Authors. Journal compilation (c) 2010 Eur J Oral Sci.)

The purpose of this study was to evaluate the durability of one-bottle self-etching adhesive during long-term water-storage testing. Resin-dentin bonded specimens were prepared using four commercially available one-bottle self-etching adhesives. The specimens were sectioned perpendicular to the adhesive interface to produce beam-shaped specimens that were stored in water for 24 h (control group) and 100, 200, and 300 d (experimental groups). After each storage period, the beams were subjected to a microtensile bond test. After the bond test, fractured surfaces were examined using a scanning electron microscope. In addition, interfacial observations of the silver tracer were performed using the secondary and back-scatter modes of the scanning electron microscope. The bond strength of all tested adhesives decreased significantly after 100 or more days in water. The interfacial observations showed an oxygen-inhibition zone as electron lucent in the adhesive-composite border in control specimens, displaying silver impregnation with breakage after aging. The deterioration of the oxygen-inhibition zone in the adhesive-resin composite junction resulted in a decrease in bond strength after 100 d in water for one-bottle self-etching adhesives.

This study examined the effect of dentinal water on bonding, comparing one-bottle and two-step self-etching adhesives using microtensile bond test and scanning electron microscope. The bond strength of resin to dentin was measured for wet dentin (control) and dry dentin substrates. Wet dentin is the normal substrate for bond testing, whereas dry dentin was dehydrated in a desiccator at different drying times (5 to 60 min) before bonding. After bond testing, the fractured surfaces were examined. Although no correlation was found for two-step self-etching adhesives, the bond strength of the dry-dentin was significantly increased with the increase in the drying-time for one-bottle adhesives. With increased drying-time, the amount of water-bubbles was decreased for one-bottle adhesives; however, no bubble formation was seen in two-step adhesives in any group. The hydrophilic resin adhesive may entrap the water from dentin by osmosis during and after bonding. This effect may depend on the "hydrophilicity" of adhesives.

Gold alloys with Cu contents of 10 mass%, 20%, and 30% were used for morphological observation of porous surface structures after heating at 800 degrees C in air followed by pickling with acid solution. With increasing Cu content in the gold alloy, the internal oxidation zone became well-developed in the alloy matrix. The mechanism by which a porous structure was formed on the surface of a gold alloy containing only Cu as a base metal was thought to be as follows: Cu2O which formed along the grain boundaries acted as a diffusion path, permitting the penetration of O2- into the inner alloy matrix, and thereby resulting in internal oxidation occurring predominantly along the grain boundaries.

Objective: The purpose of this study was to improve adhesion between dental adhesive resins and 14K gold alloy by creating a sponge-like structure on the alloy surface which enhanced mechanical bonding., Methods: The internal oxidation particles of Cu oxides precipitated on a 14K gold alloy surface after high-temperature oxidation at 800 degrees C in air were removed by pickling with an acid solution to create a sponge-like structure on the alloy surface. A PMMA resin containing 4-META as an adhesive monomer and a self-cured resin without 4-META were used to examine the effects of mechanical and chemical factors on bond strength. A thiophosphate-type metal primer (M-Primer II) was used in combination with 4-META resin to strengthen the chemical bonding of 4-META resin to the porous alloy surface. The surfaces of the alloy specimen treated by oxidation, pickling, and bonding with 4-META resin were analyzed using an electron probe X-ray micro-analyzer., Results: SEM observation showed many resin tags on the resin side of the bond structure after removal of the gold alloy matrix with aqua regia. The bond strength of 4-META resin to the porous alloy surface was 38+/-3 (mean+/-SD) MPa whereas that to a flat alloy surface with the same composition was 19+/-1 MPa. The bond strength of a self-cured resin without 4-META to the porous alloy surface was 24+/-2 MPa., Significance: A high bond strength was obtained when 4-META resin was bonded to the porous 14K gold alloy surface treated with M-Primer II.

Self-etching primer adhesives have recently been introduced to simplify bonding. However, the fundamental bonding mechanism of self-etching primers to enamel is not yet fully understood. This study aimed to investigate resin-enamel bonds of self-etching primer adhesives on ground enamel. Two self-etching primer adhesives (Clearfil Liner Bond 2 V and Clearfil SE Bond) were used in this study. A total-etch adhesive (One-Step) was used as a control. Resin-enamel beams were subjected to the microtensile bond test. Subsequently, the failure modes of all specimens were quantified using image analysis. Undemineralized and demineralized ultrathin sections of the resin-enamel bonded specimens were examined using transmission electron microscopy. The bond strengths of Clearfil SE Bond (39.8 +/- 11.9 MPa) and One-Step (46.2 +/- 12.7 MPa) were significantly greater than that of Clearfil Liner Bond 2V (30.4 +/- 6.2 MPa). Scanning electron microscopy of the fractured surfaces revealed the failure direction and weakest portion within each bond. Transmission electron microscopy showed a thin hybridized complex of resin in enamel produced by the self-etching primers without the usual micrometer-sized resin tags seen in resin-enamel bonds produced using the total-etch adhesive. The morphological features of the resin-enamel bonds produced by two self-etching primers tested were different from that created with the total-etch adhesive.

Our knowledge of the mechanisms responsible for the degradation of resin-dentin bonds are poorly understood. This study investigated the degradation of resin-dentin bonds after 1 year immersion in water. Resin-dentin beams (adhesive area: 0.9mm(2)) were made by bonding using a resin adhesive, to extracted human teeth. The experimental beams were stored in water for 1 year. Beams that had been stored in water for 24h were used as controls. After water storage, the beams were subjected to microtensile bond testing. The dentin side of the fractured surface was observed using FE-SEM. Subsequently, these fractured beams were embedded in epoxy resin and examined by TEM. The bond strength of the control specimens (40.3+/-15.1MPa) decreased significantly (p<0.01) after 1 year of water exposure (13.3+/-5.6MPa). Loss of resin was observed within fractured hybrid layers in the 1 year specimens but not in the controls. Transmission electron microscopic examination revealed the presence of micromorphological alterations in the collagen fibrils after 1 year of water storage. These micromorphological changes (resin elution and alteration of the collagen fibrils) seem to be responsible for the bond degradation leading to bond strength reduction.

Various types of resin adhesives and procedures are available in the clinical field, so comprehensive understanding of degradation is required for each material and bonding procedure. The objective of this study was to investigate the bond durability for different adhesives and bonding procedures. Resin-dentin bonded beams were prepared with the use of two adhesives (One-Up Bond F/self-etching primer system and One Bond/total-etch adhesive) and two experimental groups for the bonding procedure (wet and dry bonding of the total-etch adhesive). Those samples were soaked in water for 24 h(control), 6 and 12 months. After the water immersion, the bond strengths were measured by the microtensile bond test, and subsequently fractography was performed with the use of SEM. Statistically significant reduction of the bond strength (p < 0.05) was apparent after 12 months of water exposure in the range 22-48% of the control. The bonding resin was eluted from the hybrid layer of the self-etching and the total-etch adhesives for the wet bonding. Micromorphological alterations were found due to the hydrolysis of collagen fibrils with the total-etch adhesive for the dry bonding mode. These pathologic alterations were in accord with the bond strength., (Copyright 2003 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater 66B: 324-330, 2003)

Purpose: To characterize resin-dentin bond structures of three adhesive resin systems using fractographic analysis to measure the area of failure at the fractured surface. Materials and Methods: Flat dentin surfaces were ground perpendicular to the long axis of the tooth. The prepared dentin surfaces were treated by one of three adhesive resin systems (Mac Bond II, One-Step, and Single Bond). The samples were sectioned perpendicular to the adhesive interface to produce a square bar-shaped specimen (adhesive area: 0.9 mm²) using a diamond saw. A micro-tensile test was then conducted at a crosshead speed of 1.0 mm/min. The mean tensile bond strengths were statistically compared using one-way ANOVA and Fisher's PLSD test (P< 0.05). The fractured surfaces of all specimens were examined using SEM and the area of failure was measured using an image analyzer on SEM microphotographs. Results: No significant differences in tensile bond strength were observed between Single Bond (62.1 ± 18.2 MPa) and One-Step (53.8 ± 13.1 MPa) (P > 0.05). However, the bond strength of Mac Bond II (36.5 ± 13.7 MPa) was significantly lower than that of One-Step or Single Bond (P< 0.05). At the fractured surface, except for the cohesive failure of the bonding resin and resin-based composite, different failure patterns were observed for each resin system as follows: the failure of the hybrid layer and demineralized dentin was observed in the two wet bonding systems (One-Step and Single Bond) and of the hybrid layer but not the demineralized dentin in the self-etching primer system (Mac Bond II). The results demonstrated that the integrity of the hybrid layer depends on the adhesive system. [ABSTRACT FROM AUTHOR]