Effects of a peripheral enamel bond on the long-term effectiveness of dentin bonding agents exposed to water in vitro

This study evaluated the effects of water exposure on the in vitro microtensile bond strength (muTBS) of etch-and-rinse and self-etching adhesives to human dentin over a 1-year storage period. Five adhesive systems used were as follows: a one-step self-etching adhesive (One-up Bond F-OB), two two-step self-etching primers (Clearfil SE Bond-SE and Clearfil Protect Bond-CP), and two etch-and-rinse adhesives (Single Bond-SB and Prime&Bond NT-PB). Dentin surfaces were bonded, restored, and assigned to four subgroups, according to the degree of water exposure: 24 h of peripheral water exposure (24 h-PE) (having circumferential enamel); and 1 year of peripheral exposure (1 yr-PE), direct exposure (1 yr-DE) (dentin directly water-exposed), or directly exposed to oil only (no water exposure) (1 yr-DOE). A composite-enamel bond adjacent to the restoration is determined if the water exposure was peripheral or direct. After storage periods, specimens were serially sectioned, trimmed to an hourglass shape with a cross-sectional area of 1 mm(2) at the interface, and tested in tension. Results were analyzed by two-way ANOVA and Tukey test (alpha = 0.05). No difference was found between 24 h-PE and 1 yr-PE for OB, CP, SB, and PB. However, muTBS values significantly dropped after 1 yr-DE for SE, CP, SB, and PB. A decreased muTBS was seen in SE after 1 yr-PE, but no differences existed between 1 yr-PE and 1 yr-DE. Similar or increased muTBS values were noted in 1 yr-DOE for all adhesives. Water-storage for 1 year significantly decreased muTBS for all adhesives. However, except for SE, the presence of a peripheral composite-enamel bond seemed to reduce the degradation rate in resin-dentin interfaces for all materials.     

Differential effect of in vitro degradation on resin-dentin bonds produced by self-etch versus total-etch adhesives

OBJECTIVE: To evaluate the effect of an in vitro challenge (NaOCl immersion) on microtensile bond strength (MTBS) of five adhesive systems to dentin. METHODS: Flat dentin surfaces from 40 molars were bonded with three total-etch adhesives (Single Bond, Prime&Bond NT and the experimental Prime&Bond XP), and two self-etching agents (Clearfil SE Bond and Etch&Prime 3.0). Composite build-ups were constructed with Tetric Ceram. Teeth were then sectioned into beams of 1.0 mm2 cross-sectional area. Half of the beams were immersed in 10% NaOCl aqueous solution for 5 h. Each beam was tested in tension in an Instron machine at 0.5 mm/min. Data were analyzed by 2-way ANOVA and multiple comparisons tests (p < 0.05). RESULTS: Clearfil SE Bond and Single Bond attained higher MTBS than the other three adhesives. Prime&Bond NT and Prime&Bond XP performed equally, and Etch&Prime resulted in the lowest MTBS. After NaOCl immersion, MTBS decreased in all groups. The highest MTBS values were obtained for Clearfil SE Bond and Prime&Bond XP. Scaning electron microscopy observation of debonded sticks evidenced dissolution and microstructural alterations of intertubular dentin, except when Clearfil SE Bond was used. CONCLUSIONS: Resin-dentin bonds are prone to chemical degradation. The extent of the resin degradation is adhesive system specific. Chemical degradation of the nonresin infiltrated collagen fibers does also exist in total-etch adhesives. Both processes may reduce long-term resin-dentin bond strength.     

Characterisation of resin-dentine interfaces by compressive cyclic loading

The aims of this in vitro study were to evaluate the ultra-morphological changes in resin-dentine interfaces after different amounts of thermomechanical load (TML), and to determine the corresponding microtensile bond strengths (microTBS). Enamel/dentine discs with a thickness of 2 mm were cut from 24 human third molars and bonded with four adhesives involving different adhesion approaches: Syntac (Ivoclar Vivadent; used as multi-step etch-and-rinse adhesive), Clearfil SE Bond (Kuraray; two-step self-etch adhesive), Xeno III (Dentsply DeTrey; mixed all-in-one self-etch primer adhesive system), and iBond (Heraeus Kulzer; non-mixed all-in-one self-etch adhesive). The resin-dentine discs were cut into beams (width 2 mm; 2 mm dentine, 2 mm resin composite) and subsequently subjected to cyclic TML using ascending amounts of mechanical/thermal cycles (20 N at 0.5 Hz of mechanical load and 5-55 degrees C of thermal cycles: for 0/0, 100/3, 1,000/25, 10,000/250, 100,000/2,500 cycles). Loaded specimens were either cut perpendicularly in order to measure microTBS (n=20; crosshead speed: 1 mm/min) or were immersed in an aqueous tracer solution consisting of 50 wt% ammoniacal silver nitrate and processed for ultra-morphological nanoleakage examination using transmission electron microscopy (TEM). microTBS were significantly decreased by increasing amounts of TML for all adhesives (p<0.05). Bond strengths after 0 vs. 100,000 thermomechanical cycles were: Syntac: 41.3/30.1 MPa; Clearfil SE Bond 44.8/32.5 MPa; Xeno III 27.5/13.7 MPa; iBond 27.0/6.2 MPa. Relatively early, a certain amount of nanoleakage was observed in all groups by TEM, which was more pronounced for Xeno III and iBond. The incidence of nanoleakage remained stable or was even reduced with increasing load cycles for all adhesives except iBond, where exact failure origins were detected within the adhesive and at the top of the hybrid layer.     

In vitro effect of nanoleakage expression on resin-dentin bond strengths analyzed by microtensile bond test, SEM/EDX and TEM

This study evaluated the effect of multiple consecutive adhesive resin coatings of adhesive bonded to human dentin on nanoleakage and resin-dentin bond strength. Resin bonded dentin specimens were prepared using a total-etch adhesive (One-Step Plus) applied as multiple consecutive coating, or using two self-etch adhesive systems (iBond or Fluoro Bond). For the total-etch adhesive, resin application and air evaporation were performed 1, 2, 3, or 4 times. The self-etch adhesives were applied according to manufacturers' instructions. Resin-dentin bonded beams were prepared and immersed in water (control) or ammoniacal silver nitrate. After storage, microtensile bond strengths were measured. The fractured surfaces were examined by scanning and transmission electron microscopy (SEM and TEM), and energy-dispersive X-ray spectrometry (EDX). No significant differences in bond strength were found between water and silver nitrate storage groups. Several types of silver depositions (spotted, reticular, or water trees) were found in adhesive joints. The bond strengths of the single coated specimens of the total-etch adhesive were significantly lower than those receiving 2-4 coatings. Single coats produced more nanoleakage than multiple coats. However, no correlation was found between the bond strengths and nanoleakage between the different adhesives (total-etch adhesive with different conditions or self-etch adhesives).     

Initial adhesion of glass-fiber-reinforced composite to the surface of porcine calvarial bone

The aim of this preliminary study was to compare the initial bond strength of the glass-fiber-reinforced composite veil to the surface of the porcine calvarial compact bone using different adhesives. Fiber-reinforced composite (FRC) made of E-glass fiber veil with the BisGMA-PMMA resin system was used in the study. For the shear bond strength test, porcine calvarial bone cubes were mounted into resin matrix. FRC-veil discs were bonded to compact bone with different types of adhesives: (A) BisGMA-HEMA based (3M-ESPE Scotchbond Multi-Purpose Adhesive), (B) 4-META/UDMA/BisGMA based (Unifil Bond Bonding Agent) and MDP based (Clearfil Se Bond adhesive), (C) UDMA/BisGMA/PMMA-based experimental adhesive, and (D) silane-based (APS, ICS, MPS) experimental adhesives. The surface of the bone was mechanically roughened and was either used as such, treated with dental primers (Unifil Bond Self-etching Primer, Clearfil Se Bond Primer), or treated with an experimental silane mixture (APS, ICS, MPS), or with a mixture of the experimental silane liquid and Clearfil Se Bond Primer. The 3M-ESPE Scotchbond Multi-Purpose Adhesive and UDMA/BisGMA/PMMA experimental adhesive gave poor results in the shear bond test (0.58 and 0.40 MPa, respectively). Unifil Bond Bonding Agent and Clearfil Se Bond adhesive with respective primers markedly improved the shear bond strength; with Unifil the result was 3.40 MPa, and with Clearfil it was 6.19 MPa. When the bone surface was primed with a mixture of Clearfil Se Bond Primer and Clearfil Porcelain Bond Activator, the Clearfil Se Bond adhesive-impregnated FRC veil gave the best adhesion to the bone surface in this test: 9.50 MPa. The addition of bioactive glass granules between the veil and the bone lowered the shear bond strength in the test system described above to 6.72 MPa. The test systems with the silane mixture were also promising. In the SEM study, it was found that the mechanical treatment reveals the pores of the bone surface. Chemical treatments of the bone surface improved the adhesion of the FRC veil to the bone. The results showed that the adhesion of the FRC to the surface of the bone can be significantly improved with mechanical roughening and with special chemical treatments of the bone surface.     

Degradation patterns of different adhesives and bonding procedures

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.     

Effect of cyclic loading on bonding of fiber posts to root canal dentin

This study evaluated the effect of mechanical loading on microtensile bond strength (MTBS) when luting fiber posts to root canal dentin. Forty maxillary premolars were endodontically treated, and the roots were prepared for post cementation using the FRC Postec system. A light-cured composite (Clearfil Photo Core, Kuraray) was used in combination with four adhesive systems: Single Bond (3M ESPE), Multilink Primer (Vivadent), Clearfil Photo Bond (Kuraray), and Clearfil New Bond (Kuraray). A composite build-up was performed around the root to provide adequate gripping during testing. For each experimental group, half of the specimens were load cycled under 90 N (5000 cycles, 3 cycles/s). Specimens were cut to obtain beams with the post in the center and with the radicular dentin overlaid by the composite build-up on each side. Microtensile testing was performed with a universal testing machine at a cross-head speed of 0.5 mm/min. The failure mode was classified under a stereomicroscope. ANOVA and Student-Newman-Keuls multiple comparison tests were performed. After 24 h, all adhesives performed similarly. When specimens were subjected to mechanical loading, decreases in MTBS were observed for Clearfil New Bond and Multilink Primer.     

Adhesion to chondroitinase ABC treated dentin

Dentin bonding relies on complete resin impregnation throughout the demineralised hydrophilic collagen mesh. Chondroitin sulphate-glycosaminoglycans are claimed to regulate the three-dimensional arrangement of the dentin organic matrix and its hydrophilicity. The aim of this study was to investigate bond strength of two etch-and-rinse adhesives to chondroitinase ABC treated dentin. Human extracted molars were treated with chondroitinase ABC and a double labeling immunohistochemical technique was applied to reveal type I collagen and chondroitin 4/6 sulphate distribution under field emission in-lens scanning electron microscope. The immunohistochemical technique confirmed the effective removal of chondroitin 4/6 sulphate after the enzymatic treatment. Dentin surfaces exposed to chondroitinase ABC and untreated specimens prepared on untreated acid-etched dentin were bonded with Adper Scotchbond Multi-Purpose or Prime and Bond NT. Bonded specimens were submitted to microtensile testing and nanoleakage interfacial analysis under transmission electron microscope. Increased mean values of microtensile bond strength and reduced nanoleakage expression were found for both adhesives after chondroitinase ABC treatment of the dentin surface. Adper Scotchbond Multi-Purpose increased its bond strength about 28%, while bonding made with Prime and Bond NT almost doubled (92% increase) compared to untreated specimens. This study supports the hypothesis that adhesion can be enhanced by removal of chondroitin 4/6 sulphate and dermatan sulphate, probably due to a reduced amount of water content and enlarged interfibrillar spaces. Further studies should validate this hypothesis investigating the stability of chondroitin 4/6 and dermatan sulphate-depleted dentin bonded interface over time.     

Effect of load cycling and in vitro degradation on resin-dentin bonds using a self-etching primer

The objective of this study was to evaluate the effect of in vitro degradation and mechanical loading on microtensile bond strength (MTBS) and microleakage (ML) of a resin composite to dentin using a self-etching primer adhesive [Clearfil SE Bond (SEB)] under two hydration statuses. Twenty-four flat dentin surfaces were divided in groups: 1) blot-dried, 2) air-dried. SEB was applied and resin buildups were performed with Tetric Ceram. Specimens were divided in four subgroups: a) sectioned into beams, b) load cycled, c) beams were immersed in NaOCl for 5 h, d) load cycled and immersed in NaOCl. Beams were tested in tension. For ML testing, 80 Class V cavities were prepared and molars divided in subgroups as described above (in group c and d, specimens were kept in distilled water for 1 year, instead of the 5-h NaOCl immersion). ML was assessed by dye penetration. Analysis of variance and multiple comparisons tests were used for MTBS. For ML, Mann-Whitney U and Wilcoxon matched pairs signed ranked were used (p<0.05). SEB applied to completely dehydrated dentin produced the highest MTBS, at 24-h evaluation. In vitro degradation always decreased MTBS, and fatigue loading only diminished MTBS on dehydrated dentin. Load cycling increased dye penetration on dentin margins. Degradation always increased ML in both enamel and dentin margins.     

Microtensile bond strength of etch and rinse versus self-etch adhesive systems

The aim of this study was to compare the microtensile bond strength of the etch and rinse adhesive versus one-component or two-component self-etch adhesives. Twelve intact human molar teeth were cleaned and the occlusal enamel of the teeth was removed. The exposed dentin surfaces were polished and rinsed, and the adhesives were applied. A microhybride composite resin was applied to form specimens of 4?mm height and 6?mm diameter. The specimens were sectioned perpendicular to the adhesive interface to produce dentin-resin composite sticks, with an adhesive area of approximately 1.4?mm(2). The sticks were subjected to tensile loading until failure occurred. The debonded areas were examined with a scanning electron microscope to determine the site of failure. The results showed that the microtensile bond strength of the etch and rinse adhesive was higher than that of one-component or two-component self-etch adhesives. The scanning electron microscope examination of the dentin surfaces revealed adhesive and mixed modes of failure. The adhesive mode of failure occurred at the adhesive/dentin interface, while the mixed mode of failure occurred partially in the composite and partially at the adhesive/dentin interface. It was concluded that the etch and rinse adhesive had higher microtensile bond strength when compared to that of the self-etch adhesives.     

A challenge to the conventional wisdom that simultaneous etching and resin infiltration always occurs in self-etch adhesives

This study provided morphological evidence that discrepancies between the depth of demineralisation and the depth of resin infiltration can occur in some mild self-etch adhesives. Sound dentine specimens derived from extracted human third molars were bonded with 5 one-step and 5 two-step self-etch adhesives. One millimeter thick slabs containing the resin-dentine interfaces were immersed in 50 wt% aqueous ammoniacal silver nitrate and processed for TEM examination. A zone of partially etched but uninfiltrated dentine was identified beneath the hybrid layers in the milder versions of both one-step and two-step self-etch adhesives. This zone was characterised by the occurrence of silver deposits along the interfibrillar spaces of mineralised collagen fibrils. The silver infiltrated interfibrillar spaces were clearly identified from the one-step self-etch adhesives Xeno III, iBond, Brush&Bond and the experimental adhesive, and were thinner and only occasionally observed in the two-step self-etch adhesives Clearfil SE Bond and Clearfil Protect Bond. The more aggressive one-step and two-step adhesives that exhibit more abrupt transitions from completely demineralised to mineralised dentin were devoid of these silver-infiltrated interfibrillar spaces beneath the hybrid layers. Incomplete resin infiltration observed in some self-etch adhesives may be caused by the reduced etching potential of the acidic monomers toward the base of hybrid layers, or the presence of acidic but non-polymerisable hydrolytic adhesive components, creating potential sites for the degradation of the bonded created by these self-etch adhesives.     

Effect of light-cure time of adhesive resin on the thickness of the oxygen-inhibited layer and the microtensile bond strength to dentin

A thick oxygen-inhibited layer (OIL) on a cured adhesive layer (AL) is believed to result in both good adaptation of composite resin (CR) and high bond strength. A high degree of conversion (DC) of the AL is also needed for durable bonding. This study evaluated the hypothesis that increasing the DC by prolonging the light-curing time of adhesive bonding resin might decrease the bond strength of the adhesive to dentin because of the subsequent thinning of the OIL thickness. The OIL thickness and the DC of solvent-removed One Step and D/E bonding resin of All Bond 2 (Bisco, USA) were measured simultaneously with FT-NIR spectroscopy according to increasing light-cure times (10, 20, 30, and 60 s) so as to evaluate their effect on the microtensile bond strength. The bonded interfaces were evaluated using scanning electron microscopy. Excessive irradiation of light-curing adhesives increased the DC, but decreased the OIL thickness. When the OIL was significantly thin by curing the adhesives for 30 or 60 s, defects were observed at the interface between the AL and the CR, as well as at the interface between the AL and the hybrid layer. When the OIL was thick, free radicals from the overlying CR may have diffused into the unreacted monomer mixtures of the OIL, chemically connecting the cured AL and the newly curing composite. It was found that to obtain maximum dentin bond strength, light-curing adhesives should be cured for the irradiation time recommended by the manufacturer.     

Nanoleakage and microshear bond strength in deproteinized human dentin

This study evaluated the influence of dentin deproteinization with NaOCl on the microshear bond strength (microSBS) and the nanoleakage patterns of three dentin bonding systems (DBS). Occlusal dentin surfaces, obtained from extracted noncarious human molars, were divided into two experimental groups, according to dentin surface treatment: Group I-37% H(3)PO(4)/15s and Group II-37% H(3)PO(4)/15s + 10% NaOCl/1 min. The dentin surfaces were bonded with one of the following DBS: Scotchbond Multipurpose-SBMP, Prime & Bond NT-PB and Clearfil SE Bond-SE. After 1 week storage in water at 37 degrees C, the specimens were subjected to the microSBS test. The data were analyzed by two-way ANOVA and Student-Newman-Keuls' test (p = 0.05). The nanoleakage was evaluated using scanning electron microscopy (SEM) in backscattered electron imaging regime. No significant difference in microSBS between dentin treatments was found for SBMP. For PB, microSBS increased after NaOCl dentin treatment. SE showed a reduction in microSBS in deproteinized specimens. SEM analysis showed different nanoleakage patterns for each DBS. Irrespective of dentin treatments, all SBMP specimens showed nanoleakage. SE did not show nanoleakage with the two dentin treatments. PB showed nanoleakage within the hybrid layer only in acid-etched specimens. The influence of dentin deproteinization was dependent on the dentin bonding system formulation.     

In vitro microTBS of one-bottle adhesive systems: sound versus artificially-created caries-affected dentin

This in vitro study aimed to evaluate a pH-cycling model for simulation of caries-affected dentin (CAD) surfaces, by comparing the bond strength of etch-and-rinse adhesive systems on sound and artificially-created CAD. Dentin substrates with different mineral contents and morphological patterns were created by submitting buccal bovine dentin to the following treatments: (1) immersion in artificial saliva during the experimental period (sound dentin, SD), or (2) induction to a CAD condition by means of a dynamic pH-cycling model (8 cycles, demineralization for 3 h followed by mineralization for 45 h). The bond strength of Excite or Prime and Bond NT adhesive systems was assessed using the microtensile bond strength (microTBS) test. Dentin microhardness was determined by cross-sectional Knoop evaluations. Resin-dentin morphology after the treatments was examined by scanning electron microscopy. SD produced significantly higher microTBS than CAD for both adhesives evaluated, without differences between materials. CAD exhibited lower microhardness than SD. Morphological analysis showed marked distinctions between SD and CAD bonded interfaces. Under the conditions of this study, differences in morphological pattern and dentin mineral content may help to explain resin-dentin bond strengths. The proposed pH-cycling model may be a suitable method to simulate CAD surfaces for bonding evaluations.     

Micro-tensile bond strength of sound and caries-affected primary tooth dentin measured with original designed jig

To measure the micro-tensile bond strength (MTBS) on sound and caries-affected primary tooth dentin using an original designed jig that was developed for making symmetric and uniformly-sized specimens for the micro-tensile strength testing. The MTBS of dumbbell-shaped specimens and matchstick-shaped specimens were measured. Dumbbell-shaped specimens: The occlusal surfaces of 15 sound primary molars were ground with a water-cooled air turbine using a diamond bur. The adhesive systems and resin-based composites were Clearfil SE Bond and Clearfil AP-X (SE group) and Single Bond and Z250 (SB group). Matchstick-shaped specimens: Sixteen primary molars (5 sound and 11 carious) were used. The occlusal surfaces of sound teeth were ground with a water-cooled air turbine using a diamond bur. Infected dentin was determined by a caries detecting dye solution and removed with a round-shaped steel bur under water-cooling and with a hand instrument. SE was applied. Data was statistically analyzed using ANOVA and Fisher's PLSD at p < 0.05. The MTBSs (MPa) for the dumbbell-shaped specimens were 8.9 +/- 7.0 in the SE group and 10.3 +/- 5.8 in the SB group and that for the matchstick-shaped specimens were 9.0 +/- 6.3 in the sound-SE group and 9.2 +/- 5.8 in the carious-SE group. No significant difference was observed among them.     

Effects of adhesive systems and luting agents on bonding of fiber posts to root canal dentin

The study evaluated the influence of different luting materials on the microtensile bond strength of glass fiber posts to root canal dentin. Thirty extracted maxillary premolars were endodontically treated, and the roots were prepared for post cementation using the FRC Postec system (Vivadent). Two luting materials (Multilink, Vivadent and Clearfil Photo Core, Kuraray) were used in combination with three adhesive: Multilink Primer (Vivadent), Clearfil Photo Bond, and Clearfil New Bond (Kuraray). A composite build-up was performed around the root to provide adequate gripping during testing. Specimens were cut to obtain beams with the post in the center and with the radicular dentin overlaid by the composite build-up on each side. Microtensile testing was performed with a universal testing machine at a cross-head speed of 0.5 mm/min. The failure mode was classified under a stereomicroscope and four representative beams of each group were selected for SEM analysis. Bond strength data that were analyzed with two-way ANOVA and Student-Newman-Keuls multiple comparisons tests revealed that adhesive systems, luting materials, and the interaction between these two factors significantly influenced the bond strength results (p < 0.01). Multilink applied with its own adhesive system obtained the best results, while the lowest bond strength was achieved with clearfil photo core in combination with multilink primer.     

Bonding performance of different adhesive systems to deproteinized dentin: microtensile bond strength and scanning electron microscopy

Deproteinization has been shown to optimize dentin bonding, but differences in adhesive composition should be considered. The objective of this study was to evaluate the effect of dentin deproteinization on microtensile bond strength (microTBS) of four total-etch adhesive systems (Single Bond/SB, Prime & Bond NT/PB, One Coat Bond/OC, and PQ1/PQ). The ultrastructure of the resin-dentin interfaces was also examined using scanning electron microscopy. Tukey's multiple-comparison tests indicated that PB and PQ produced significantly higher microTBS (p<0.05) after dentin deproteinization (PB=61.53 MPa, PQ=58.18 MPa). This treatment provided statistically lower results for SB (39.08 MPa), but the microTBS of OC to dentin was unaffected by dentin deproteinization. The bonding performance on deproteinized dentin surfaces depended on the characteristics of each adhesive system, as well as the adhesive dentin specificity to the oxidant effect of sodium hypochlorite. Incorporation of fillers in the adhesive, a possible self-etching action, and the presence of a volatile solvent (acetone) were the main factors for a better union between the adhesive system and deproteinized substrate.     

Nanoleakage within the hybrid layer: a correlative FEISEM/TEM investigation

The aim of this study was to compare the nanoleakage patterns of the resin-dentin interfaces of three dentin bonding systems at both TEM and field emission in lens SEM (FEI-SEM) levels. A standardized smear layer was created with 180-grit silicon carbide paper (SiC) on dentin disks obtained from 18 noncarious human third molars. Specimens were randomly divided into three groups and bonded with a two-step total etching adhesive (Single Bond, SB), a two-step, self-etching adhesive (Clearfil SE BOND, SEB), and a one-step, self-etching adhesive (XENO III, XEIII). Nanoleakage was evaluated by using an ammoniacal silver-nitrate solution. Specimens were processed for TEM and FEI-SEM observation. The TEM of SB revealed silver deposits in adhesive and hybrid layers (HL). High-magnification FEI-SEM micrographs clearly identified these deposits as spherical clusters mainly associated with nonembedded collagen fibrils. TEM and FEI-SEM examination of SEB revealed some clusters of silver deposits within porosities and small channels of the HL. Additional silver deposits were observed between the peritubular dentin walls and the resin tags. XEIII revealed very fine and diffuse silver grains throughout the entire HL. SEM visualization of nanoleakage at a high level of resolution has not been previously described. FEI-SEM technology supported the TEM visualization with three-dimensional morphological data of the relations between the HL constituents and nanoleakage. The results of the present study confirm the hypothesis that both total- and self-etch adhesives are not able to fully infiltrate the dentin substrate.     

Elemental distributions and microtensile bond strength of the adhesive interface to normal and caries-affected dentin

The aim of this study was to evaluate the microtensile bond strength (microTBS) and the elemental contents of the adhesive interface created to normal versus caries-affected dentin. Extracted human molars with coronal carious lesions were used in this study. A self-etching primer/adhesive system (Clearfil Protect Bond) was applied to flat dentin surfaces with normal and caries-affected dentin according to the manufacturer's instructions. After 24 h water storage, the bonded specimens were cross-sectioned and subjected to a microTBS test and electron probe microanalysis for the elemental distributions [calcium (Ca), phosphorus (P), magnesium (Mg), and nitrogen (N)] of the resin-dentin interface after gold sputter-coating. The microTBS to caries-affected dentin was lower than that of normal dentin. The demineralized zone of the caries-affected dentin-resin interface was thicker than that of normal dentin (approximately 3 microm thick in normal dentin; 8 microm thick in caries-affected dentin), and Ca and P in both types of dentin gradually increased from the interface to the underlying dentin. The caries-affected dentin had lost most of its Mg content. The distributions of the minerals, Ca, P, and Mg, at the adhesive interface to caries-affected dentin were different from normal dentin. Moreover, a N peak, which was considered to be the collagen-rich zone resulting from incomplete resin infiltration of exposed collagen, was observed to be thicker within the demineralized zone of caries-affected dentin compared with normal dentin.     

Adhesive performance of dentin bonding agents applied in vivo and in vitro. Effect of intrapulpal pressure and dentin depth

The purpose of this study was to evaluate the influence of intrapulpal pressure and dentin depth on bond strengths of an etch-and-rinse and a self-etching bonding agent to dentin in vitro and in vivo. Twenty-four pairs of premolars were randomly divided into four groups (n = 6) according to the dentin bonding agent, Single Bond and Clearfil SE Bond, and intrapulpal pressure, null or positive. Each tooth of the pair was further designated to be treated in vivo or in vitro. The intrapulpal pressure was controlled in vivo by the delivery of local anesthetics containing or not a vasoconstrictor, while in vitro, it was achieved by keeping the teeth under hydrostatic pressure. Class I cavities were prepared and the dentin bonding agents were applied followed by incremental resin restoration. For the teeth treated in vitro, the same restorative procedures were performed after a 6 month-storage period. Beams with 1 mm(2) cross-sectional area were prepared and microtensile tested. Clearfil SE Bond was not influenced by any of the variables of the study, while bond strengths produced in vitro were significantly higher for Single Bond. Overall, lower bond strengths were produced in deep dentin, which reached statistical significance when Single Bond was applied under physiological or simulated intrapulpal pressure. In conclusion, in vitro bonding may overestimate the immediate adhesive performance of more technique-sensitive dentin bonding systems. The impact of intrapulpal pressure on bond strength seems to be more adhesive dependent than dentin morphological characteristics related to depth.