Adhesive phase separation at the dentin interface under wet bonding conditions

Under in vivo conditions, there is little control over the amount of water left on the tooth and, thus, there is the danger of leaving the dentin surface so wet that the bonding resin undergoes physical separation into hydrophobic and hydrophilic-rich phases. The purpose of this study was to investigate phase separation in 2,2-bis[4(2-hydroxy-3-methacryloyloxy-propyloxy)-phenyl] propane (BisGMA)-based adhesive using molecular microanalysis and to examine the effect of phase separation on the structural characteristics of the hybrid layer. Model BisGMA/HEMA (hydroxyethl methacrylate) mixtures with/without ethanol and commercial BisGMA-based adhesive (Single Bond) were combined with water at concentrations from 0 to 50 vol%. Macrophase separation in the BisGMA/HEMA/water mixtures was detected using cloud point measurements. In parallel with these measurements, the BisGMA/HEMA and adhesive/water mixtures were cast as films and polymerized. Molecular structure was recorded from the distinct features in the phase-separated adhesive using confocal Raman microspectroscopy (CRM). Human dentin specimens treated with Single Bond were analyzed with scanning electron microscopy (SEM) and CRM mapping across the dentin/adhesive interface. The model BisGMA/HEMA mixtures with ethanol and the commercial BisGMA-based adhesive experienced phase separation at approximately 25 vol% water. Raman spectra collected from the phase-separated adhesive indicated that the composition of the particles and surrounding matrix material was primarily BisGMA and HEMA, respectively. Based on SEM analysis, there was substantial porosity at the adhesive interface with dentin. Micro-Raman spectral analysis of the dentin/adhesive interface indicates that the contribution from the BisGMA component decreases by nearly 50% within the first micrometer. The morphologic results in corroboration with the spectroscopic data suggest that as a result of adhesive phase separation the hybrid layer is not an impervious 3-dimensional collagen/polymer network but a porous web characterized by hydrophobic BisGMA-rich particles distributed in a hydrophilic HEMA-rich matrix.     

Chemical profile of adhesive/caries-affected dentin interfaces using Raman microspectroscopy

In clinical practice, dentists must frequently bond adhesives to caries-affected dentin substrates, but the bond that characteristically forms with these substrates does not provide the durability necessary for long-term clinical function. The purpose of this study was to characterize and compare the interfacial chemistry of adhesive with caries-affected and noncarious dentin using micro-Raman spectroscopy. The results indicated that the differences in the Raman spectra between noncarious and caries-affected dentin could not be accounted for by simple decreased mineralization. Both the structure of collagen and mineral in the caries-affected dentin has been altered by the caries process. The differences in structure and composition not only interfered with acid-etching process but also subsequent resin monomer penetration. It was shown that the interface between the adhesive and caries-affected dentin was wider and more complicated than that of the adhesive and noncarious dentin. As a result of adhesive phase separation, a structurally integrated hybrid layer did not form at the interface with either caries-affected or noncarious dentin. Using chemical imaging techniques, this study provides the direct evidence of adhesive phase separation at the interface with caries-affected dentin. Although our group previously reported adhesive phase separation at the interface with noncarious dentin, the chemistry of caries-affected dentin leads to greater variability and a more highly irregular composition along the length and breadth of the interface.     

Overestimating hybrid layer quality in polished adhesive/dentin interfaces

The most popular techniques for determining the quality of the hybrid layer (HL) have relied on morphologic characterization of the polished adhesive/dentin (a/d) interfaces before and after acid-bleach chemical treatment. Using these techniques, the existence of smooth, acid-resistant layers has been consistently reported for most adhesive systems. The purpose of this study was to determine whether popular specimen preparation techniques that include polishing and acid-bleach treatment modify the a/d interface, mask the complexity of the HL, and lead to inaccurate assessment of the quality of the HL. To understand the impact of specimen preparation techniques on the morphology of the resin-dentin interface, polished and unpolished specimens from the same tooth were closely compared after different acid-bleach chemical treatment procedures. Two one-bottle adhesives, that is, 3M Single Bond and Pulpdent UNO, exhibiting distinct differences in hydrophilic/hydrophobic composition, were used in this investigation. Using specimens from the same tooth, the effect of chemical treatments on the morphology of the resin-dentin interdiffusion zone and the differences in the morphology of polished and unpolished specimens after these same treatments were studied with scanning electron microscopy. It was shown that conventional specimen preparation techniques that include polishing and acid-bleach treatment can adversely affect and even obscure the structural detail of the a/d interface in specimens that possess a porous HL. The results indicated that the Pulpdent UNO/dentin interface had better quality than the 3M Single Bond/dentin interface. The difference in the quality of HL can be attributed to factors such as compositional differences that impact the adhesive interaction with water, that is present within the substrate during wet bonding. The inability of the conventional acid-bleach procedure to reveal the differences in the scanning electron microscopy interfacial morphology was overcome in this investigation by using a multistep technique.     

Interfacial chemistry of class II composite restoration: structure analysis

The gingival margins of class II composite restorations are particularly vulnerable to marginal leakage and secondary caries. In identifying the factors contributing to caries development, the molecular structure and differences in the structure at the proximal and gingival margins have been largely overlooked. The purpose of this study was to compare the molecular structure at the adhesive/dentin interface of the proximal and gingival walls of class II composite restorations. Class II preparations were cut in 12 unerupted third molars with a water-cooled high-speed dental handpiece. The prepared teeth were randomly selected for treatment with Single Bond (SB) + Z100 (3M). Teeth were restored, per manufacturer's directions, under humidity and temperature characteristic of the oral cavity. Restored teeth were kept in sterile Delbecco's phosphate saline for 48 h. The samples were sectioned occluso-gingivally and micro-Raman spectra were acquired at approximately 1.5-microm spatial resolution across the composite/adhesive/dentin interfaces. Samples were wet throughout spectral acquisition. Raman spectral characteristics at the proximal and gingival margins were distinctly different; the depth of demineralized dentin was 6-7 microm at proximal margin, 12-13 microm at gingival margin. SB adhesive penetrated the depth of demineralized dentin in a gradient at the proximal margin. The "single bottle" adhesive used in this study, gradually penetrated the depth of the demineralized dentin at the proximal margin but failed to infiltrate the depth at the gingival margin, leaving a thick exposed collagen layer.     

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.     

Microleakage and interfacial morphology of self-etching adhesives in class V resin composite restorations

The purpose of the study was to evaluate the marginal leakage of three adhesive systems in Class V resin composite restorations. Two adhesive systems containing acidic primers: Clearfil SE Bond (CSEB) and Etch & Prime 3.0 (E&P), were compared with a conventional water-based primer: Scotchbond Multipurpose Plus (SBMP). Class V cavities were made at the cementum-enamel junction of extracted human molars, which were then divided between three groups. One of the adhesive systems was applied to each group following manufacturers' instructions. Composite restorations were placed, light cured for 40 s, and polished. Specimens were then immersed in a solution of 2% basic fuchsin dye for 24 h. Longitudinal sections were obtained and studied with a stereomicroscope for assessment of the microleakage according to the degree of dye penetration (scale of 0-3). Data were analyzed by Kruskal-Wallis one-way ANOVA, Mann-Whitney tests, and the Wilcoxon matched-pairs signed rank test. Two specimens for each group were analyzed by scanning-electron microscopy (SEM). Bonded interfaces of dentin were also examined by transmission-electron microscopy (TEM). On enamel, there were no significant differences between the three groups. On dentin, CSEB showed the lowest dye penetration values among the three adhesive systems. SEM and TEM studies showed hybrid layer and resin tag formations in all groups.     

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.     

Effect of solvent content on resin hybridization in wet dentin bonding

With wet bonding techniques, the channels between the demineralized dentin collagen fibrils are filled with debris, solvent, and water. Commercial adhesives include solvents such as ethanol or acetone to facilitate resin-infiltration into this wet substrate. Under in vivo conditions, the solvent may be diluted because of repeated exposure of the material to the atmosphere, or concentrated because of separation of the bonding liquids into layers within the bottle. The purpose of this study was to investigate the effect of different concentrations of ethanol (10-50%) on infiltration of the adhesive resin and collagen fibril encapsulation in the adhesive/dentin interface using light microscopy, micro-Raman spectroscopy, and scanning electron microscopy. The results indicated that under wet bonding conditions the hybridization process was highly sensitive to the initial solvent concentration in the adhesive system. The staining and scanning electron microscopy results showed that the quality of the interfacial hybrid layer was poor at the lower (10%) or higher (50%) ethanol content. Micro-Raman analysis indicated that there was a distinct difference in the degree of adhesive penetration among adhesives containing different concentrations of ethanol. Adhesives containing 10 or 50% ethanol did not realize effective penetration; the penetration of the adhesive monomers increased dramatically when the initial ethanol content was 30%. The amount of solvents are essential for achieving effective bonding to dentin.     

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.     

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.     

Micromechanical properties of demineralized dentin collagen with and without adhesive infiltration

In a previous study, we reported the upper limit of Young's modulus of the unprotected protein at the dentin/adhesive interface to be 2 GPa. In this study, to obtain a more exact value of the moduli of the components at the d/a interface, we used demineralized dentin collagen with and without adhesive infiltration. The prepared samples were analyzed using micro-Raman spectroscopy (micro RS) and scanning acoustic microscopy (SAM). Using an Olympus UH3 SAM (Olympus Co., Tokyo), measurements were recorded with a 400 MHz burst mode lens (120 degrees aperture angle; nominal lateral resolution, 2.5 microm). A series of calibration curves were prepared using the relationship between the ultrasonically measured elastic moduli of a set of known materials and their SAM response. Finally, both the bulk and bar wave elastic moduli were computed for a set of 13 materials, including polymers, ceramics, and metals. These provided the rationale for using extensional wave measurements of the elastic moduli as the basis for extrapolation of the 400 MHz SAM data to obtain Young's moduli for the samples: E = 1.76 +/- 0.00 GPa for the collagen alone; E = 1.84 +/- 0.65 GPa for the collagen infiltrated with adhesive; E = 3.4 +/- 1.00 GPa for the adhesive infiltrate.     

Micromechanics of the dentin/adhesive interface.

Scanning acoustic microscopy (SAM) was used in the burst mode at 400 MHz, nominal lateral resolution 2.5 microm, to study the micromechanical properties of the dentin/adhesive interface. Corresponding specimens from the same tooth were investigated using mu Raman spectroscopy, light microscopy, and scanning electron microscopy.12 The elastic moduli of the components of the dentin/adhesive interface were determined by comparing the recorded acoustic impedance values to a calibration curve generated on standard materials. The standard materials, which include polypropylene, Teflon, PMMA, pyrex glass, aluminum, titanium, and stainless steel, provide the appropriate range of acoustic impedance values. The elastic moduli of the components of the dentin/adhesive interface are: partially demineralized dentin, 13 Gpa; mineralized dentin, 28 GPa; adhesive, 5.0 GPa; and unprotected protein at the interface < 2.0 GPa.     

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).     

Interaction patterns between dentin and adhesive on prepared class V cavities in vitro and in vivo

The interface between dentin and an acetone-based single-component adhesive system (Prime&Bond 2.1, DeTrey Dentsply, Germany) was morphologically investigated by scanning electron microscopy (SEM). Interaction patterns of human teeth were correlated in vivo and in vitro. The SEM examination proved that the formation of a hybrid and an adhesive layer, the peri- and intratubular adhesive penetration, as well as hiatus and nanoleakage formation were no different on vital and nonvital dentin within the limitation of the experimental arrangement of this study.     

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.     

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.     

Micro-Raman imaging analysis of monomer/mineral distribution in intertubular region of adhesive/dentin interfaces

It is generally proposed that bonding of resins to dentin results from infiltration of the adhesive monomers into the superficially demineralized dentin. However, it is still not clear how well the mineral phase of dentin is removed and how far each monomer penetrates into the thin zone of "wet" demineralized dentin. The quality and molecular structure of adhesive/dentin interfaces formed under "wet" bonding conditions are studied using 2-D Raman microspectroscopic mapping/imaging techniques. Micro-Raman imaging analysis of the adhesive/dentin interface provides a reliable and powerful means of identifying the degree and depth of dentin demineralization, adhesive monomer distribution, and flaws or defects in the pattern of adhesive penetration. The image of mineral reveals a partially demineralized layer on the top of dentin substrate. Adhesive monomers readily penetrate into dentin tubules and spread into intertubular region through open tubules. The extent of adhesive monomer penetration is higher in the intertubular regions close to tubules as compared to the middle regions between the tubules. The diffusion of resin monomers differs substantially. In a comparison with a hydrophilic monomer, the hydrophobic monomer resists diffusion into the demineralized intertubular dentin area.     

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.     

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.