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Objective: To analyze the effect of Katana™ Cleaner (KC) in nanomechanical and triboscopic properties of etched dentin., Methods: Dentin disks from human third molars were prepared. Two main groups of study were established in function of the etching conditioning, phosphoric acid (PA) and Clearfil SE Bond primer (CSEB). Four subgroups were tested within each group: i) untreated dentin (UD), ii) etched dentin (ED) [(PAED/CSEB)], iii) etched dentin contaminated with saliva (PAED+S)/(CSEB+S), and iv) etched and contaminated dentin treated with KC (PAED+S+KC)/(CSEB+S+KC). Nano-DMA testing and imaging, atomic force microscopy (AFM) analysis and nanoroughness (SRa) measurements were obtained. Field emission scanning electron microscopy (FESEM) images were also acquired., Results: Phosphoric acid etched dentin samples and those specimens contaminated with saliva (PAED+S) attained the highest SRa values, that decreased after Katana™ Cleaner application (PAED+S+KC). In the group of dentin treated with CSEB primer, all subgroups performed similar, except in CSEB+S that attained the highest SRa values. The treatment with KC restored the original values of complex modulus of the untreated dentin. KC application produced the lowest and the highest tan delta values on PAED and CSEB groups, respectively., Conclusion: Katana™ Cleaner provided equally mature dentin surfaces after any of the etching methods. Tan delta increased when Katana™ Cleaner was applied on the dentin surface previously etched and contaminated with saliva, regardless the kind of etchant, thus facilitating the dissipation of energy for elastic recoil during loading., Clinical Significance: Katana™ Cleaner application after saliva contamination originated similar low roughness levels, regardless the type of etching method. Both complex and storage moduli were similar, after Katana™ Cleaner application, in any case., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier Ltd. All rights reserved.)

The aim of this study was to ascertain the effect of Zn-doping of dental adhesives and mechanical load cycling on the micromorphology of the resin-dentin interdiffusion zone (of sound and caries affected dentin). The investigation considered two different Zn-doped adhesive approaches and evaluated the interface using a doubled dye fluorescent technique and a calcium chelator fluorophore under a confocal laser scanning microscopy. Sound and carious dentin-resin interfaces of unloaded specimens were deficiently resin-hybridized, in general. These samples showed a rhodamine B-labeled hybrid layer and adhesive layer completely affected by fluorescein penetration (nanoleakage) through the porous resin-dentin interface. It was thicker after phosphoric acid-etching and more extended in carious dentin. Zn-doping promoted an improved sealing of the resin-dentin interface, a decrease of the hybrid layer porosity, and an increment of dentin mineralization. Load cycling augmented the sealing of the Zn-doped resin-dentin interfaces, as porosity and nanoleakage diminished, and even disappeared in caries-affected dentin substrata conditioned with EDTA. Sound and carious dentin specimens analyzed with the xylenol orange technique produced a clearly outlined fluorescence when resins were Zn-doped, due to a consistent Ca-mineral deposition within the bonding interface and inside the dentinal tubules. It was more evident when load cycling was applied on specimens treated with self-etching adhesives that were Zn-doped. Micropermeability at the resin-dentin interface diminished after combining EDTA pretreatment, ZnCl 2 -doping and mechanical loading stimuli on restorations. It is clearly preferable to include the zinc compounds into the bonding constituents of the self-etching adhesives, instead of into the primer ingredients. The promoted new mineral segments contributed to reduce or avoid both porosity and nanoleakage from the load cycled Zn-doped resin dentin interfaces. EDTA+SB-ZnCl 2 or SEB·Bd-Zn doping are preferred to treat caries-affected dentin surfaces. ZnO-doping encouraged for etch-and-rinse adhesives., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

The aim of this study was to evaluate changes in the mechanical and chemical behavior, and bonding ability at dentin interfaces infiltrated with polymeric nanoparticlesstandard deviations and modes of failure are (NPs) prior to resin application. Dentin surfaces were treated with 37% phosphoric acid followed by application of an ethanol suspension of NPs, Zn-NPs or Ca-NPs followed by the application of an adhesive, Single Bond (SB). Bonded interfaces were stored for 24h, submitted to microtensile bond strength test, and evaluated by scanning electron microscopy. After 24h and 21 d of storage, the whole resin-dentin interface adhesive was evaluated using a Nano-DMA. Complex modulus, storage modulus and tan delta (δ) were assessed. AFM imaging and Raman analysis were performed. Bond strength was not affected by NPs infiltration. After 21 d of storage, tan δ generally decreased at Zn-NPs/resin-dentin interface, and augmented when Ca-NPs or non-doped NPs were used. When both Zn-NPs and Ca-NPs were employed, the storage modulus and complex modulus decreased, though both moduli increased at the adhesive and at peritubular dentin after Zn-NPs infiltration. The phosphate and the carbonate peaks, and carbonate substitution, augmented more at interfaces promoted with Ca-NPs than with Zn-NPs after 21 d of storage, but crystallinity did not differ at created interfaces with both ions-doped NPs. Crosslinking of collagen and the secondary structure of collagen improved with Zn-NPs resin-dentin infiltration. Ca-NPs-resin dentin infiltration produced a favorable dissipation of energy with minimal stress concentration trough the crystalline remineralized resin-dentin interface, causing minor damage at this structure., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

Introduction: Demineralized collagen fibers at the hybrid layer are susceptible to degradation. Remineralization may aid to improve bond longevity., Objectives: The aim of the present study was to infiltrate zinc and calcium-loaded polymeric nanoparticles into demineralized dentin to facilitate hybrid layer remineralization., Materials and Methods: Zinc or calcium-loaded polymeric nanoparticles were infiltrated into etched dentin, and Single Bond Adhesive was applied. Bond strength was tested after 24 h and 6 months storage. Nanomechanical properties, dye-assisted confocal laser microscopy, and Masson's trichrome staining evaluation were performed to assess for the hybrid layer morphology, permeability, and remineralization ability after 24 h and 3 months. Data were analyzed by ANOVA and Student-Newman-Keuls multiple comparisons tests (p < 0.05)., Results: Immediate bond strength was not affected by nanoparticles infiltration (25 to 30 MPa), while after 6 months, bond strengths were maintained (22 to 24 MPa). After 3 months, permeability occurred only in specimens in which nanoparticles were not infiltrated. Dentin remineralization, at the bottom of the hybrid layer, was observed in all groups. After microscopy analysis, zinc-loaded nanoparticles were shown to facilitate calcium deposition throughout the entire hybrid layer. Young's modulus at the hybrid layer increased from 2.09 to 3.25 GPa after 3 months, in specimens with zinc nanoparticles; meanwhile, these values were reduced from 1.66 to 0.49 GPa, in the control group., Conclusion: Infiltration of polymeric nanoparticles into demineralized dentin increased long-term bond strengths. Zinc-loaded nanoparticles facilitate dentin remineralization within the complete resin-dentin interface., Clinical Relevance: Resin-dentin bond longevity and dentin remineralization at the hybrid layer were facilitated by zinc-loaded nanoparticles.

The purpose of this study was to evaluate the remineralization ability of an etch-and-rinse Zn-doped resin applied on caries-affected dentin (CAD). CAD surfaces were subjected to: (i) 37% phosphoric acid (PA) or (ii) 0.5M ethylenediaminetetraacetic acid (EDTA). 10wt% ZnO nanoparticles or 2wt% ZnCl2 were added into the adhesive Single Bond (SB), to create the following groups: PA+SB, PA+SB-ZnO, PA+SB-ZnCl2, EDTA+SB, EDTA+SB-ZnO, EDTA+SB-ZnCl2. Bonded interfaces were submitted to mechanical loading or stored during 24h. Remineralization of the bonded interfaces was studied by AFM nano-indentation (hardness and Young׳s modulus), Raman spectroscopy [mapping with principal component analysis (PCA), and hierarchical cluster analysis (HCA)] and Masson׳s trichrome staining technique. Dentin samples treated with PA+SB-ZnO attained the highest values of nano-mechanical properties. Load cycling increased both mineralization and crystallographic maturity at the interface; this effect was specially noticed when using ZnCl2-doped resin in EDTA-treated carious dentin. Crosslinking attained higher frequencies indicating better conformation and organization of collagen in specimens treated with PA+SB-ZnO, after load cycling. Trichrome staining technique depicted a deeper demineralized dentin fringe that became reduced after loading, and it was not observable in EDTA+SB groups. Multivariate analysis confirmed de homogenizing effect of load cycling in the percentage of variances, traces of centroids and distribution of clusters, especially in specimens treated with EDTA+SB-ZnCl2., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

To obtain more durable adhesion to dentin, and to protect collagen fibrils of the dentin matrix from degradation, calcium- and phosphate-releasing particles have been incorporated into the dental adhesive procedure. The aim of the present study was to incorporate zinc-loaded polymeric nanocarriers into a dental adhesive system to facilitate inhibition of matrix metalloproteinases (MMPs)-mediated collagen degradation and to provide calcium ions for mineral deposition within the resin-dentin bonded interface. PolymP- N : Active nanoparticles (nanoMyP) were zinc-loaded through 30-minute ZnCl2 immersion and tested for bioactivity by means of 7 days' immersion in simulated body fluid solution (the Kokubo test). Zinc-loading and calcium phosphate depositions were examined by scanning and transmission electron microscopy, elemental analysis, and x-ray diffraction. Nanoparticles in ethanol solution infiltrated into phosphoric-acid-etched human dentin and Single Bond (3M/ESPE) were applied to determine whether the nanoparticles interfered with bonding. Debonded sticks were analyzed by scanning electron microscopy. A metalloproteinase collagen degradation assay was also performed in resin-infiltrated dentin with and without nanoparticles, measuring C-terminal telopeptide of type I collagen (ICTP) concentration in supernatants, after 4 wk of immersion in artificial saliva. Numerical data were analyzed by analysis of variance (ANOVA) and Student-Newman-Keuls multiple comparisons tests (p < .05). Nanoparticles were effectively zinc-loaded and were shown to have a chelating effect, retaining calcium regardless of zinc incorporation. Nanoparticles failed to infiltrate demineralized intertubular dentin and remained on top of the hybrid layer, without altering bond strength. Calcium and phosphorus were found covering nanoparticles at the hybrid layer, after 24 h. Nanoparticle application in etched dentin also reduced MMP-mediated collagen degradation. Tested nanoparticles may be incorporated into dental adhesive systems to provide the appropriate environment in which dentin MMP collagen degradation is inhibited and mineral growth can occur., (© International & American Associations for Dental Research.)

Objective: This study evaluated the ability of different in vitro mechanical loading tests to promote new mineral formation at the bonded dentine interfaces created with a two-step self-etching resin adhesive., Methodology: Restored teeth were divided in the following groups: (1) unloaded, load cycling with (2) sine waveform, (3) square waveform, and hold waveform for (4) 24h, and (5) 72 h. Raman spectroscopy and cluster analysis were used to assess the resin-dentine interface., Results: Mechanical loading in CSEB-treated samples promoted a generalized increase of relative presence of minerals and ratio of phosphate peaks, except in square waveform, where the nature of collagen resulted damaged. Crystallinity of carbonate was higher than phosphate. The organic component showed, in general terms, an increase in crosslinking. Molecular orientation (α-helices) peaks augmented in all tests. Pentosidine vibration increases in all tests, except in hold 72 h. Ratios amide I and II/CH2 incremented, in general. Non uniform parameters of Bis-GMA and adhesive penetration were encountered, as both increased at the bottom of the hybrid layer when loading square and hold 72 h were applied., Significance: Functional remineralisation at the resin-dentine interface was attained after in vitro mechanical stimuli application. When loading in square waveform, the lowest vibrations to favor remineralisation were attained., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

Unlabelled: Design of restorative materials should be focused on promoting not only adhesion but also dentine self-repair processes., Objective: To ascertain if ZnO and ZnCl2-doped resins are materials able to induce calcium (Ca) and phosphate (P) deposition., Methods: 48 resin disks were prepared with the following materials: (1) single bond -3M/ESPE-, (2) single bond+ZnO particles 20wt% and (3) single bond+ZnCl2 2wt%. Specimens were polymerised and polished. Bioactivity was tested through a simulated body fluid solution (SBFS) immersion test. At time 24h, 7 d and 21 d surfaces were analyzed by stereomicroscope, high resolution scanning electron microscope (HRSEM), energy-dispersive analysis (EDX), confocal laser Raman, and X-ray diffraction (XRD) for morphological and chemical composition., Results: Under the stereomicroscope, crystal formations were encountered in both zinc-doped resin adhesives after 7 d of immersion. It was, detected by EDX, that the ZnO-doped resin produced Zn, Ca and P deposition (globular formations were observed by HRSEM) after 7 d. Zn and P crystals were detected by HRSEM and EDX in the experimental ZnCl2-doped resin after 7 d and 21 d. Hopeite formation was identified by Raman on both Zn-doped resins. Single bond did not produce mineral or crystal precipitation., Conclusions: ZnO-doped resin induced Ca and P deposition after SBFS immersion. On ZnCl2-doped resin hopeite formation was detected, if this hopeite may be further converted into apatite, after SBFS immersion, remains to be ascertained., Clinical Significance: Bonding with ZnO-doped resin may facilitate incorporation of Ca and P at the interfacial bonding zone., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

Objective: The objective of the study was to determine if zinc-doped etch-and-rinse dentin adhesive may induce therapeutic effects within the resin-dentin interface., Methods: Human acid-etched dentin was infiltrated with Adper™ Single Bond Plus (SB, 3M ESPE, St. Paul, MN, USA), SB doped with 10wt.% ZnO nanoparticles (ZnO-SB) or SB doped with 2wt.% ZnCl2 (ZnCl2-SB). AFM/nanoindentation analysis was performed on fully hydrated specimens to evaluate the nanomechanical properties (Hi: hardness; Ei: modulus of elasticity) across the resin-dentin interface after different SBF storage periods (24h, 1m, 3m). Confocal laser microscopy (CLSM) was used to evaluate the ultramorphology and micropermeability at 24h and 3m of SBF storage., Results: SB control specimens exhibited a decrease in Hi in the hybrid layer (HL) and bottom of the hybrid layer (BHL) and a decrease in Ei in the HL after 3m of SBF storage, indicating that severe degradation occurred in the control interface. ZnO-SB bonded specimens preserved the initial Hi and Ei at the HL and BHL subsequent SBF storage; ZnCl2-SB bonded specimens showed a decrease in Ei, in the HL over time. CLSM analysis confirmed that both Zn-doped adhesives were able to preserve the integrity of the HL., Significance: Specific formulation of Zn-doped etch-and-rinse adhesives may offer the possibility to maintain the nano-mechanical properties along the dentin-bonded interface by inhibiting dentin MMPs and by protective mineral crystals formation within the resin-dentin interface. Clinical advantages may be expected by preserving and improving the integrity of the hybrid layer when Zn-doped adhesives are employed., (Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

Objectives: To determine effect of ageing on deciduous dentine-resin interfaces bond strength and the metalloproteinases (MMPs) activity at the hybrid layer compared to permanent dentine., Methods: Microtensile bond strength (MTBS) tests were performed in human deciduous and permanent dentine after 24h, 3 and 6 months using an etch and rinse adhesive. C-terminal telopeptide concentrations (ICTP) were calculated, in order to determine MMPs mediated collagen degradation at the hybrid layer., Results: The highest MMPs-mediated collagen degradation values occurred in phosphoric acid demineralized dentine, ICTP values were similar for deciduous and permanent dentine after 1 week. Resin infiltration decreased collagen degradation in both dentins and ICTP values were similar to those attained by for untreated dentine. In resin infiltrated and untreated dentine specimens collagen degradation was always higher for deciduous dentine. At 24h, MTBS was higher in permanent dentine. After ageing MTBS decreased and performed similarly in both dentins., Conclusions: Higher collagenollytic activity is found in deciduous than in permanent dentine. At 24h, collagen cleavage by MMPs at the hybrid layer is higher in deciduous dentine leading to a lower MTBS., Clinical Significance: The presence of resin monomers reduced collagen degradation when applied on demineralized dentine, but exerted protection was lower in deciduous dentine., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

Objective: The aim of this study was to assess by using confocal microscopy (CLSM), AFM nano-indentation and microtensile bond strength test (μTBS) the quality of the resin-dentin interfaces created with selected bonding parameters., Methods: Dentin conditioned with H(3)PO(4) or EDTA was bonded in ethanol- or water-wet condition using a HEMA-free or HEMA-containing adhesive. The resin-bonded teeth were stored in distilled water (24h) and sectioned as match-sticks (0.9 mm(2)) for μTBS. Further resin-bonded teeth were sectioned and analyzed using CLSM, and AFM nano-indentation. The AFM imaging and nano-indentation processes were undertaken using a Berkovich diamond indenter. The modulus of elasticity (Ei) and hardness (Hi) across the interface were evaluated with the specimens in a fully hydrated status. The AFM imaging was performed both in dry and wet conditions for evaluating the shrinkage of the hybrid layer on dehydration., Results: The HEMA-containing adhesive applied onto H(3)PO(4)-etched ethanol or water-wet dentin created hybrid layers with the lowest biomechanical nano-properties (p<0.05); no significant differences in μTBS were found between the two wet-bonding techniques (p>0.05). However, the ethanol-wet bonding reduced the dye penetration into the adhesive layer created with the HEMA-containing adhesive. Hybrid layers with high biomechanical properties, low micropermeability and no shrinkage were only possible when using HEMA-free adhesive applied in ethanol wet-dentin. In particular, a significant increase in Ei and Hi was achieved at the hybrid layer and underneath the resin-dentin interface of ethanol-wet EDTA-treated dentin., Significance: The use of HEMA-free adhesives applied onto ethanol-wet dentin may be considered as an alternative and suitable bonding strategy to achieve high quality resin-dentin interfaces., (Copyright © 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

The aim was to study the effect of solvents on the phase separation of four commercial dental adhesives. Four materials were tested: Clearfil™ 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 nm² for CSE, from 15 to 285 nm² for CPB, from 149 to 380 nm² for CS3, and from 26 to 157 nm² 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.

The aim of the study was to ascertain whether the addition of zinc to adhesives may decrease metalloproteinase-mediated collagen degradation without affecting bonding efficacy. Human dentin beams were treated with phosphoric acid, with Clearfil SE Bond Primer or with Clearfil SE Bond Primer plus ZnCl(2) (2 wt%). Acid-etched dentin was infiltrated with Single Bond, Single Bond plus ZnCl(2) (2 wt%), or Single Bond plus ZnO nanoparticles (10 wt%), and Clearfil SE Bond-primed dentin was infiltrated with Clearfil SE Bonding resin, Clearfil SE-Bonding resin with ZnCl(2) (2 wt%), or Clearfil SE-Bonding resin with ZnO nanoparticles (10 wt%). The C-terminal telopeptide concentrations were determined 24 h, and 1 and 4 wk after treatment. Microtensile bond strength to dentin was determined for the tested adhesives. Matrix metalloproteinases-mediated collagen degradation occurred in acid-etched and SE-primed dentin. Resin infiltration decreased collagen degradation. Lower collagen degradation was found for SE Bond than for Single Bond. Zinc-doped Single Bond resin always reduced collagen degradation, the ZnO particles being more effective than ZnCl(2) . Zinc-doped SE Bond reduced the liberation of C-terminal telopeptide only at 24 h. Bond strength to dentin was not decreased when Zn-doped resins were employed, except when ZnCl(2) was added to SE Primer. Zinc-doped resin reduced collagen degradation in Single Bond hybrid layers, but did not affect bond strength. The addition of zinc to SE Bond had no beneficial effects., (© 2011 Eur J Oral Sci.)

Objectives: To evaluate the bond stability of resin cements used for luting alumina-based all-ceramic dental restorations., Background Data: Although different pretreatments may be applied on alumina to improve bond strengths, any previous study investigated the bond stability of resin-based cements luted to laser-irradiated alumina., Methods: 64 sintered, glass-infiltrated alumina blocks were sandblasted and randomly assigned to the following subgroups: 1. no additional treatment (NT); 2. Rocatec (Roc); 3. Nd:YAG laser (L); and 4. Nd:YAG laser plus Rocatec (LRoc). Composite samples were bonded to conditioned ceramics using two different resin based cements: a self-etching adhesive cement-Panavia F (PF) and a self-adhesive resin cement-RelyX Unicem (RXU). After 24 h, bonded specimens were cut into microtensile sticks (1 ± 0.1 mm(2)). One-half of the beams were loaded in tension until failure. The remaining one-half was immersed in 10%-NaOCl aqueous solution (NaOCl(aq)) for 12 h before testing. ANOVA and Student-Newman-Keuls tests were run (P < 0.05). Failure mode was recorded. Ceramic topography was SEM-analyzed., Results: After 24 h, L-sticks achieved the highest MTBS despite the cement type, whereas NT-samples recorded the lowest values. After NaOCl(aq) immersion bond strengths decreased except for RXU luted to NT-alumina. PF luted to L- and LRoc-samples, and RXU luted to L-sticks attained the highest bond strength., Conclusions: Nd:YAG laser irradiation improved bond strength between alumina ceramics and resin cements (PF or RXU). Chemical challenging impaired adhesion, mainly through resin matrixes and silane coupling degradation. Laser-treated specimens remained with the highest bond strength.

Objective: To compare microtensile bond strengths (MTBS) subsequent to load cycling of resin bonded acid-etched or EDTA-treated dentin using a modified ethanol wet-bonding technique., Methods: Flat dentin surfaces were obtained from extracted human molars and conditioned using 37% H(3)PO(4) (PA) (15s) or 0.1M EDTA (60s). Five experimental adhesives and one commercial bonding agent were applied to the dentin and light-cured. Solvated experimental resins (50% ethanol/50% comonomers) were used as primers and their respective neat resins were used as the adhesives. The resin-bonded teeth were stored in distilled water (24h) or submitted to 5000 loading cycles of 90N. The bonded teeth were then sectioned in beams for MTBS. Modes of failure were examined by scanning electron microscopy., Results: The most hydrophobic resin 1 gave the lowest bond strength values to both acid and EDTA-treated dentin. The hydrophobic resin 2 applied to EDTA-treated dentin showed lower bond strengths after cycling load but this did not occur when it was bonded to PA-etched dentin. Resins 3 and 4, which contained hydrophilic monomers, gave higher bond strengths to both EDTA-treated or acid-etched dentin and showed no significant difference after load cycling. The most hydrophilic resin 5 showed no significant difference in bond strengths after cycling loading when bonded to EDTA or phosphoric acid treated dentin but exhibited low bond strengths., Significance: The presence of different functional monomers influences the MTBS of the adhesive systems when submitted to cyclic loads. Adhesives containing hydrophilic comonomers are not affected by cycling load challenge especially when applied on EDTA-treated dentin followed by ethanol wet bonding., (Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

Purpose: To evaluate the laboratory resistance to degradation and the use of different bonding treatments on resin-dentin bonds formed with three self-etching adhesive systems., Methods: Flat, mid-coronal dentin surfaces from extracted human molars were bonded according to manufacturer's directions and submitted to two challenging regimens: (A) chemical degradation with 10% NaOC1 immersion for 5 hours; and (B) fatigue loading at 90 N using 50,000 cycles at 3.0 Hz. Additional dentin surfaces were bonded following four different bonding application protocols: (1) according to manufacturer's directions; (2) acid-etched with 36% phosphoric acid (H3PO4) for 15 seconds; (3) 10% sodium hypochlorite (NaOClaq) treated for 2 minutes, after H3PO4-etching; and (4) doubling the application time of the adhesives. Two one-step self-etch adhesives (an acetone-based: Futurabond/FUT and an ethanol-based: Futurabond NR/FNR) and a two-step self-etch primer system (Clearfil SE Bond/CSE) were examined. Specimens were sectioned into beams and tested for microtensile bond strength (microTBS). Selected debonded specimens were observed under scanning electron microscopy (SEM). Data (MPa) were analyzed by ANOVA and multiple comparisons tests (alpha= 0.05)., Results: microTBS significantly decreased after chemical and mechanical challenges (P< 0.05). CSE showed higher microTBS than the other adhesive systems, regardless the bonding protocol. FUT attained the highest microTBS after doubling the application time. H3PO4 and H3PO4 + NaOCl pretreatments significantly decreased bonding efficacy of the adhesives.

Objective: To determine the role of an anti-oxidant agent (ascorbic acid-AA) on resin-dentin bonds resistance to degradation of two adhesives., Methods: Flat dentin surfaces from 48 human molars were bonded as per manufacturer's instructions with: a two-step etch-and-rinse self-priming adhesive (Single Bond-SB) and a two-step self-etch adhesive (Clearfil SE Bond-CSE). Half of the specimens were bonded with the same adhesives, but after the addition of 10% AA into their formulation. Resin composite build-ups were constructed incrementally and sectioned into resin-dentin beams (1.0mm(2)) that were stored under four conditions: (1) water immersion for 24h; (2) water immersion for 1 year; (3) water immersion for 4 years; and (4) chemical challenging (immersion in 10% NaOCl for 5 h). Beams were pulled to failure in tension at 0.5mm/min. Mean microtensile bond strength (MTBS) data were analysed with ANOVA and multiple comparisons tests (P<0.05). Analysis of debonded dentin beams was performed by scanning electron microscopy (SEM)., Results: After 24 h, SB and CSE performed equally, regardless of AA incorporation. Inclusion of AA on CSE formulation decreased MTBS following one-year water storage, but maintained SB bond strength values even after four years of water storage. NaOCl challenge diminished MTBS for both adhesives, but when AA was added to SB, this reduction was significantly lower., Conclusions: The inclusion of AA on adhesive's formulation exerts a protective role on resin-dentin bonds resistance to degradation when SB is used. Bonding durability of CSE may be compromised by the addition of sodium ascorbate., (Copyright © 2010 Elsevier Ltd. All rights reserved.)

Our aim was to evaluate the influence of different application parameters on microtensile bond strength (microTBS) of an "all in one" water-based self-etching primer/adhesive to dentin. Extracted human third molars had their crowns transversally sectioned next to the dentinoenamel junction. Prompt-L-Pop adhesive was applied using five modes: (1) following the manufacturer's instructions (MI); (2) after 36% H(3)PO(4) etching (15 s) (AG); (3) after H(3)PO(4) etching and 5% NaOCl (2 min) with constant agitation (HG); (4) as a double layer (DL); and (5) for double the application time (DT). Resin build-ups were constructed with Tetric Ceram. After storage for 24 h, 6 months, or 12 months in water at 37 degrees C, the specimens were vertically sectioned into beams (cross-sectional areas, 1 mm(2)). Each beam was tested in an Instron Machine at 0.5 mm/min. Analysis of variance and Student-Newman-Keuls were used (P < 0.05). Bonded interfaces were examined by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The highest microTBS values were obtained when AG was used, and the lowest when MI was employed. The HG, DL, and DT modes resulted in similar microTBS values. Water storage reduced microTBS in all groups except the MI group. SEM and TEM revealed hybrid layer and resin tag formation in all groups. Applied after AG, HG, DL, and DT, Prompt L-Pop adhesive provided adequate bond strength to dentin after 24 h of water storage. Bond strength decreased when specimens were stored in distilled water for 6 or 12 months.

Purpose: To evaluate the effect of oxalate during total-etch bonding, under different dentin moisture conditions, over time. The null hypothesis tested was that microtensile bond strength (microTBS) was not affected by oxalate treatment and dentin moisture during two evaluation periods., Methods: Extracted human third molars had their mid-coronal dentin exposed flat and polished with 600-grit SiC paper. The surfaces were etched with 35% phosphoric acid for 15 seconds, washed and blot dried. After etching, a 3% potassium oxalate gel was applied for 120 seconds, except for the control group (no desensitizer). The surface was then washed and left moist (Wet bonding) or air-dried for 30 seconds (Dry bonding). The surfaces were bonded with: (1) two 2-step etch-and-rinse adhesives: Single Bond (SB); Prime & Bond NT (PBNT) and (2) one 3-step etch-and-rinse adhesive: Scotchbond Multi Purpose (SBMP). Composite buildups were constructed incrementally with Tetric Ceram resin composite. Each increment was cured for 40 seconds. After storage in water for 24 hours or 1 year at 37 degrees C, the specimens were prepared for microTBS testing with a cross-sectional area of approximately 1 mm2. They were then tested in tension in an Instron machine at 0.5 mm/minute. Data were analyzed by ANOVA and Student-Newman-Keuls at alpha = 0.05., Results: Application of potassium oxalate had no significant effect on the bond strengths of SBMP and PBNT, regardless of the surface moisture condition (P > 0.05). Conversely, reduced bond strengths were observed after oxalate treatment for SB in both moisture conditions, that being significantly lower when using a dry-bonding procedure (P < 0.05). Lower bond strength was obtained for PBNT when a dry-bonding technique was used, regardless of the oxalate treatment (P < 0.05). After aging the specimens for 1 year, bond strengths decreased. Smaller reductions were observed for SBMP, regardless of moisture conditions. For the WB technique, smaller reductions after 1 year were observed without oxalate treatment for SB and after oxalate treatment for PBNT.

Objective: To compare resin-dentin bond strengths and the micropermeability of hydrophobic vs. hydrophilic resins bonded to acid-etched or EDTA-treated dentin, using the ethanol wet-bonding technique., Methods: Flat dentin surfaces from extracted human third molars were conditioned before bonding with: 37% H(3)PO(4) (15s) or 0.1M EDTA (60s). Five experimental resin blends of different hydrophilicities and one commercial adhesive (SBMP: Scotchbond Multi-Purpose) were applied to ethanol wet-dentin (1 min) and light-cured (20s). The solvated resins were used as primers (50% ethanol/50% comonomers) and their respective neat resins were used as the adhesive. The resin-bonded teeth were stored in distilled water (24h) and sectioned in beams for microtensile bond strength testing. Modes of failure were examined by stereoscopic light microscopy and SEM. Confocal tandem scanning microscopy (TSM) interfacial characterization and micropermeability were also performed after filling the pulp chamber with 1 wt% aqueous rhodamine-B., Results: The most hydrophobic resin 1 gave the lowest bond strength values to acid-etched dentin and all beams failed prematurely when the resin was applied to EDTA-treated dentin. Resins 2 and 3 gave intermediate bond strengths to both conditioned substrates. Resin 4, an acidic hydrophilic resin, gave the highest bond strengths to both EDTA-treated and acid-etched dentin. Resin 5 was the only hydrophilic resin showing poor resin infiltration when applied on acid-etched dentin., Significance: The ethanol wet-bonding technique may improve the infiltration of most of the adhesives used in this study into dentin, especially when applied to EDTA-treated dentin. The chemical composition of the resin blends was a determining factor influencing the ability of adhesives to bond to EDTA-treated or 37% H(3)PO(4) acid-etched dentin, when using the ethanol wet-bonding technique in a clinically relevant time period., (Copyright (c) 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

Objectives: To evaluate the effect of shortening the etching time on roughness, microhardness and bond strength of three adhesive systems to primary tooth dentin., Methods: Flat dentin surfaces from primary molars were randomly assigned to six experimental groups. Three different adhesive systems were used: an etch-and-rinse adhesive (Single Bond), a two-step self-etching (Clearfil SE Bond), and a one-step self-etching (One-Up Bond F) adhesive. In half of the specimens, the recommended etching time was used, in the other half the etching time was 50% reduced. After applying the adhesive, resin composite build-ups were constructed and stored in a humid environment for 24h at 37 degrees C. Specimens were sectioned into 1mm(2) beams and tested for microtensile bond strength (MTBS). Debonded surfaces were analyzed by scanning electron microscopy (SEM). Additional surfaces were conditioned for microhardness measurements (KHN) and for atomic force microscopy (AFM) analysis. Intertubular and total surface roughness (Ra) were recorded. Results were analyzed with ANOVA and Student-Newman-Keuls tests (P<0.05)., Results: Single Bond and Clearfil SE Bond showed higher MTBS than One-Up Bond F. Bond strength and intertubular roughness increased when Single Bond and One-Up Bond F were used with a reduced etching time. For Clearfil SE Bond no differences in MTBS were detected when reducing the etching time. The application of phosphoric acid, Clearfil SE Bond primer and One-Up Bond F decreases dentin microhardness., Conclusions: Shortening One-Up Bond F application time and reducing the etching time of phosphoric acid to one-half of the manufacturer's recommended etching time when using Single Bond are recommended when bonding to primary dentin., (Copyright 2009 Elsevier Ltd. All rights reserved.)

The effects of dentin surface treatments on the microtensile bond strengths and on the interfacial characteristics of self-adhesive resin cements were investigated. Flat dentin surfaces were obtained from human molars and were treated as follows: (i) no treatment of dentin; (ii) 0.1 M EDTA scrubbed for 60 s; or (iii) 10% polyacrylic acid applied for 30 s. Three self-adhesive cements were used to lute composite overlays on deep-coronal dentin surfaces in the presence of simulated pulpal pressure (15 cm of H(2)O). Bonded specimens were cut into beams 1 mm thick and stressed in tension until failure. Fractured sticks were examined under a scanning electron microscope. Additional specimens were stained with Masson's trichrome and observed under light microscopy for interfacial evaluations. The bond strength to dentin of the hydrophobic and solvent-free cement (RelyX Unicem) was unaffected by the tested dentin treatments. The bond strength of the 2-hydroxyethyl methacrylate (HEMA)-based cement (Bis-Cem) decreased after treatment of dentin with EDTA and/or polyacrylic acid. The hydrophilic and water-containing cement (G-Cem) attained a higher bond strength when luted on polyacrylic acid-conditioned dentin. In conclusion, smear layer removal, opening of dentinal tubules, and the water content of dentin differently influence the bond strengths and the interfacial characteristics of self-adhesive cement-dentin interfaces.

Purpose: To evaluate the degradation of resin-enamel interfaces bonded with different adhesive systems., Methods: Flat enamel surfaces were ground buccally on bovine incisors. Two etch & rinse self-priming adhesives (Single Bond, Prime & Bond NT), three two-step self-etch adhesives (Clearfil SE Bond, Resulcin Aquaprime, NRC/Prime & Bond NT) and two all-in-one adhesives (Etch & Prime 3.0, Adper Prompt-L-Pop) were used for bonding. A hybrid resin composite (Tetric Ceram) was selected for coronal build-up. Bonded specimens were stored in water at 37 degrees C for 24 hours, 6 months and 1 year, respectively, and then sectioned into 1 mm2 beams. Each microtensile stick was loaded in tension until failure (crosshead speed: 0.5 mm/minute). Bond strength data were analyzed with two-way ANOVA and Student Newman Keuls tests (P < 0.05). Etching patterns resulting from phosphoric acid etching and self-etch adhesives application on ground enamel were analyzed under SEM., Results: All adhesives attained similar bond strengths after 24 hours. All-in-one adhesives and Resulcin Aqua Prime recorded a significant reduction in bond strengths after 6 months and 1 year of water aging.

Objectives: The aim of this study was to investigate the droplet formation using a real-time/confocal microscopy technique, when different self-etching and etch-and-rinse adhesives were applied in the presence or absence of pulpal pressure. Resin-dentin permeability (%P) was also evaluated., Methods: Optibond FL, Silorane adhesive, Scotchbond 1XT, G-Bond and DC-Bond were bonded in the presence or in absence of simulated pulpal pressure. A fluid-transport model was used to measure the water permeability through resin-bonded dentin. Half of the specimens bonded in the presence of the hydrostatic pulpal pressure (20 cm H2O) were light cured, whereas the remnant half received no light curing. The same was done with the half of the specimens bonded under no pulpal pressure. The specimens were investigated under a confocal TSM., Results: Optibond FL and G-Bond had the lowest dentin permeability. Optibond FL adhesive showed few water droplets on the polymerized external surface and within the resin-dentin interface. G-Bond showed static interfacial globular-like droplet formation. DC-Bond and Scotchbond 1XT were the most water permeable adhesives both in the presence and in absence of pulpal pressure. A dynamic interfacial non-globular-like droplet formation was observed. Severe droplet formation was observed on the polymerized external surface., Significance: The presence of the pulpal pressure may cause increasing in fluid filtration and droplet formation in simplified adhesives containing HEMA. The adhesives containing 4-META (G-Bond) may be affected by static phase separation but by very low osmotic droplets formation and water permeability. The three-step adhesives are less affected by these problems.

One way of possibly improving bond strength is by changing the application mode of self-etch adhesives. The current study evaluated the resin-dentin microtensile bond strength (MTBS) promoted by two- and one-step self-etching adhesives after different bonding application procedures. Flat dentin surfaces from extracted human molars were bonded: 1) according to the manufacturers' instructions, 2) duplicating the number of adhesive coats and 3) doubling the application time of the acidic primers. Two-step (Clearfil SE Bond/SEB and Resulcin AquaPrime/RE) and one-step (Etch & Prime 3.0/EP and One-Up Bond F/OUB) self-etch adhesives were used. Resin-dentin beams were tested in tension at 0.5 mm/minute. Selected debonded beams were observed under scanning electron microscopy (SEM). MTBS data were analyzed by ANOVA and multiple comparison tests (p < 0.05). The highest MTBS was always attained with SEB, regardless of the bonding procedure. RE, EP and OUB showed similar MTBS when bonded as per the manufacturers' instructions. The MTBS of OUB increased after doubling the application time and duplicating the adhesive coats. The two-step self-etch adhesives were insensible to changes in bonding application procedures. Attempts to improve the bonding performance of water/ethanol-based self-etching systems by using different bonding application parameters were system-specific and only effectively detected in one-step adhesive systems.

Objectives: The objectives of this work were to study the spatially resolved extent of photopolymerization and the final volumetric contraction of the self-etching adhesive Xeno IV (Dentsply/Caulk, Milford, DE, USA) in association with the self-curing agent Aurora (Dentsply/Caulk, Milford, DE, USA), using (1)H Stray-Field magnetic resonance imaging ((1)H STRAFI-MRI)., Methods: One-dimensional (1)H STRAFI-MRI images (projections along an axis, profiles) were acquired from the adhesive with and without Aurora, before and after solvent removal. Specimens were observed after the irradiation period recommended by the manufacturers and new profiles were recorded. Extent of polymerization and volumetric contraction were obtained by subtracting the profile of the cured adhesive from the profile of the liquid; the profiles were previously normalized using an external reference signal and the highest magnetization intensity recorded from the cured adhesive, respectively. Data were obtained in the presence of oxygen. Solvent evaporation was measured by gravimetry., Results: High volumetric contraction was observed for Xeno IV and Xeno IV and Aurora mixture mainly related to solvent evaporation. A drying period favourably influenced the extent of photopolymerization of Xeno IV, which did not increase in the presence of Aurora., Conclusions: The incorporation of Aurora reduced the extent of polymerization of the one-step adhesive, probably due to the increase in the solvent content of the mixture. It may be that enhancing solvent evaporation is important in order to reach a higher extent of polymerization during the bonding procedure.

Objective: To evaluate the effect of EDTA pre-treatment of dentine on resistance to degradation of the bond between dentine and resin-modified glass-ionomer cements., Methods: Sixty non-carious human molars underwent cavity preparations. Teeth were restored with Fuji II LC or Vitremer. Half of the cavities were restored following manufacturers' instructions whereas the other half was pre-treated with EDTA (0.1M, pH 7.4) for 60s. Teeth were stored in water at 37 degrees C for 24h, 3 months or submitted to 10% NaOCl immersion for 5h. Teeth were sectioned into beams (1+/-0.1mm) and tested to failure in tension at 0.5mm/min. Bond strength data (MPa) were analyzed by ANOVA and SNK multiple-comparisons tests (p<0.05)., Results: When EDTA was used for pre-treatment of dentine, higher bond strengths were observed for both cements. Degradation challenges produced a decrease in bond strength values only in the Vitremer group. This decrease was avoided when EDTA was used for dentine treatment before restoring with Vitremer., Conclusions: EDTA pre-treatment of dentine increases bond strength of resin modified glass-ionomers cements to dentine and improves resistance to degradation of the bond between Vitremer and dentine.

Objectives: To evaluate the bond strength (microTBS) of self-etching adhesives in different solvent evaporation conditions., Methods: Flat dentine surfaces from extracted human third molars were bonded with: (1) 2 two-steps self-etching adhesives (Clearfil SE Bond-CSEB); (Protect Bond-PB) and (2) 2 one-step self-etch systems (Adper Prompt L Pop-ADPLP); (Xeno III-XIII). Bonded dentine surfaces were air-dried for 5s, 20s, 30s or 40s at either 21 degrees C or 38 degrees C. Composite build-ups were constructed incrementally. After storage in water for 24h at 37 degrees C, the specimens were prepared for microtensile bond strength testing. Data were analyzed by two-way ANOVA and Student-Newman-Keuls at alpha=0.05., Results: CSEB and PB performed better at warm temperature with only 20s of air-blowing. The bond strength increased when XIII was performed at warm temperature at 40s air-blowing. Extended air-blowing not affect the performance of ADPLP, except at 30s air-blowing time at warm temperature., Conclusions: The use of a warm air-dry stream seems to be a clinical tool to improve the bond strength to self-etching adhesives.

Objectives: The aim of this study was to reduce hybrid layer degradation created with simplified dentine adhesives by using two different methods to condition the dentine surface., Methods: A smear-layer was created on flat dentine surfaces from extracted human third molars with a 180-grit/SiC-paper. Dentine specimens were conditioned before bonding with the following procedures: 37% H(3)PO(4); H(3)PO(4)/0.5% NaOCl; 0.1M EDTA; 0.1M EDTA/0.5% NaOCl. Two etch-and-rinse adhesives: (Scotchbond 1XT or Optibond Solo Plus) were applied and light-cured. Composite build-ups were constructed. The bonded teeth were sectioned into beams, stored in distilled water (24h) or 12% NaOCl solution (90 min) and finally tested for microtensile bond strengths (microTBS). Additional dentine surfaces were conditioned and bonded as previously described. They were prepared for a pulpal-micropermeability confocal microscopy study and finally observed using confocal microscopy., Results: microTBS results revealed that both adhesives gave high bond strengths to acid-etched dentine before, but not after a 12% NaOCl challenge. Bonds made to acid-etched or EDTA-treated dentine plus dilute NaOCl, gave high microTBS that resisted 12% NaOCl treatment, as did EDTA-treated dentine alone. A confocal micropermeability investigation showed very high micropermeability within interfaces of the H(3)PO(4), etched specimens. The lowest micropermeability was observed in H(3)PO(4)+0.5% NaOCl and 0.1M EDTA groups., Conclusions: The use of dilute NaOCl (0.5%) after acid-etching, or the conditioning of dentine smear layers with 0.1M EDTA (pH 7.4) produced less porous resin-dentine interfaces. These dentine-conditioning procedures improve the resistance of the resin-dentine bond sites to chemical degradation (12% NaOCl) and may result in more durable resin-dentine bonds.

Objectives: This study aimed to investigate if the use of protease inhibitors (EDTA and chlorhexidine) may influence microtensile bond strength (MTBS) of an etch-and-rinse adhesive system to caries-affected human dentin., Methods: Flat middle coronal dentin surfaces with a central region of caries-affected dentin surrounded by sound dentin were bonded with Adper Scotchbond 1 after: (1) etching with 35% H3PO4; (2) etching with 0.1M EDTA and (3) 35% H3PO4-etching followed by 5% chlorhexidine application. Resin composite build-ups were constructed incrementally and trimmed to yield hourglass specimens (0.8mm2 bonded area) that contained sound or caries-affected dentin (confirmed after debonding by microhardness measurements - KHN). Bonded specimens were tensioned at 0.5mm/min. Data were analyzed by ANOVA and multiple comparisons tests (p<0.05). Failure mode analysis was performed by scanning electron microscopy (SEM)., Results: H(3)PO(4), EDTA and chlorhexidine pre-treatments yielded similar MTBS values, in both dentin substrates. Bond strength to sound dentin was significantly higher than that to caries-affected dentin after H3PO4-etching. Caries-affected dentin exhibited lower KHN than sound dentin., Conclusions: Conditioning of caries-affected dentin with EDTA or a combined use with H3PO4 and chlorhexidine may be proposed as these protease inhibitors do not reduce MTBS to caries-affected dentin if compared to conventional H3PO4 treatment.

Resin cement diffusion into dentin may differ as a function of the pre-treatment regimen. Since self-adhesive cements do not require substrate pre-treatment for luting, penetration of and interaction with the underlying dentin are questioned. We hypothesized that differences in the resin cement diffusion into dentin may exist among current commercial adhesive cements. Composite cylinders were luted on mid-coronal dentinal surfaces by an etch-and-rinse cement (Calibra), a self-etching system (Panavia F 2.0), and 4 self-adhesive cements (Multilink Sprint, Rely X Unicem, G-Cem, Bis-Cem). Dentin/cement interfacial characteristics were analyzed by a staining technique (Masson's trichrome) and by scanning electron microscopy. Conventional acid etching resulted in partially infiltrated adhesive interfaces differing from those achieved with the application of self-etching primer. No hybrid layer and/or resin tag formation was detectable at the interfaces bonded with self-adhesive cements. Limited decalcification/infiltration was observed for self-adhesive cements into the underlying dentin. Self-adhesive cements were not able to demineralize/dissolve the smear layer completely.

Objectives: To evaluate the bonding effectiveness of self-adhesive luting cements to dentin in the presence of simulated hydrostatic intrapulpal pressure (PP)., Methods: Thirty composite overlays (Aelite All Purpose Body) were luted to deep-coronal dentin surfaces using four self-adhesive resin cements (Rely X Unicem, G-Cem, Multilink Sprint, Bis-Cem) and one total-etch system (Calibra). Half of the specimens resin cements were applied under a PP of 15 cm H2O. After storage in a moist condition for 1 month (37 degrees C, 100% relative humidity), specimens were sectioned into microtensile beams (1mm2) and stressed to failure with the microtensile bond strength test (microTBS). Data were statistically analyzed with Kruskal-Wallis ranking (p<0.05) and Mann-Whitney tests (p<0.001). The fracture pattern was evaluated under SEM., Results: Bond strength of Calibra fell significantly when PP was applied during bonding (p<0.05). Rely X Unicem and Bis-Cem performed better under PP. No significant differences for Multilink Sprint and G-Cem bonded specimens were recorded with or without PP., Significance: Simulated PP influences the adhesive performance of resinous cements. The predominance of acid-base reactions or radical polymerization may explain the different behavior of self-adhesive cements when changing substrate wetness. The application of constant intrapulpal perfusion should be considered when simulating luting procedures in vitro.

Objectives: To evaluate the longevity of sound (SD) and caries-affected dentin (CAD) bonds made with etch-and-rinse and self-etching adhesives after a 6-month water-storage period, using bond strength and morphological evaluations., Methods: Extracted human molars with coronal carious lesions were selected. Flat surfaces of CAD surrounded by SD were bonded with etch-and-rinse (Adper Scotchbond 1) or with self-etching (Clearfil Protect Bond and AdheSE) adhesives. Trimmed resin-dentin bonded interfaces (1mm2) were stored in distilled water for 24h or 6 months and subjected to microtensile bond strength (microTBS) evaluation. The quality of the dentin beneath fractured specimens was measured by Knoop microhardness (KHN). ANOVA and multiple comparisons tests were used (P<0.05). Fractographic analysis and interfacial nanoleakage evaluation were performed by scanning electron microscopy (SEM). Resin-dentin bonded sections (10microm thick) were stained with Masson's trichrome and examined using light microscopy. Collagen exposure and adhesive penetration were examined qualitatively., Results: microTBS to SD was significantly higher than that to CAD for all bonding agents. Bonds made with AdheSE were weaker than the other adhesives after 6-months storage regardless of the dentin substrate. CAD bonded specimens presented a significant muTBS decrease over time. Lower KHN was recorded in CAD compared to SD. An increase in the exposed collagen zone and a decrease in the quality of the adhesive infiltration were observed in CAD interfaces., Significance: CAD bonded interfaces are more prone to hydrolytic degradation than SD bonds. Additionally, as compared to SD, there were remarkable differences in depth of demineralization, adhesive infiltration and interfacial bond strength with CAD.

Purpose: To determine the marginal leakage of Class V restorations bonded with etch-and-rinse and self-etching adhesives applied after different dentin pretreatments over a maximum storage time of 24 months., Materials and Methods: Standardized mixed Class V cavities (5 mm x 3 mm and 2 mm deep) were cut on the buccal and lingual surfaces of 180 human molars. Two self-etching adhesive systems, Adper Prompt L-Pop (3M ESPE) and Clearfil SE Bond (Kuraray), and one etch-and-rinse bonding agent (One Step, Bisco) were applied as follows: 1. according to manufacturers' instructions; 2. after 37% H3PO4 etching for 15 s; 3. after 37% H3PO4 etching for 15 s and 5% NaOCl aq application for 2 min. Teeth were stored for 24 h, 6, 12, and 24 months in saline solution at 37 degrees C before being stained in 0.5% solution of basic fuchsine. Dye penetration was scored on a 0 to 3 ordinal scale and analyzed with the Kruskal-Wallis H test (p < 0.05), Mann-Whitney U-test (p < 0.01), and Wilcoxon paired test (p < 0.05)., Results: Significant differences exist after using the tested adhesives at dentin and enamel margins. Adhesive type and substrate pretreatment had a significant effect on the long-term sealing of Class V restorations, and aging increased leakage overtime. The extent of leakage at the enamel margins was lower than that at dentin margins. One Step recorded the best results after 24 months., Conclusion: Optimal adhesion of restorative materials to enamel and dentin is hampered by a reduction in marginal seal over time. Alternative dentinal treatments (etching or collagen removal) might increase bonding efficacy, depending on the adhesive system used.

Objectives: To evaluate resin-dentine bond degradation after 1 year of water storage., Methods: Human dentine surfaces were bonded with two etch-and-rinse self-priming adhesives (Single Bond/SB and Prime & Bond NT/PBNT), three 2-step self-etching adhesives (Clearfil SE Bond/SEB, Resulcin Aqua Prime/RES and Non-Rinse Conditioner with Prime & Bond NT/NRC-PBNT), and five 1-step self-etching adhesives (Etch & Prime 3.0/EP, Prompt L-Pop/PLP, Solist/SOL, Futurabond/FUT and AQ Bond/AQ). Adhesives were applied according to manufacturers' instructions. Composite build-ups were constructed and the bonded teeth were stored (24 h, 6 months, 1 year) in distilled water at 37 degrees C. After storage, the intact teeth were sectioned into beams and all specimens were tested for microtensile bond strengths (MTBS). ANOVA and multiple comparisons tests were applied at alpha = 0.05. Fractographic analysis of debonded beams was performed using scanning electron microscopy., Results: SB, PBNT and SEB attained the highest MTBS, regardless of the storage period. A significant decrease in MTBS was observed after 6 months for SOL. After 12 months the only groups that did not reduce bond strength were SB and SEB. Bonded specimens in NRC-PBNT, RES and FUT produced pre-testing failures after 12 months, and MTBS could not be measured., Conclusions: The resistance of resin-dentine bonds to degradation is material-dependent. When the enamel-resin interface is preserved, the etch-and-rinse adhesives and the mild 2-step self-etch adhesive SEB exhibited the best resin-dentine bond durability. Those tested self-etching adhesives having a pH < or 1 and using water or acetone as solvent attained catastrophic bond failure after 1 year of water storage.

Purpose: To determine the microtensile bond strength (microTBS) of one- and two-step self-etch adhesives bonded to sound dentin conditioned or not with phosphoric acid (H3PO4) and sodium hypochlorite (H3PO4 + NaOCl)., Methods: Extracted human third molars had their crowns transversally sectioned to expose flat dentin surfaces that were divided into four groups, and bonded as follow: (1) according to the manufacturers' directions, (2) acid etched with 36% H3PO4, and (3) 10% NaOCl treated for 2 minutes, after H3PO4 etching. Two two-step self-etching primers (Clearfil SE Bond/SEB and Resulcin/RE), and two one-step adhesives (One-Up Bond F/OUB and Etch & Prime 3.0/EP) were examined. Composite build-ups were constructed incrementally with Tetric Ceram. The specimens were stored in humidity for 24 hours at 37 degrees C and sectioned into beams of 1.0 mm2 cross-sectional area. Each beam was tested in tension in an Instron machine at 0.5 mm/minute, and mean microTBS data (MPa) were analyzed by 2-way ANOVA and post-hoc multiple comparisons tests (P < 0.05)., Results: The two-step adhesive SEB exhibited the highest bond strength when bonded to smear layer-covered dentin, whereas RE was not affected by all dentin surface conditions. H3PO4 and H3PO4 + NaOCl pretreatments significantly increased bonding efficacy of the one-step adhesives OUB and EP, respectively.

Objectives: To evaluate the microtensile bond strength (MTBS) of self-etch (with or without H(3)PO(4)-etching) and total-etch bonding systems bonded to different regions of dentin., Methods: Long flat dentin cavity preparations extending from top-crown to root-apex within the same tooth were performed and bonded: using two-step (Clearfil SE Bond/SEB, Resulcin Aqua Prime/RES) and one-step (Etch & Prime 3.0/EP, One-Up Bond F/OUB, Prompt L-Pop/PLP, Solist/SOL and Futurabond/FUT) self-etch adhesives; these same adhesives were also applied following H(3)PO(4)-etching of dentin and finally two more groups were bonded with total-etch adhesives (Single Bond/SB and Prime & Bond NT/PBNT). Build-ups of resin composite were constructed incrementally to ensure sufficient bulk for the MTBS test and the different regions of dentin were identified by painting with different colours on the top of the resin composite. Specimens were sliced into beams and tested in tension. ANOVA and multiple comparisons tests were used (p<0.05)., Results: Regardless of the tested dentin region, SEB attained the highest MTBS to smear layer-covered surfaces (i.e., coronal dentin: 42.7MPa), while H(3)PO(4)-etching of dentin hampered bonds (i.e., coronal dentin: 27.7MPa). When bonding with PBNT, SB, RES, EP, PLP, SOL and FUT, MTBS was similar for different dentin regions. H(3)PO(4)-etching of dentin did not alter the attained MTBS., Significance: SEB yielded the highest MTBS to all regions of dentin. When bonding to parallel-cut dentin, previous H(3)PO(4)-etching of dentin did not increase MTBS and differences in bond strength among dentin regions were absent.

The objective of this study is to evaluate the effect of a bacterial collagenase on the degradation of resin-dentin bonds. Human dentin surfaces were bonded with: an etch-&-rinse self-priming adhesive (SB), a two-step self-etching primer/adhesive (SEB), and a 1-step self-etching adhesive (OUB). Composite build-ups were constructed. The bonded teeth were stored (24 h, 3 months, 1 year) in distilled water or in a buffered bacterial collagenase solution. Half of the specimens were stored as intact bonded teeth (Indirect Exposure/IE). The other half were sectioned into beams prior to storage (Direct Exposure/DE). After storage the intact teeth were sectioned into beams and all specimens were tested for microtensile bond strengths (MTBS). ANOVA and multiple comparisons tests were performed. Fractographic analysis was performed by scanning electron microscopy. The inclusion of bacterial collagenase in the storing solution did not lower the MTBS values over those seen in specimens stored in water. SB and SEB bonds strength were equal, and were superior to OUB. After 3 months of DE, SB and OUB bonded specimens showed decreases in MTBS; similar reductions required 1 year for SEB/DE. MTBS did not decrease in IE specimens except for OUB. Resin and collagen dissolution were evident in DE groups after storing.

Purpose: To evaluate the effect of different fiber post surface treatments on bond strength., Methods: Extracted endodontically-treated premolars were prepared for the cementation of a methacrylate resin-based fiber post (FRC Postec). The posts received one of the three surface pre-treatments: silane application; hydrofluoric acid-etching and silane application or no treatment. A light-cured composite was used with one of the three dentin adhesives for luting: Single Bond; Clearfil Photo Bond and Clearfil New Bond, followed by a light-cured composite core build-up. Specimens were serially sliced into 0.8 x 0.8 mm-thick beams and loaded in tension until failure., Results: Significant differences in bond strengths were recorded among the dentin adhesives (P< 0.05). However, post pre-treatment did not affect the bonding efficacy of the adhesives except for Clearfil New Bond.

Objectives: To evaluate the longevity of resin-dentin bonds of three adhesives using different storage media and specimen size., Methods: Flat dentin surfaces from extracted human third molars were bonded with: a two-step etch-and-rinse self-priming adhesive (Single Bond), a two-step self-etching adhesive (Clearfil SE Bond), and a one-step self-etching adhesive (One-Up Bond F). Composite build-ups were constructed. The bonded teeth were stored under three conditions: dry, distilled water, or mineral oil. Half of the specimens were stored as intact bonded teeth (Indirect Exposure/IE). The other half were first sectioned into beams and stored under same conditions (Direct Exposure/DE). After storage periods of 24h, 3 months or 1 year, the intact teeth (IE) were sectioned into beams and both subgroups (DE and IE) were tested for microtensile bond strengths. Results were analyzed with multiple ANOVA and Student-Newman-Keuls tests. Fractographic analysis was performed by SEM., Results: After 24h, Single Bond and Clearfil SE Bond performed equally and were superior to One-Up Bond F. After 3 months of DE to water storage, decreases in bond strengths were observed for Single Bond and One-Up Bond F, this decrease occurred for Clearfil SE Bond after 12 months of water storage. Bonded specimens aged in dry did not alter bond strengths over time. Bond strength increased when Single Bond was stored in mineral oil after 3 and 12 months. Micromorphological alterations were evident after water storage., Significance: Although dentin bond strength of all the adhesives fell over time in DE, SE Bond fells the least.

Objectives: Dentin bonds made with one-bottle etch-and-rinse and self-etch adhesives are affected by the formation of interfacial blisters, porosities and deterioration. The first objective of this study was to evaluate the fluid flow through resin-dentin interfaces created by self-etching adhesives applied to deep dentin using a replica technique and by directly measuring dentin permeability (P). The second objective was to examine the effect of intrapulpal pressure on the microtensile bond strength of these adhesives., Methods: A fluid-transport model was used to measure the fluid permeability (%P) through different adhesives. Impressions of bonded dentin were taken with a polyvinylsiloxane impression material to monitor fluid transudation from the surface of the adhesive. Positive replicas were fabricated for SEM examination. Two groups of resin-bonded specimens (pulpal pressure versus no pulpal pressure) were created for microtensile bond strength evaluation. Adhesive application was performed under 0 cm H(2)O. Pulpal pressure group was submitted to 20 cm H(2)O of pulpal pressure during build-up procedures., Results: Clearfil Protect Bond exhibited the lowest permeability and fewest numbers of fluid droplets over the surface of the bonded dentin. G-Bond and Clearfil-S3 Bond were more permeable than Clearfil Protect Bond. One Up Bond F was the most permeable adhesive. A highly significant correlation was observed between the relative permeability of these adhesives (%P) and the number of fluid droplets on the adhesive surfaces. The application of pulpal pressure significantly reduced bond strength., Significance: Resin-dentin bonds created by contemporary self-etch adhesives are susceptible to fluid permeation induced by pulpal pressure. HEMA-based adhesives showed the largest reductions in bond strengths after pulpal pressure application.

This study investigated the microtensile bond strength (microTBS) of a one-step self-etching adhesive to human dentin and bovine enamel following different bonding treatments. Occlusal portions of human molars and labial surfaces of bovine incisors were ground flat to provide uniform dentin and enamel surfaces, respectively. Futurabond was used following five different protocols: 1) according to the manufacturer's directions, 2) acid etched with 36% phosphoric acid (H3PO4) for 15 seconds, 3) 10% sodium hypochlorite (NaOCl) treated for two minutes after H3PO4-etching, 4) doubling the application time of the adhesive and 5) doubling the number of adhesive coats. Composite build-ups (6 mm in height) were constructed incrementally with Arabesk resin composite. The specimens were stored in 100% humidity for 24 hours at 37 degrees C and sectioned into beams of 1.0 mm2 cross-sectional area. Each beam was tested in tension in an Instron machine at 0.5 mm/minute, and mean microTBS data (MPa) were analyzed by one-way ANOVA and post-hoc multiple comparisons tests (alpha = 0.05). Doubling the application time of Futurabond attained the highest microTBS to dentin; whereas, no differences among all bonding application parameters evaluated could be detected when the adhesive was applied to enamel.

Objective: To evaluate the resistance to degradation of resin-dentin bonds formed with a one-step acetone-containing and HEMA-free adhesive., Methods: Flat, mid-coronal dentin surfaces were bonded with G Bond under dry and wet conditions. The bonded teeth were subjected to fatigue loading (90 or 250 N) using 5000 or 50000 cycles (at 3.0 Hz) and to chemical degradation (10% NaOCl immersion for 5 h). Specimens were sectioned into beams and tested for microtensile bond strength. Fractographic analysis was performed by scanning electron microscopy (SEM). Additional specimens were processed for morphological examination of the interfaces., Results: Bond strength significantly decreased after the chemical challenge (p<0.05), but not after load cycling. Dentinal moisture did not affect bond strength. Most of the recorded failures were adhesive and located at the top of the hybrid layer. A poorly infiltrated hybrid layer with bubbles entrapped within the adhesive was observed in all groups., Conclusions: A discrepancy between water/solvent evaporation rate and convective and evaporative water fluxes from the underlying dentin may be responsible of the droplet formation within the adhesive layer, thus reducing bond strength. A "stress relieving" effect may occur during loading. A loss of bonding effectiveness is expected overtime, mainly due to chemical degradation of the hybrid layer.

The hydrolytic stability of a pre-activated MPS silane (Monobond-S) and a 2-component 4-META/ gamma-MPTS silane (Porcelain Liner M) to H202-etched quartz fiber posts was investigated using a modeling approach. Composite build-ups around silanized posts were stored dry for 24 hours, stored in deionized water at 37 degrees C for 24 hours, 1 week, 1 month or they were thermocycled. Sectioned specimens were prepared for microtensile bond testing and SEM examination; 4-META/gamma-MPTS silane produced a rapid decline in bond strength after 1 week and 1 month of water storage and after thermocycling. This was not apparent in pre-activated MPS silane. SEM revealed debonding along the post-composite interfaces, which were coupled with 2-component silane. The use of a hydrophilic resin monomer (4-META) for on-demand hydrolysis of the gamma-MPTS silane expedited interfacial water sorption and hydrolytic degradation, which may be prevented with alternative coupling strategies.

Endogenous matrix metalloproteinases (MMPs) release from crown dentin and their activation results in degradation of hybrid layers created by dentin adhesives. This study tested the hypothesis that instrumented intraradicular dentin possesses latent collagenolytic activity that is activated by mild self-etching adhesives. Root dentin shavings were produced from 50 cleaned and shaped, saline-irrigated root canals using Gates Glidden drills and rinsed with sodium azide to prevent bacterial growth. Dried dentin powder aliquots were treated with two clinically-relevant MMP inhibitors, 2% chlorhexidine for 10 minutes and 17% EDTA for 1 minute. Additional dentin powder was mixed with Clearfil Liner Bond 2V or Clearfil Tri-S Bond for 1 minute followed by extracting the adhesives with acetone. Dentin powder was also treated with 2% chlorhexidine for 10 minutes before or after adhesive application. Collagenolytic activities of the nine groups were assayed with a fluorometer in 96-well plates, by recording the changes in fluorescence before and after addition of fluorescein-labeled type I collagen. Epoxy resin-embedded powders were examined with TEM for the extent of demineralization. Instrumented, mineralized intraradicular dentin possessed low but detectable collagenolytic activity that was inhibited by chlorhexidine (p < 0.001) and EDTA (p < 0.001). Both adhesives partially demineralized the dentin powder and activated latent MMPs, with 14- to 15-fold increases in collagenolytic activities (p < 0.001) that were significantly (p < 0.001) but incompletely inactivated after 10 min application of chlorhexidine. Mild self-etching adhesives activate latent MMPs without denaturing these enzymes, and may adversely affect the longevity of bonded root canal fillings and posts.

The influence of different silane/dentin adhesives on the microtensile bond strengths of a hybrid composite to sodium ethoxide-etched quartz fiber posts was investigated. A prehydrolyzed silane was applied without an adhesive and compared to two-component systems in which hydrolysis of the silane occurred after mixing with the acidic monomer present in the dentin adhesives. Nanoleakage along post/core interfaces was examined after silver nitrate tracer penetration using scanning electron microscopy. Higher interfacial strengths and more uniform adaptation between the etched fiber post surface and the composite core were recorded after post treatment with silane/adhesive couplings. The combination of silane with two-step self-etch adhesives improves the chemical retention of composites around etched fiber posts with minimal nanoleakage. Although the one-step self-etching adhesive/silane combination enhances post adhesion, the extensive nanoleakage provides channels for rapid water sorption that may expedite hydrolytic degradation of the post/core interface.

Objective: To evaluate the effect of mechanical loading on the microtensile bond strength (MTBS) of five adhesive systems to dentin., Methods: Flat dentin surfaces from human molars were divided into five groups and bonded with total-etch self-priming adhesives (Single Bond, Prime&Bond NT and Prime&Bond XP), two-step self-etching primer (Clearfil SE Bond) and an all-in-one adhesive (Etch&Prime 3.0), according to the manufacturers' instructions. Composite build-ups were constructed incrementally with Tetric Ceram. After 24 hours of water storage, half the specimens were load cycled (5000 cycles, 90 N). The teeth were then sectioned into beams of 1.0 mm2 cross-sectional area. Each beam was tested in tension in an Instron machine at 0.5 mm/minute. Data were analyzed by two-way ANOVA and Student Newman Keuls 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 3.0 resulted in the lowest MTBS. After mechanical loading, MTBS decreased in all groups except Prime&Bond XP. Clearfil SE Bond, Single Bond and Prime&Bond XP obtained higher MTBS than Prime&Bond NT. Specimens bonded with Etch&Prime 3.0 resulted in premature failures and MTBS could not be measured., Clinical Relevance: When using Etch&Prime 3.0, bond structures did not withstand mechanical loading, which may have an influence on the long-term success of restorations. If dentin is acid-etched, alcohol-based adhesive systems showed higher bond strength after mechanical loading.

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., (Copyright (c) 2005 Wiley Periodicals, Inc.)

Purpose: To evaluate the microtensile bond strengths (MTBS) of a dual-cured dentin adhesive bonded to dentin using a light-cured resin-based composite (composite) or a polyacid-modified resin-based composite (compomer), and to investigate the effect of water aging on the bond strengths of these systems., Methods: Flat dentin surfaces prepared from extracted human third molars were bonded with Prime&Bond NT Dual-Cured version (PBNT). Resin build-up crowns were constructed incrementally with two different materials: a composite (Z250) or a compomer (Dyract AP). When Dyract AP was used as the restorative material, half of the specimens were etched with 36% phosphoric acid, and the other half of the specimens were not etched. After storage in water for 24 hours or for 6 months, the teeth were sectioned to obtain bonded 1.3 mm2 beams containing the bonded interface. Each beam was tested in tension in an Instron machine at 0.5 mm/minute. Results were analyzed by multiple ANOVA and Student-Newman-Keuls multiple comparison tests., Results: The group PBNT/Dyract AP bonded to acid-etched dentin showed the highest bond strength, in the 24-hour evaluation. Bond strength values decreased significantly after aging. The groups treated with PBNT in light-cured, dual-cured and self-cured modes performed equally well in the 24-hour evaluation. After 6 months of water aging, bond-strengths of the light-cured groups remained stable. By contrast, decreases in the bond strengths of the self-cured groups were observed.

Purpose: To determine the bond strength of five adhesives systems to either superficial or deep dentin., Methods: Extracted human third molars had their crowns transversally sectioned either next to the occlusal DEJ or next to the pulp, to expose flat, superficial or deep dentin surfaces. The surfaces were bonded with: 1) three two-step, total-etch, self-priming adhesives (Single Bond, Prime&Bond NT, and Excite), 2) a two-step, self-etching primer (Clearfil SE Bond), and 3) a single-step, self-etching all-in-one adhesive (Etch & Prime 3.0) according to manufacturers' directions. Composite build-ups were constructed incrementally with Z250. After storage for 24 hours in water at 37 degrees C, the teeth were sectioned to obtain several bonded beams of 1.0 mm2 cross-sectional area. Each beam was tested in tension in an Instron machine at 0.5 mm/minute. Results were analyzed by two-way ANOVA and post-hoc multiple comparisons (P = 0.05). Bonded interfaces were also examined by TEM. Nanoleakage was examined using a silver-staining technique., Results: Single Bond, Prime&Bond NT and Clearfil SE Bond performed equally when were bonded to superficial dentin; the lowest value was obtained with Etch & Prime 3.0. On deep dentin, the highest bond strengths were attained with Clearfil SE Bond and Prime & Bond NT. The bond strengths of Prime & Bond NT and Excite were significantly higher to deep than to superficial dentin and the rest of the adhesives showed similar bond strength to both dentin depths. Nanoleakage was manifested to variable extent within all hybrid layers examined.