Long-term nanomechanical properties and gelatinolytic activity of titanium tetrafluoride-treated adhesive dentin interface

ObjectiveThis study investigated the effects of dentin pretreatment with 2.5% titanium tetrafluoride (TiF₄) on nanomechanical properties, and the in situ gelatinolytic activity of the dentin–resin interface, for up to 6 months.MethodsTwenty-four human teeth were prepared by exposing occlusal flat dentin surfaces, and were randomly assigned to experimental groups, according to application or non-application of a TiF₄ pretreatment, and to the adhesive systems (Clearfil SE Bond or Scotchbond Universal). Resin composite (Filtek Supreme Ultra) was built up incrementally on the teeth in all the groups. Then, the specimens were sectioned and randomly selected for evaluation at 24 h, 3 months and 6 months of storage time. The reduced modulus of elasticity (E_r) and the nanohardness of the underlying dentin, as well as the hybrid layer and the adhesive layer were measured using a nanoindenter. Gelatinolytic activity at the dentin–resin interfaces was assessed by in situ zymography using quenched fluorescein-conjugated gelatin at 24 h and 6 months. Statistical analyses were performed with ANOVA and Tukey’s tests.ResultsThere were no differences in E_r and nanohardness values between adhesives systems and pretreatment (p = 0.1250). In situ zymography showed significantly higher gelatinolytic activity after 6 months for all the experimental groups (p = 0.0004), but no differences between the adhesive systems (p = 0.7708) and the surface pretreatment (p = 0.4877). Significance: Dentin pretreatment with 2.5% TiF₄ followed by self-etching adhesive systems did not influence nanomechanical properties or gelatinolytic activity of the adhesive–dentin interface layers, over time.     

Stability of bonds made to superficial vs. deep dentin,before and after thermocycling

ObjectivesBonding stability of resinous adhesives to dentin is still problematic and may involve regional variations in dentin composition. This study is to evaluate the effect of dentin depth on the stability of resin-dentin bonds under thermocycling challenge.MethodsDentin slabs with two flat surfaces parallel to the tooth axis were obtained from extracted human third molars. The slabs were randomized into eight groups according to the location of dentin [deep dentin (DD) or superficial dentin (SD)], the adhesive treatment (Single Bond 2 or Clearfil S³ Bond), and the storage treatment (thermocycling for 5000 times vs. no). After the adhesive treatment and composite buildup on the dentin slabs, the micro-shear bond strength (μSBS) of each group was detected. The concentrations of cross-linked carboxyterminal telopeptide of type I collagen (ICTP) were also evaluated using an immunoassay to detect the degree of collagen degradation in each group.ResultsDentin depth, adhesive treatment and storage treatment all showed significant effects on both the μSBSs and the ICTP values (P < 0.05). Regardless of the adhesive type, thermocycling decreased the μSBSs and increased the ICTP values (P < 0.05). The DD groups showed significantly lower μSBSs and higher ICTP values than SD groups after thermocycling aging (P < 0.05). The treatment with Single Bond 2 significantly increased the ICTP values (P < 0.05), whereas Clearfil S³ Bond showed no effect on the ICTP values (P > 0.05).SignificanceDeep dentin showed significantly more bond degradation after thermocycling than did superficial dentin.     

Nanoleakage,ultramorphological characteristics,and microtensile bond strengths of a new low-shrinkage composite to dentin after artificial aging

ObjectivesTo study the microtensile bond strengths and nanoleakage of low-shrinkage composite to dentin. The null hypotheses tested were (1) aging does not affect the bonding of low-shrinkage composite; (2) there is no difference in microtensile bond strengths and nanoleakage using different bonding strategies.Methods32 extracted molars were assigned to one of four groups: LS System Adhesive (LS, 3M ESPE); dentin etched for 15 s with phosphoric acid + LS System Adhesive (LSpa); Adper Single Bond Plus (SB, 3M ESPE); SB + LS Bond (SBLS). Occlusal dentin was exposed and restored with Filtek LS (3M ESPE). The samples were tested after 24 h or after 20,000 thermocycles and 6 months of aging. Teeth were sectioned with a cross-section of 0.8 ± 0.2 mm² and fractured at a crosshead speed of 1 mm/min. The data were submitted to ANOVA/Duncan's post hoc test, at p < 0.05. Five slabs from each group were selected and immersed in 50 wt% ammoniacal silver nitrate. Then, specimens were processed for SEM, the silver penetration was measured and data analyzed with Kruskal–Wallis at p < 0.05.ResultsNo statistically significant difference was found among the experimental groups for the factor dentin treatment (p = 0.165) and aging (p = 0.091). All experimental groups exhibit some degree of nanoleakage. There was no adhesion of Filtek LS applied directly over dentin surfaces treated with SB.SignificanceThe new low-shrinkage resin composite showed compatibility only with its dedicated adhesive. Pre-etching did not improve the bond strengths to low-shrinkage resin composite. Some degree of nanoleakage was evident in all groups.     

Immediate bonding properties of universal adhesives to dentine

ObjectivesTo evaluate the dentine microtensile bond strength (μTBS), nanoleakage (NL), degree of conversion (DC) within the hybrid layer for etch-and-rinse and self-etch strategies of universal simplified adhesive systems.Methodsforty caries free extracted third molars were divided into 8 groups for μTBS (n = 5), according to the adhesive and etching strategy: Clearfil SE Bond [CSE] and Adper Single Bond 2 [SB], as controls; Peak Universal Adhesive System, self-etch [PkSe] and etch-and-rinse [PkEr]; Scotchbond Universal Adhesive, self-etch [ScSe] and etch-and-rinse [ScEr]; All Bond Universal, self-etch [AlSe] and etch-and-rinse [AlEr]. After restorations were constructed, specimens were stored in water (37 °C/24 h) and then resin–dentine sticks were prepared (0.8 mm²). The sticks were tested under tension at 0.5 mm/min. Some sticks from each tooth group were used for DC determination by micro-Raman spectroscopy or nanoleakage evaluation (NL). The pH for each solution was evaluated using a pH metre. Data were analyzed with one-way ANOVA and Tukey's test (α = 0.05).ResultsFor μTBS, only PkSe and PkEr were similar to the respective control groups (p > 0.05). AlSe showed the lowest μTBS mean (p < 0.05). For NL, ScEr, ScSe, AlSe, and AlEr showed the lowest NL similar to control groups (p < 0.05). For DC, only ScSe showed lower DC than the other materials (p < 0.05).ConclusionsPerformance of universal adhesives was shown to be material-dependent. The results indicate that this new category of universal adhesives used on dentine as either etch-and-rinse or self-etch strategies were inferior as regards at least one of the properties evaluated (μTBS, NL and DC) in comparison with the control adhesives (CSE for self-etch and SB for etch-and-rinse).     

Microtensile bond strength of a new silorane-based composite resin adhesive

Filtek LS is a new composite resin restorative system with a unique, low-shrinking, silorane-based monomer matrix. The current study was conducted to compare the durability of the bond to dentin of the new silorane-based bonding agent, Filtek Silorane System Adhesive, to the gold standard methacrylate-based bonding agent, Clearfil SE Bond. Extracted human molar teeth were sectioned to expose dentin. Either Filtek Silorane System Adhesive with Filtek LS composite or Clearfil SE Bond with Clearfil Majesty Posterior composite was applied to the dentin according to the manufacturer's instructions. The composites were placed incrementally and sectioned perpendicular to the composite-tooth interface to obtain rectangular beams. The beams were stored for 24 hours, 6 months, or 12 months in distilled water and stressed in tension in a universal testing machine. Data were analyzed with a two-way ANOVA/Tukey test. The 24-hour microtensile bond strengths were significantly greater than the 6- and 12-month bond strengths. Overall, there was no significant difference in the microtensile bond strength to dentin between the Filtek Silorane System Adhesive and the Clearfil SE Bond adhesive bonding agents. After one year of water storage, the new silorane-based composite resin bonding agent performed as well as the methacrylate-based composite resin bonding agent.     

Mechanical and physical properties of silorane and methacrylate-based composites

ObjectivesThis study measured the degree of conversion (DC), sorption, solubility and microhardness of methacrylate (Filtek Z250 and Filtek Z350XT) and silorane-based composites (Filtek P90).MethodsDC was measured using near infrared spectroscopy immediately and 24 h after the photoactivation. Sorption and solubility measurements were performed after 24 h, 4 weeks and 12 weeks of storage in water. Knoop microhardness was measured after 24 h and after thermal cycling. The data were statistically analyzed using ANOVA followed by Tukey's, Tamhane or paired t-tests (α = 0.05).ResultsThe DC for P90 (37.22 ± 1.46) was significantly lower than the Z250 (71.44 ± 1.66) and Z350 (71.76 ± 2.84). Water sorption was highest in the Z250 and lowest in the P90. All the tested composites exhibited similar values after 24 h of immersion, and no significant differences were observed. No significant differences were observed between the solubilities of the P90 composite (12 weeks) and the Z250 or Z350 composites (4 weeks). KHN values were less elevated for the P90 composite and similar for the Z250 and Z350 composites. An effect of thermal cycling on KHN values was observed for all the composites (p < 0.001).ConclusionsSilorane produced the lowest DC and KHN values and exhibited lower water sorption and solubility compared to methacrylate-based composites. These differences suggest that silorane composites exhibit better hydrolytic stability after 3 months of water immersion compared to conventional methacrylate-based composites.Clinical significanceSilorane had higher hydrolytic stability after 3 months of water immersion than the methacrylate-based resins, despite the lower values of DC and KHN recorded.     

Impact of shelf-life simulation on bonding performance of universal adhesive systems

ObjectivesTo evaluate the micro-tensile bond strength to dentin (μTBS), the degree of conversion (DC) and nanoleakage expression (NL) of eight dental adhesives considering their expiry date (as-received, half-life and or end of shelf-life) after shelf-life simulation.MethodsFive universal adhesives (Single Bond Universal, SBU; Tetric Bond Universal, TBU; OneCoat Universal, OCU; OptiBond Universal, OBU; and Prime&Bond Elect, P&B), two two-step self-etch adhesives (Clearfil SE, CSE; and AdheSE, ASE) and one two-step etch-and-rinse adhesive (Adper Singlebond 2, ASB) were evaluated. Shelf-life was simulated by storing the materials in an acclimatization chamber for different periods of time. The μTBS was tested in accordance with ISO/TS 11,405. DC was evaluated by means of FTIR spectroscopy. NL was evaluated after ammoniacal silver challenge. The significance level of α = 0.05 was used for all statistical analyses.ResultsThe μTBS to dentin of TBU, P&B, ASE, and ASB adhesive systems remained stable throughout the shelf-life periods evaluated, while for SBU, OCU, OBU, and CSE, decreased significantly after evaluation in the ‘half-life’ or ‘end of shelf-life’ condition (p < 0.05). Except for P&B, ASE and OBU, the degree of conversion significantly decreased after the shelf-life simulation (p < 0.05). OCU, ASE, and CSE showed significantly increased percentage of silver deposition within the adhesive layer (p < 0.05).SignificanceStoring conditions and progressively longer storage time affect the performance of universal adhesives systems.     

Marginal integrity of low-shrinking versus methacrylate-based composite: effect of different one-step self-etch adhesives

The aim of the study was to evaluate the influence of composite type and adhesive system on the quality of marginal adaptation in standardized Class V cavities before and after thermo-mechanical loading (TML). The cavities were restored using different combinations of three adhesive systems [(Silorane System Adhesive (SSA), Clearfil S³ Bond (S3), G-Bond (G-B)] and two resin composite materials (Filtek Silorane, Clearfil AP-X). Six groups (n = 10): Group A (SSA-Primer + SSA-Bond, Filtek Silorane), Group B (SSA-Primer + SSA-Bond, Clearfil AP-X), Group C (S3 + SSA-Bond, Filtek Silorane), Group D (S3 + SSA-Bond, Clearfil AP-X), Group E (G-B + SSA-Bond, Filtek Silorane) and Group F (G-B + SSA-Bond, Clearfil AP-X) were defined. Marginal adaptation was assessed on replicas in the SEM at 200 × magnification before and after TML (3000 × 5–55 °C, 1.2 10⁶ × 49 N; 1.7 Hz) under simulated dentinal fluid. The highest scores of continuous margins (%CM) were observed in the group F (G-B + SSA-Bond, Clearfil AP-X: before loading 96.4 (±3.2)/after loading 90.8 (±7.0)). A significant effect of adhesive system, composite type and loading interval was observed on the results (p < 0.05). Significantly lower scores of %CM were observed for silorane-based composite (Filtek Silorane) after TML in comparison with methacrylate-based composite (Clearfil AP-X) considering total marginal length (p < 0.05). For both Filtek Silorane and Clearfil AP-X, G-Bond performed significantly better than SSA-Primer and Clearfil S³ Bond (p < 0.05). For all combinations of one-step self-etch adhesives and SSA-Bond resin coating, silorane-based low-shrinking composite exhibited inferior marginal adaptation than did the methacrylate-based composite.     

Effect of dentin pre-treatment with a casein phosphopeptide-amorphous calcium phosphate (CPP-ACP) paste on dentin bond strength in tridimensional cavities

Abstract

Objective. This study aimed to evaluate the push-out bond strength of dimethacrylate (Clearfil SE Bond/Filtek Z250; and Adper SE Plus/Filtek Z250) and silorane-based (Filtek P90 adhesive system/Filtek P90 composite resin) restorative systems following selective dentin pre-treatment with a CPP-ACP-containing paste (MI Paste). Materials and methods. Sixty bovine incisors were utilized. The buccal surface was wet-ground to obtain a flat dentin area. Standardized conical cavities were then prepared. Adhesive systems were applied according to manufacturers' directions and the composites were bulk-inserted into the cavity. The push-out bond strength test was performed at a universal testing machine (0.5 mm/min) until failure; failure modes were analyzed by scanning electron microscopy. Data were analyzed by two-way ANOVA and Tukey post-hoc test (p < 0.05). Results. For Clearfil SE Bond/Filtek Z250 and Filtek P90 adhesive system/Filtek P90 composite resin, the dentin pre-treatment did not influence bond strength means. For Adper SE Plus/Filtek Z250, dentin samples treated with MI Paste had statistically higher bond strength means than non-treated specimens. Adhesive failures were more frequent. Conclusion. Dentin pre-treatment with the CPP-ACP containing paste did not negatively affect bond strength for Clearfil SE Bond/Filtek Z250 and Filtek P90 adhesive system/Filtek P90 composite resin restorative systems and improved bond strength for the Adper SE Plus/Filtek Z250 restorative system.     

Fluoride-containing adhesive: Durability on dentin bonding

ObjectivesTo evaluate (1) the influence of fluoride-containing adhesive on microtensile bond strength (μTBS) and (2) in vitro secondary caries inhibition at the resin–dentin interface after 24 h and 3 months water-storage and (3) the degree of conversion of different adhesives after 24 h 1 month.MethodsFlat surfaces of human teeth were ground and randomly assigned to six groups: (SBMP-24) Scotchbond Multi-Purpose control [SBMP], 24 h; (SE-24) SBMP etch and primer + Clearfil SE Bond adhesive [SE], 24 h; (PB-24) SBMP etch and primer + Clearfil Protect Bond adhesive [PB], 24 h; (SBMP-3) SBMP, 3 months; (SE-3) SBMP + SE, 3 months; and (PB-3) SBMP + PB, 3 months. To evaluate the effect of the adhesive resin alone, all teeth were etched with 35% phosphoric acid and primed with SBMP primer prior to applying the adhesive resin. Bonded assemblies were prepared for μTBS and stored in distilled water at 37 °C for 24 h and 3 months. Sections of restored teeth of each group were exposed to an acid challenge. The specimens were sectioned, polished, and then observed with polarized light microscopy (PLM). Also, the degree of conversion (DC) of the adhesives was measured using Fourier Transform-Infrared spectroscopy (FTIR) at 24 h and 1 month, after polymerization.ResultsμTBS values obtained in MPa (24 h/3 m) were: (MP) 61.5 ± 10.5/52.9 ± 8.9, (SE) 55.5 ± 11.8/55.6 ± 13, and (PB) 50.3 ± 9.9/61.0 ± 13.6. For interface analysis by PLM, an inhibition zone (IZ) adjacent to the hybrid layer was created only when the fluoride-containing adhesive (PB) was used. The DC in percentage (24 h, 1 month) were: (MP) 60.5 ± 2.8/61.3 ± 0.6, (SE) 69.6 ± 1.3/70.7 ± 0.05, and (PB) 53.1 ± 0.4/58.3 ± 1.6.SignificanceThe fluoride-containing adhesive demonstrated significant increase of bond strength values after water-storage. This material was also able to create an acid inhibition zone in dentin. There was a significant increase of degree of conversion after 1 month only for PB.     

Dentin-smear remains at self-etch adhesive interface

ObjectiveThe bonding potential of ‘mild’ self-etch adhesives may be compromised due to smear interference, as they may not dissolve/penetrate the smear layer effectively due to their relatively low acidity. We observed that the thickness of the dentin smear layer differed depending on the surface-preparation methodology used.MethodsThe interaction of an (ultra-)mild self-etch adhesive (Clearfil S3 Bond, Kuraray Noritake) with human dentin, prepared either using a medium-grit diamond bur (‘thick’, clinically relevant smear layer) or 600-grit SiC-paper (‘thin’ smear layer), or just fractured (smear-free), was evaluated using high-resolution transmission electron microscopy (TEM). Non-demineralized/demineralized 30–100 nm interfacial cross-sections were prepared following common TEM-specimen processing and diamond-knife ultra-microtomy.ResultsThe adhesive did not dissolve the bur-cut, nor the SiC-ground smear layer, but impregnated it. Within this ‘resin-smear complex’, hydroxyapatite was abundantly present. At fractured dentin, this complex was not present, while the actual layer of interaction of the adhesive was limited to about 100 nm. Non-demineralized ‘ultra-thin’ (30–50 nm) sections confirmed the interfacial ultra-structure to differ for the three surface-preparation methods. An electron dense band was consistently disclosed at the adhesive interface, most likely representing the documented chemical interaction of the functional monomer 10-MDP with Ca.SignificanceThe dentin surface-preparation method significantly affects the nature of the smear layer and the interaction with the ultra-mild self-etch adhesive.     

Influence of dentin pretreatment with 2.5% titanium tetrafluoride on inhibiting caries at the tooth-restoration interface in situ

ObjectiveInvestigate the effects of dentin pretreatment with 2.5% titanium tetrafluoride (TiF₄) aqueous solution followed by two-step self-etching (CLE/Clearfil SE Bond) and one-step self-etching adhesive systems (SBU/Single Bond Universal) on carious lesion inhibition at the tooth-restoration interface using an in situ model.DesignSixty-four cavities at the enamel-dentin junction of dental fragments were randomly distributed according to groups (n = 16): 1) TiF₄ + CLE; 2) TiF₄ + SBU; 3) CLE; 4) SBU. Cavities were restored using resin composite, and placed in intraoral palatal devices used by 16 volunteers for 21 days, to induce caries formation in situ. The fragments were then ground-flat to perform Knoop microhardness tests. Nine indentations were performed on each enamel and dentin substrate, subjacent to the restoration. Analysis of variance and Tukey’s test were applied.ResultsEnamel: groups receiving TiF₄ dentin pretreatment (regardless of adhesive system and tooth-restoration interface distance) presented higher hardness means at a depth of 25 μm from the outer tooth surface (p < 0.0001). Dentin: groups receiving CLE presented higher means when applying TiF₄ pretreatment, whereas groups restored with SBU presented higher means without pretreatment (p = 0.0003).ConclusionsDentin pretreatment with TiF₄ inhibited demineralization of the enamel interface in situ, regardless of the adhesive, and TiF₄ pretreatment followed by CLE application showed higher potential for inhibiting dentin demineralization at the interface.     

Effect of biomimetic mineralization on enamel and dentin: A Raman and EDX analysis

ObjectiveTo investigate the effect of an experimental biomimetic mineralization kit (BIMIN) on the chemical composition and crystallinity of caries-free enamel and dentin samples in vitro.MethodsEnamel and dentin samples from 20 human teeth (10 for enamel; 10 for dentin) were divided into a control group without treatment and test samples with BIMIN treatment. Quantitative analysis of tissue penetration of fluoride, phosphate, and calcium was performed using energy-dispersive X-ray spectroscopy (EDX). Mineralization depth was measured by Raman spectroscopy probing the symmetric valence vibration near 960 cm⁻¹ as a marker for crystallinity. EDX data was statistically analyzed using a paired t-test and Raman data was analyzed using the Student’s t-test.ResultsEDX analysis demonstrated a penetration depth of fluoride of 4.10 ± 3.32 μm in enamel and 4.31 ± 2.67 μm in dentin. Calcium infiltrated into enamel 2.65 ± 0.64 μm and into dentin 5.58 ± 1.63 μm, while the penetration depths for phosphate were 4.83 ± 2.81 μm for enamel and 6.75 ± 3.25 μm for dentin. Further, up to 25 μm of a newly mineralized enamel-like layer was observed on the surface of the samples. Raman concentration curves demonstrated an increased degree of mineralization up to 5–10 μm into the dentin and enamel samples.SignificanceBiomimetic mineralization of enamel and dentin samples resulted in an increase of mineralization and a penetration of fluoride into enamel and dentin.     

Effects of solvent evaporation time on immediate adhesive properties of universal adhesives to dentin

ObjectiveTo evaluate the microtensile bond strengths (μTBS) and nanoleakage (NL) of three universal or multi-mode adhesives, applied with increasing solvent evaporation times.MethodsOne-hundred and forty caries-free extracted third molars were divided into 20 groups for bond strength testing, according to three factors: (1) Adhesive – All-Bond Universal (ABU, Bisco, Inc.), Prime&Bond Elect (PBE, Dentsply), and Scotchbond Universal Adhesive (SBU, 3 M ESPE); (2) Bonding strategy – self-etch (SE) or etch-and-rinse (ER); and (3) Adhesive solvent evaporation time – 5 s, 15 s, and 25 s. Two extra groups were prepared with ABU because the respective manufacturer recommends a solvent evaporation time of 10 s. After restorations were constructed, specimens were stored in water (37 °C/24 h). Resin–dentin beams (0.8 mm²) were tested at 0.5 mm/min (μTBS). For NL, forty extracted molars were randomly assigned to each of the 20 groups. Dentin disks were restored, immersed in ammoniacal silver nitrate, sectioned and processed for evaluation under a FESEM in backscattered mode. Data from μTBS were analyzed using two-way ANOVA (adhesive vs. drying time) for each strategy, and Tukey's test (α = 0.05). NL data were computed with non-parametric tests (Kruskal–Wallis and Mann–Whitney tests, α = 0.05).ResultsIncreasing solvent evaporation time from 5 s to 25 s resulted in statistically higher mean μTBS for all adhesives when used in ER mode. Regarding NL, ER resulted in greater NL than SE for each of the evaporation times regardless of the adhesive used. A solvent evaporation time of 25 s resulted in the lowest NL for SBU-ER.SignificanceResidual water and/or solvent may compromise the performance of universal adhesives, which may be improved with extended evaporation times.     

Mechanical stability of adhesives under water storage

ObjectivesTo evaluate the effects of storage condition (wet or dry) and storage time (24 h and 3 months) on the ultimate tensile strength (UTS) of Single Bond (SB), 3M-ESPE; Opti Bond Solo Plus (OB), Kerr; One Step (OS), Bisco, and Prime & Bond NT (PB), Dentsply adhesive resins.MethodsHourglass-shaped specimens were obtained from a metallic matrix. Each adhesive was dispensed to fill the molds completely and left undisturbed in a dark chamber for 4 min at 37 °C for solvent evaporation. They were individually light-cured for 80 s at 500 mW/cm² and randomly divided into three groups: 24 h of water storage; 3 months of water storage; 3 months of dry storage. The specimens were tested in tension at 0.5 mm/min using the microtensile method and data were analyzed by two-way ANOVA and SNK tests for each material.ResultsWater storage for 3 months did not cause significant changes in the UTS of any of the adhesives (p-value). Values for water storage ranged from 25.9 MPa for Single Bond at 24 h to 32.7 MPa for Prime & Bond NT after 3 months. Dry storage for 3 months yielded significantly higher UTS for most adhesives, which ranged from approximately 20% for Opti Bond to 160% higher values for Single Bond compared to their 3 months wet storage values.ConclusionThe effects of storage condition and time on the UTS of adhesives were material-dependent.     

The viscoelastic behavior of dental adhesives: A nanoindentation study

ObjectivesIn order to predict the long-term performance of dental adhesives, it is necessary to understand their mechanical properties. The objective of this study was to use a new nanoindentation technique to characterize the in-plane linear viscoelastic properties of dental adhesive layers.MethodsThe dental adhesives used were Clearfil SE Bond (CSE) and Clearfil Tri-S Bond (CTS) by Kuraray Medical and Single Bond (SIB) and Single Bond Plus (SBP) by 3M ESPE. A thin film of each adhesive was made on a micro-glass slide, and was then tested on a nanoindenter system (ENT 1100, Elionix) with a Berkovich indenter at a constant loading rate of 0.1 mN/s up to a maximum load of 1.8 mN. The load–displacement data of the loading segment were fitted to a curve to find best fit parameters for a generalized Kelvin viscoelastic model, from which creep compliance and Young's modulus were calculated. The modulus results were compared to the values calculated by the nanoindentation device.ResultsThe experimental data fitted well to the viscoelastic model for all materials (R > 0.9999). SIB and CTS showed higher creep compliance compared to SBP and CSE. The modulus values obtained using the model were 4.0, 2.6, 2.4 and 4.2 GPa for CSE, CTS, SIB and SBP, respectively. The nanoindentation default software designed for time-independent materials significantly overestimated the modulus values up to 2.5 times.ConclusionAs generally expected for polymer materials, the adhesives tested showed time-dependent viscoelastic behavior. The mechanical evaluation techniques developed for time-independent materials ignore this behavior and may not be appropriate for dental adhesives.     

Oxygen inhibition and incremental layer bond strengths of resin composites

ObjectivesWhen dentists light cure resin composite restorations in increments or after contouring the surface layer to shape with a hand instrument the surface layer is exposed to air during polymerization. The presence of an oxygen inhibited resin surface layer may impact on clinical performance. Conflicting data has been produced in vitro regarding this topic.MethodsTo shed further light on this subject the current investigation assessed the thickness of the oxygen inhibited layer (OIL) and subsequent interfacial bond strength at various times post-cure of an “initial increment” for a range of experimental and commercial resin composites. The latter included conventional methacrylate-based composites and a novel low shrink Silorane resin chemistry product.ResultsA decrease in composite viscosity brought about by an increase in diluent monomer content in the matrix for the experimental composite formulations led to increase in OIL thickness. The OIL surface layer thickness for the commercial methacrylate-based RBC specimens cured in air were 19.2 ± 6.3 and 13.8 ± 5.3 μm, respectively and 9.0 ± 6.6 μm for Silorane. No test material exhibited a measurable OIL thickness polymerized in the nitrogen atmosphere.SignificanceFrom the current findings it may be concluded that incremental bond strength is not wholly reliant on surface inhibition since no differences in bond strength following immediate placement were observed between air and nitrogen atmosphere for any experimental or commercial material. For large restorations requiring multiple increments which are placed on fresh material, the bond strength between successive layers of Silorane should be no different to conventional methacrylate materials. Repair and bonding to aged Silorane restorations may be more problematic as inferior incremental bond strengths ensued when addition was delayed.     

The influence of various light curing units on the cytotoxicity of dental adhesives

ObjectivesThe objective of this study was to test the hypothesis that various light curing units (LCUs) have an influence on the cytotoxic action of adhesive systems.MethodsSamples of the dental adhesives (Syntac^®, iBondTM, Clearfil? Protect Bond, Prime & Bond? NT, Adper? Prompt? L-Pop?) were prepared in microwell plates, making use of the LCUs Voco Polofil Lux (VPL), EMS Swiss Master Light^® (SML) and the LED prototype developed by the IMT of Jena University. To obtain extracts, the samples were topped with cell culture medium, which was changed daily on the 1st to 7th days and then on the 14th, 21st and 28th day, and stored for further use at ?20 °C. Human gingival fibroblasts (HGFs) were cultivated in the extract-containing medium for 48 h. The viability of the HGFs was determined by the neutral red (NR) uptake test. The statistical test was performed by one-way ANOVA according to Bonferroni.ResultsDuring the first few days, reduction of the viability rates of the HGFs by 85–90% were observed in all adhesives. A rise up to a plateau phase was observed at different times depending on the materials. The influence of the LCUs on the cytotoxic action of the dental adhesives was clearly evident for the adhesives Syntac^® and Clearfil? Protect Bond. In case of the Syntac^® extracts, cytotoxicity after polymerization with the VPL was statistically significant reduced compared to the other LCUs used (p < 0.001). A comparison between all the adhesives used proved that Adper? Prompt? L-Pop? and Prime & Bond NT^® had the lowest overall cytotoxicities.SignificanceIn practice, one should use combinations of dental adhesive and LCU in which the material has the least toxic influences.     

Demineralization capacity of commercial 10-methacryloyloxydecyl dihydrogen phosphate-based all-in-one adhesive

Objective

We determined the amounts of calcium salt of 10-methacryloyloxydecyl dihydrogen phosphate (MDP-Ca salt) and dicalcium phosphate dihydride (DCPD) with an amorphous phase developed during the application of commercial MDP-based all-in-one adhesives to enamel and dentin. This is because the demineralization by MDP and following calcium salt formation of MDP may be limited by an ionic bond formation of MDP to hydroxyapaptite in the enamel and dentin and following intermediary layer formation of MDP, since MDP forms a chemically-stable adsorption layer.

A dual energy micro-CT methodology for visualization and quantification of biofilm formation and dentin demineralization

ObjectiveThe aim of this study was to induce artificial caries in human sound dentin by means of a microcosm model using human saliva as source of bacteria and to apply a novel dual-energy micro-CT technique to quantify biofilm formation and evaluate its demineralization potential.DesignEight sound third molars had the occlusal enamel removed by cutting with a diamond disk and five cylindrical cavities (±2 mm diameter; ±1.5 mm depth) were prepared over the dentin surface in each specimen (n = 40 cavities). After sterilization, each specimen received the bacterial salivary inoculum obtained from individuals without any systemic diseases presenting dentin caries lesions and were incubated in BHI added of with 5% sucrose for 96 h to allow biofilm formation. After that, two consecutive micro-CT scans were acquired from each specimen (40kv and 70kv). Reconstruction of the images was performed using standardized parameters. After alignment, registration, filtering and image calculations, a final stack of images containing the biofilm volume was obtained from each prepared cavity. Dentin demineralization degree was quantified by comparison with sound dentin areas. All data were analyzed using Shapiro-Wilk test and Spearman correlation using α=5%.ResultsDual-energy micro-CT technique disclosed biofilm formation in all cavities. Biofilm volume inside each cavity varied from 0.30 to 1.57 mm³. A positive correlation between cavity volume and volume of formed biofilm was obtained (0.77, p < 0.01). The mineral decrease obtained in dentin was high (± 90%) for all cavities and all demineralized areas showed mineral density values lower than a defined threshold for dentin caries (1.2 g/cm³).ConclusionDual-energy micro-CT technique was successful in the quantification of a microcosm human bacterial biofilm formation and to quantify its demineralization potential in vitro.