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.     

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.     

Fatigue of enamel bonds with self-etch adhesives

ObjectiveFatigue testing of adhesive bonds to tooth structures in conjunction with bond strength testing can provide more useful information for examining the effectiveness of dental adhesives. The purpose of this study was to determine the shear bond strength (SBS) and shear fatigue limit (SFL) of composite to enamel bonds using modern adhesive systems.MethodsTwelve specimens each were used to determine 24-h resin composite (Z100-3M ESPE) to enamel shear bond strengths with an etch-and-rinse system (ERA), Adper Single Bond Plus (SB), and four self-etch adhesives (SEA)—Adper Prompt-L-Pop (PLP), Clearfil SE (CSE), Clearfil S³ (CS3) and Xeno IV (X4). A staircase method of fatigue testing was used in a four-station fatigue cycler to determine the SFL of composite to enamel bonds with the adhesives (16–20 specimens for each adhesive) at 0.25 Hz for 40,000 cycles. ANOVA and Tukey's post hoc test were used for the SBS data and a modified t-test with Bonferroni correction was used for comparisons of the SFL.ResultsThe SBS and SFL of the etch-and-rinse system were significantly greater (p < 0.05) than those of the four self-etch adhesives. The SBS and SFL of CSE were also significantly greater than for the other three self-etch systems. The ratio of SFL to SBS was highest with the etch-and-rinse system and the ratio became increasing smaller in the same order that the values for SBS decreased with the self-etch systems.SignificanceThe lower fatigue limits for composite to enamel bonds obtained with the self-etch adhesive systems may indicate that greater enamel margin breakdown will occur with restorations where these systems are used for bonding.     

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).     

Apoptotic effect of different self-etch dental adhesives on odontoblasts in cell cultures

ObjectivesWe aimed to evaluate the potential cytotoxicity (apoptosis-induction) of three types of self-etch dental adhesives: two-component one-step (Xeno III), two-component two-steps (Clearfil Protect Bond) and one-component one-step (Xeno V) on cultured odontoblasts.MethodsEach adhesive was prepared to simulate its clinical manipulation. Cured sterile individual masses were immersed in DMEM and left at 37 °C for 24 h. Then a volume of 100 μL of the extract medium was added to the cultured odontoblasts and incubated for additional 24 h, 48 h and 72 h, respectively. Acridine orange–propidium iodide (AO–PI) labelling was employed to assess the proportion of dead to total number of cells. In addition, an in situ apoptosis detection kit was used to evaluate the DNA cleavage and chromatin condensation employing the immunohistochemical (IHC) technique. Statistical analysis of the data was performed using one-way ANOVA.ResultsBoth apoptosis evaluation methods revealed comparable results with the exception that IHC showed 5–7% less number of dead cells when compared to similar groups evaluated by AO–PI. The percentages of dead to total cells after treatment with Clearfil Protect Bond, Xeno III and Xeno V, were significantly different from the percentage of dead cells after treatment with DMEM alone (?ve control), P value <0.05 and Xeno V dental adhesive had the weakest cytotoxic effect on odontoblasts followed by Xeno III especially after 24 h of incubation. Clearfil Protect Bond had the strongest cytotoxic effect on odontoblasts that was almost closer to that of Staurosporine in DMEM (+ve control).ConclusionAll tested dental adhesives had remarkable adverse effect on the odontoblasts in vitro; this might be of concern when applied clinically in deep cavities where such cytotoxic chemicals become in close contact to dental pulp. Therefore, further in vivo studies on animal models are recommended to support or refute these in vitro findings.     

3-year clinical effectiveness of one-step adhesives in non-carious cervical lesions

ObjectivesDespite representing an important component of current dental adhesives, HEMA has been said to negatively influence the long-term stability of adhesion to dentine and enamel. The aim of this randomised clinical trial was to evaluate the 3-year clinical performance of two one-step self-etch adhesives.MethodsThirty patients had 175 non-carious cervical lesions restored with composite (Gradia Direct Anterior, GC) using either the HEMA-rich adhesive Clearfil Tri-S Bond (C3S; Kuraray) or the HEMA-free adhesive G-Bond (GB; GC). The restorations were evaluated by two examiners at baseline, 6, 12, 24 and 36 months regarding retention, caries recurrence, marginal integrity and discoloration and post-operative sensitivity. The data were statistically analysed with GEE and McNemar tests (p < 0.05).ResultsThe recall rate at 6 and 12 months was 100% and decreased to 96.7% at 24 and 36 months. At 3 years, the retention rate was 93.8% for C3S and 98.8% for GB (p = 0.14). A pairwise comparison showed no significant differences between the two adhesives for all the parameters evaluated, irrespective of the recall (p > 0.05). After 3 years, both adhesives presented an increase in the percentage of clinically acceptable marginal discoloration (C3S: 32.9% and GB: 26.8%) normally associated to clinically acceptable marginal defects (C3S: 35.8% and GB: 26.5%). Only 1 dentine margin of a GB restoration presented a severe marginal defect (1.2%) and 1 C3S restoration presented caries recurrence. The overall 3-year clinical success rate was 92.6% for C3S and 97.6% for GB (p = 0.16).ConclusionBoth one-step self-etch adhesives presented an equally favourable clinical effectiveness at 3 years.Clinical significanceHEMA is a monomer frequently present in dental adhesives in order to increase their wettability and hydrophilicity. However, this monomer negatively influences hydrolytic stability and durability of the adhesive interface complex. In this 3-year clinical trial no significant difference in bonding effectiveness was noticed between a HEMA-rich and HEMA-free one-step adhesive.     

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.     

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.     

One-bottle self-etching adhesives applied to dentine air-abraded using bioactive glasses containing polyacrylic acid: An in vitro microtensile bond strength and confocal microscopy study

ObjectivesThe aim of this study was to test the microtensile bond strength (μTBS) of two “simplified” self-etching adhesives bonded to air-abraded dentine using experimental bioactive glass powders containing polyacrylic acid.MethodsSound dentine specimens were air-abraded using a pure Bioglass 45S5 (Bioglass) powder or two Bioglass powders containing different concentration of polyacrylic acid (PAA: 15 wt% or 40 wt%). The bonding procedures were accomplished by the application of two self-etching adhesives (CS3: Clearfil S3 Bond; Kuraray, Osaka, Japan or GB: G Bond; GC Ltd. Tokyo, Japan). The resin-bonded specimens were cut in beams (0.9 mm²) and the μTBS testing was performed after 24 h or 6 months of phosphate buffer solution (PBS) storage. The results were statistically analysed by three-way ANOVA and Student–Newman–Keuls test used (α = 0.05). Further bonded-dentine specimens were used for the confocal microscopy interfacial characterisation and micropermeability analysis.ResultsThe CS3 adhesive system achieved higher μTBS than those attained in the specimens bonded with GB both after 24 h and 6 months of PBS storage. The CLSM analysis performed after 6 months of PBS storage indicated severe micropermeability within the bonded-dentine interfaces created using GB applied onto dentine air-abraded with Bioglass/PAA-15 and Bioglass/PAA-40. Conversely, CS3 exhibited no dye penetration (micropermeability) at the resin–dentine interface.ConclusionIt is possible to affirm that air-abrasion procedures performed using pure Bioglass or Bioglass containing 15 wt% PAA do not interfere with the immediate bonding performance of self-etching adhesives. However, the durability of the bonded-dentine interfaces created subsequent air-abrasion procedures using bioactive glasses will depend also upon the chemical composition of the self-etch adhesive systems.     

Degree of conversion of Filtek Silorane Adhesive System and Clearfil SE Bond within the hybrid and adhesive layer: An in situ Raman analysis

ObjectivesTo examine the degree of conversion (DC) of the adhesive interfaces created by Filtek Silorane Adhesive and Clearfil SE Bond using micro-Raman spectroscopy.MethodsThe adhesives were applied on human dentin in accordance with manufacturer's instructions. Specimens were cut to expose the bonded interfaces to the micro-Raman beam (Ranishaw InVia; laser wl 785 nm). Raman spectra were collected along the dentin/self-etching primer/adhesive interface at 1 μm intervals. The relative intensities of bands associated with mineral (P–O functional group at 960 cm^?1) and adhesive (C–C–O group at 605 cm^?1) components within the bonded interface were used to detect monomer penetration into the dentin matrix and to calculate the degree of conversion (CC at 1640 cm^?1 as reaction peak, C–C–O at 605 cm^?1 as reference peak). Data were statistically analyzed with two-way ANOVA.ResultsDC of Filtek Silorane Adhesive was 69 ± 7% in the adhesive layer, increasing (p < 0.05) to 93 ± 5% in the primer and 92 ± 9% in the hybrid layer. Clearfil SE Bond showed a DC of 83 ± 3% in the hybrid and 85 ± 3% in the adhesive layer. Thus, Filtek Silorane Adhesive showed a higher DC than Clearfil SE Bond in the hybrid layer (p < 0.05), but a lower DC in the adhesive (p < 0.05).SignificanceAs high DC is a fundamental pre-requisite for the stability of the bond over time, this study supports the hypothesis that optimal stability of Filtek Silorane Adhesive can be obtained. However, further research is needed to investigate the mechanical properties of the hybrid layer created by Filtek Silorane Adhesive and its long-term stability.     

The effect of universal adhesives on dentine collagen

ObjectivesThe purpose of the study was to evaluate the integrity of dentine type I collagen after self-etching (SE) treatments with strong and mild universal adhesives.MethodsCoronal dentine specimens (n = 10/product) were imaged by optical microscopy and analyzed by ATR-FTIR spectroscopy before and after treatment with 32% phosphoric acid gel (PA-negative control), 17% neutral EDTA (ED-positive control) conditioners and Adhese Universal (AD), Clearfil Universal Bond Quick (CQ), G-Premio Bond (GP), Prelude One (PR) and Scotchbond Universal (SB) adhesives. From the spectroscopic analysis the following parameters were determined: a) Extent of dentine demineralization (DM%) and b) percentage area of the Amide I curve-fitted components of β-turns, 3₁₀-helix/β-turns, α-helix, random coils, β-sheets and collagen maturation (R) index. Statistical analysis was performed by one-way ANOVA (DM%), paired t-test/Wilcoxon test (Amide I components) and Spearman correlation coefficient (DM% vs Amide I components) at an a = 0.05 level.ResultsPA, ED and GP removed the smear-layer and opened tubule orifices, whereas all other treatments removed only the intratubular smear-layer fraction. The ranking of the statistically significant differences in DM% was PA > GP > ED > AD, SB, CQ, PR, with AD being significantly different from PR. Regarding the Amide I components, PA demonstrated a significant reduction in β-turns, α-helices and an increase in β-sheets, GP a reduction in β-turns, AD an increase in β-turns and random coils, and CQ an increase in β-turns. PR, SB and ED showed insignificant differences in all the Amide I components. Significant correlations were found between DM%-random coils and DM%-R.SignificanceThe universal adhesives used in the SE mode induced none to minimal changes in dentine collagen structure, without evidence of the destabilization pattern observed after conventional phosphoric acid treatments.     

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.     

Determination of the elastic/plastic transition of human enamel by nanoindentation

Objectives/MethodsFrom a materials scientist's perspective, dental materials used for tooth repair should exhibit compatible mechanical properties. Fulfillment of this criterion is complicated by the fact that teeth have a hierarchical structure with changing mechanical behavior at different length scales. In this study, nanoindentation with an 8 μm spherical indenter was used to determine the elastic/plastic transition under contact loading for enamel.ResultsThe indentation elastic/plastic transition of enamel at the length scale of several hundreds of hydroxyapatite crystallites, which are within one enamel rod, is revealed for the first time. The corresponding penetration depth at the determined indentation yield point of 1.6 GPa and 0.6% strain is only 7 nm. As a consequence of the small depth it is decisive for the experiment to calibrate the indenter tip radius in this loading regime. The elastic modulus of 123 GPa was evaluated directly by the Hertzian penetration and not by the unloading part of the indentation curve.SignificanceWe believe these data are also a valuable contribution to understand the mechanical behavior of enamel and to develop nanoscale biomimetic materials.     

Surface characterisation and bonding of Y-TZP following non-thermal plasma treatment

Objectives(1) To chemically characterise Y-TZP surface via X-ray photoelectron spectroscopy (XPS) and evaluate the surface energy levels (SE) after non-thermal plasma (NTP). (2) To test the microtensile bond strength (MTBS) of Y-TZP bonded to cured composite disks, after a combination of different surface conditioning methods.MethodsTwenty-four Y-TZP discs (13.5 mm × 4 mm) were obtained from the manufacturer and composite resin (Z-100) discs with similar dimensions were prepared. All discs were polished to 600 grit and divided into 8 groups (n = 3 disks each), four control (non-NTP treated) and four experimental (NTP treated for 10 s) groups. All groups received one of the four following treatments prior to cementation with Rely × Unicem cement: sand-blasting (SB), a Clearfil ceramic primer (MDP), sand-blasting + MDP (SBMDP), or baseline (B), no treatment. SE readings and surface roughness parameters were statistically analysed (ANOVA, Tukey's, p < 0.05). Mixed model and paired samples t-tests were used to compare groups on MTBS.ResultsXPS showed increase in O and decrease in C elements after NTP. The polar component increased for BP (42.20 mN/m) and SBP (43.77 mN/m). MTBS values for groups BP (21.3 MPa), SBP (31 MPa), MDPP (30.1 MPa) and SBMDPP (32.3 MPa) were significantly higher in specimens treated with NTP than their untreated counterparts B (9.1 MPa), SB (14.4 MPa), MDP (17.8 MPa) and SBMDP (24.1 MPa).Conclusions(1) Increase of O and decrease of C led to higher surface energy levels dictated by the polar component after NTP; (2) NTP application increased MTBS values of Y-TZP surfaces.     

Effect of residual solvent on performance of acrylamide-containing dental materials

ObjectiveMethacrylamide-based monomers are being pursued as novel, hydrolytically stable materials for use in dental adhesives. The impact of residual solvents, due to the chemical synthesis procedures or the need for solvated adhesives systems, on the kinetics of polymerization and mechanical properties was the aim of the present investigation.MethodsTwo base monomers (70 wt% BisGMA or HEMAM-BDI — newly synthesized secondary methacrylamide) were combined with 30 wt% N,N-dimethylacrylamide. Eethyl acetate (EtOAc), or 75 vol% ethanol/25 vol% water (EtOH/H₂O) were added as solvents in concentrations of 2, 5, 15 and 20 wt%. The resins were made polymerizable by the addition of 0.2 wt% 2,2-dimethoxy-2-phenyl acetophenone (DMPA) and 0.4 wt% diphenyliodonium hexafluorophosphate (DPI-PF6). Specimens (n = 3) were photoactivated with a mercury arc lamp (Acticure 4000, 320–500 nm, 250 mW/cm²) for 5 min. Degree of conversion (DC, %) was tracked in near-IR spectroscopy in real time and yield strength and modulus of elasticity were measured in three-point bending after dry and wet storage (n = 6). The data was subject to one-way ANOVA/Tukey’s Test (p ≤ 0.05), or Student’s t-test (p ≤ 0.001).ResultsIn all groups for both BisGMA and HEMAM-BDI-based materials, DC and DC at Rp_max increased and maximum rate of polymerization decreased as solvent concentration increased. Despite the increased DC, BisGMA mixtures showed a decrease in FS starting at 5 wt% EtOAc or 15 wt% EtOH/H₂O. Yield strength for the HEMAM-BDI groups was overall lower than that of the BisGMA groups, but the modulus of elasticity was significantly higher.SignificanceThe presence of residual solvent, from manufacturing or from practitioner’s handling, affects polymerization kinetics and mechanical properties of resins. Methacrylates appear to be more strongly influenced than methacrylamides.     

Multiple correlations of material parameters of light-cured dental composites

ObjectivesThe aim of this study was to explore the correlations between the Knoop hardness, Young's modulus, viscosity, and polymerization shrinkage of an experimental dental composite, in order to determine the temporal variations of the material properties during the polymerization process.MethodsThe digital image correlation method was employed to measure the polymerization shrinkage along the curing depth of bar-shape specimens (cross-section 4 mm × 2 mm and length 10 mm) of an experimental composite RZE045. The shrinkage data were correlated with the Knoop microhardness measured on specimens prepared in consistent conditions. Another series of tests were performed on cuboid composite samples (cross-section 4 mm × 4 mm and height 5 mm) with different degrees of conversions to determine the correlations among microhardness, Young's modulus and viscosity. Further correlations between shrinkage, Young's modulus and viscosity were then derived, from which the temporal variations of the mechanical parameters during curing were estimated.ResultsAlong the curing depth, the Knoop microhardness of the experimental composite RZE045 decreased more rapidly than its volumetric shrinkage. A power function was employed to describe their relation. On the other hand, Knoop microhardness was found to be proportional to Young's modulus and viscosity. These linear correlations also seemed to be applicable to other materials including unfilled resins, silica glass and other dental composites.SignificanceCorrelations between material parameters of dental composites allowed the rapid temporal variations of Young's modulus and viscosity during curing to be estimated based on the measured polymerization shrinkage-strain history.     

Antibacterial response of oral microcosm biofilm to nano-zinc oxide in adhesive resin

ObjectiveVarious nanoparticles are currently under investigation to impart biointeractivity for dental materials. This study aimed to: (1) formulate an experimental dental adhesive containing ZnO nanoparticles; (2) evaluate its chemical and mechanical properties; and (3) assess the antibacterial response against oral microcosm biofilm.MethodsNanosized ZnO was chemically and morphologically evaluated. ZnO was incorporated at 0 (G_CTRL), 2.5 (G_2.5%), 5 (G_5%) and 7.5 (G_5%) wt.% in an experimental dental adhesive. The adhesives were evaluated for the degree of conversion (DC), flexural strength (FS), and elastic modulus (E). The antibacterial activity was evaluated using a 48 h-microcosm biofilm model after the formation of acquired pellicle on samples’ surfaces. Colony-forming units (CFU), metabolic activity, and live/dead staining were assessed.ResultsNanosized ZnO presented characteristic peaks of Zn-O bonds, and the particles were arranged in agglomerates. The DC ranged from 62.21 (±1.05) % for G_Ctrl to 46.15 (±1.23) % for G_7.5% (p < 0.05). G_7.5% showed lower FS compared to all groups (p < 0.05). Despite achieving higher E (p < 0.05), G_2.5% did not show differences for G_Ctrl regarding the FS (p > 0.05). G_7.5% had lower CFU/mL compared to G_Ctrl for mutans streptococci (p < 0.05) and total microorganisms (p < 0.05), besides presenting lower metabolic activity (p < 0.05) and higher dead bacteria via biofilm staining.SignificanceThe dental adhesives' physicochemical properties were similar to commercial adhesives and in compliance with ISO recommendations. G_7.5% restricted the growth of oral microcosm biofilm without impairing the physicochemical performance.     

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.     

The relationship between Shore hardness of elastomeric dental materials and Young's modulus

ObjectivesHardness of elastomers can be directly related to Young's modulus, a relationship that was investigated in detail by Gent in a paper in 1958. The aim of this study was to test this relationship for 13 dental elastomers (12 silicone and 1 polyether) using the equation derived by Gent and one from BS 903 (1950) that accounts for departures at low values.MethodsThe dental elastomers were subjected to tensile testing and Shore A scale hardness measurements. Young's moduli were calculated from the hardness values using the Gent equation and the BS 903 equation. These calculated values were then compared with values derived experimentally from the tensile tests.ResultsHardness values were in the range 30.2 (±0.5)–62.9 (±0.8) with the corresponding calculated modulus values in the range 1.1–4.1 MPa and 0.9–4.3 MPa for the Gent and modified equations, respectively. Young's modulus values derived from the tensile data were in the range 0.8 (±0.3)–4.1 (±0.3) MPa, showing good agreement with those calculated from the hardness values. Providing viscoelastic creep is minimal during the duration of the test, there is a reasonably well-defined relationship between Shore hardness and Young's modulus in the hardness range studied.SignificanceSimple, non-destructive hardness measurements can be used to determine Young's modulus values. Such values are needed in any calculations of stress distributions in soft lining materials, e.g. by FEA.     

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.