To evaluate resin-dentine bond degradation after 1 year of water storage. Human dentine surfaces ... more To evaluate resin-dentine bond degradation after 1 year of water storage. 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. 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. 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.
Journal of the mechanical behavior of biomedical materials, Jan 19, 2017
The aim of this study was to ascertain the effect of Zn-doping of dental adhesives and mechanical... more 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 aim of this study was to evaluate the changes in the mechanical behavior and bonding capabili... more The aim of this study was to evaluate the changes in the mechanical behavior and bonding capability of Zn-doped resin-infiltrated caries-affected dentin interfaces. Dentin surfaces were treated with 37% phosphoric acid (PA) followed by application of a dentin adhesive, single bond (SB) (PA+SB) or by 0.5 M ethylenediaminetetraacetic acid (EDTA) followed by SB (EDTA+SB). ZnO microparticles of 10 wt. % or 2 wt. % ZnCl2 was added into SB, resulting in the following groups: PA+SB, PA+SB-ZnO, PA+SB-ZnCl2, EDTA+SB, EDTA+SB-ZnO, EDTA+SB-ZnCl2. Bonded interfaces were stored for 24 h, and tested or submitted to mechanical loading. Microtensile bond strength was assessed. Debonded surfaces were evaluated by scanning electron microscopy and elemental analysis. The hybrid layer, bottom of the hybrid layer, and peritubular and intertubular dentin were evaluated using a nanoindenter. The load/displacement responses were used for the nanodynamic mechanical analysis III to estimate complex modulus, tan delta, loss modulus, and storage modulus. The modulus mapping was obtained by imposing a quasistatic force setpoint to which a sinusoidal force was superimposed. Atomic force microscopy imaging was performed. Load cycling decreased the tan delta at the PA+SB-ZnCl2 and EDTA+SB-ZnO interfaces. Tan delta was also diminished at peritubular dentin when PA+SB-ZnO was used, hindering the dissipation of energy throughout these structures. Tan delta increased at the interface after using EDTA+SB-ZnCl2, lowering the energy for recoil or failure. After load cycling, loss moduli at the interface decreased when using ZnCl2 as doping agent, increasing the risk of fracture; but when using ZnO, loss moduli was dissimilarly affected if dentin was EDTA-treated. The border between intertubular and peritubular dentin attained the highest discrepancy in values of viscoelastic properties, meaning a risk for cracking and breakdown of the resin-dentin interface. PA used on dentin provoked differences in complex and storage modulus values at the intertubular and peritubular structures, and these differences were higher than when EDTA was employed. In these cases, the long-term performance of the restorative interface will be impaired.
The aim of this study was to investigate if load cycling affects interfacial integrity of glass i... more The aim of this study was to investigate if load cycling affects interfacial integrity of glass ionomer cements bonded to sound- or caries-affected dentin. A conventional glass ionomer, Ketac Bond, and a resin-modified glass ionomer (Vitrebond Plus), were applied to dentin. Half of the specimens were load cycled. The interfaces were submitted to dye-assisted confocal microscopy evaluation. The unloaded specimens of sound and carious dentin were deficiently hybridized when Ketac Bond was used. Ketac Bond samples showed an absorption layer and an adhesive layer that were scarcely affected by fluorescein penetration (nanoleakage), in sound dentin. Nevertheless, a higher degree of micropermeability was found in carious dentin. In Ketac Bond specimens, load cycling improves the sealing capability and remineralization at the cement-dentin interface as porosity and nanoleakage was reduced. In contrast, samples treated with Vitrebond Plus exhibited a Rhodamine B-labeled absorption layer with scarce nanoleakage in both sound and carious unloaded dentin. The adhesive layer was affected by dye sorption throughout the porous cement-dentin interface. Samples treated with Vitrebond Plus had significant increases in nanoleakage and cement-dye sorption after load cycling. Within the limitations of an in vitro study, it is expected that conventional glass ionomers will provide major clinical efficacy when applied to carious-affected or sound dentin.
Journal of the Mechanical Behavior of Biomedical Materials, 2017
The aim of this study was to evaluate changes in the mechanical and chemical behavior, and bondin... more 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.
Microscopy and microanalysis : the official journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada, Jan 29, 2016
The aim of this research was to assess the ability of amalgam restorations to induce amorphous mi... more The aim of this research was to assess the ability of amalgam restorations to induce amorphous mineral precipitation at the caries-affected dentin substrate. Sound and caries-affected dentin surfaces were subjected to both Zn-free and Zn-containing dental amalgam restorations. Specimens were submitted to thermocycling (100,000 cycles/5°C-55°C, 3 months). Dentin surfaces were studied by atomic force microscopy (nanoroughness), X-ray diffraction, field emission scanning electron microscopy, and energy-dispersive analysis, for physical and morphological surface characterization. Zn-containing amalgam placement reduced crystallinity, crystallite size, and grain size of calcium phosphate crystallites at the dentin surface. Both microstrain and nanoroughness were augmented in caries-affected dentin restored with Zn-containing amalgams. Caries-affected dentin showed the shortest mineral crystallites (11.04 nm), when Zn-containing amalgams were used for restorations, probably leading to a d...
The purposes of this study were to (1) evaluate the shear bond strength of brackets fixed to enam... more The purposes of this study were to (1) evaluate the shear bond strength of brackets fixed to enamel that has been etched for 15 or 60 seconds, (2) correlate etch time with amount of resin remaining on the enamel after debonding; and (3) evaluate enamel morphology after acid etching. Sixty recently extracted human premolars were randomly divided into two groups. Group 1 was etched for 15 seconds, and group 2 for 60 seconds. A 37% phosphoric acid solution was used for etching. The brackets were Mini-Taurus, and the bonding system was Mono-Lok2. After bonding, the teeth were held at 37 degrees C and 100% humidity for at least 48 hours. To debond, a blade was placed at the ligature groove of the bracket. The force in Newtons required to dislodge the bracket was measured, employing a crosshead speed of 1 mm/min. Bond strength was calculated on the basis of bracket area. Immediately after removal of the bracket, the teeth were rinsed and dried using an air-water syringe, and the adhesive remnant index (ARI) was assessed. Enamel surfaces were analyzed using a scanning electron microscope (SEM). The results showed that shear bond strength was greater (p=0.016) when the enamel was etched for 60 seconds, and the amount of adhesive remaining on the teeth was also greater (p=0.001). There was no significant correlation between shear bond strength and the ARI calculated in the total sample (n=60, r=0.017; p>0.05). SEM evaluation revealed that the shorter etching time created a less retentive enamel surface. Absolute enamel loss also decreased.
To evaluate the microtensile bond strength (MTBS) of a resin-based composite to smear layer-cover... more To evaluate the microtensile bond strength (MTBS) of a resin-based composite to smear layer-covered dentin using a self-etching primer, Clearfil SE Bond (CSEB), under two different hydration states. Surface roughness and wettability (contact angle measurements) of water and the CSEB primer were also evaluated on this substrate. Contact angle (CA) measurements were performed on four caries-free extracted human third molars. The specimens were sectioned parallel to the occlusal surface to expose the moderately deep dentin and ground flat (180-grit SiC) under water to provide uniform flat surfaces. In two samples, the smear layer was completely air-dried; in the other two specimens, the smear layer was briefly air-dried. Contact angle measurements were performed to assess wettability of water and CSEB primer using the Axisymmetric Drop Shape Analysis technique. Surface roughness (SR) was determined with a contact profilometer. In another four molars, CSEB was applied to the smear layer-covered dentin with both hydration states. Resin build-ups were performed incrementally with Tetric Ceram. After storage for 24 hours in water at 37 degrees C, the teeth were sectioned to obtain bonded beams with an average cross-sectional area of 1.0 mm2. Each beam was tested in tension in an Instron machine at 0.5 mm/minute. Kolmogorov-Smirnov and Student t-tests were performed at a 95% significance level. Observed water contact angles were lower on the hydrated smear layer but no differences were found between contact angles on completely and briefly air-dried smear layer when the primer was used for CA measurements. SR was similar for both substrates and MTBS was greater when the adhesive was applied on the completely air-dried smear layer.
To investigate the surface roughness and the initial adhesion of Streptococcus mutans on seven de... more To investigate the surface roughness and the initial adhesion of Streptococcus mutans on seven dental resin-based restorative materials. Five cylinder specimens, with 5 mm diameter and 3 mm height, of three resin composites (Z100, Prodigy and Tetric), three polyacid modified composite resins (Compoglass, Compoglass F and Dyract AP) and a resin modified glass ionomer (Vitremer) were made. Materials were handled following manufacturer's instructions. The materials were polished up to 1200 grit SiC abrasive paper under running water in an automatic polisher. Surface roughness measurements were carried out by a profilometer. Five diametrical measurements were made and Ra was calculated in microm. The bacterial initial cell adhesion assay was performed with S. mutans ATCC 25175. The initial adhesion of Streptococcus mutans on the materials tested was observed by SEM. ANOVA and Student-Newman-Keuls multiple comparisons were used. The statistical analyses showed no significant differences in initial cell adhesion among tested materials, even when the resin-modified glass inonomer showed a rougher surface than the rest of the materials.
Journal of the Mechanical Behavior of Biomedical Materials, 2016
The purpose of this study was to evaluate the remineralization ability of an etch-and-rinse Zn-do... more 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.
To investigate the resistance to degradation of resin modified glass-ionomer cement (RMGIC) and a... more To investigate the resistance to degradation of resin modified glass-ionomer cement (RMGIC) and adhesive/composite restorations in sound and simulated caries-affected dentin of primary teeth subjected to carious challenge using a pH-cycling model and load-cycling, by means of a microtensile test. Occlusal cavities were prepared in 60 sound exfoliated primary second molars. Half the specimens were submitted to pH-cycling to induce simulated caries lesion. The teeth were randomly restored with one of the two materials: (1) a RMGIC (Vitremer) and (2) a total-etch adhesive system (Adper Single Bond 2) followed by resin composite (Filtek Z100). After storage in distilled water at 37 degrees C for 24 hours, control group specimens were subjected to test procedures while the specimens in the experimental groups were subjected to two different aging methods: load-cycling (50,000 cycles, 90N, 3Hz) or carious challenge (pH-cycling: alternately 8 hours in demineralizing and 16 hours in remineralizing solutions, for 10 days). Teeth were sectioned into 1 mm2 beams and tested to failure under tension. ANOVA and multiple-comparisons tests were used (P<0.05). Vitremer bond strength was not altered by the condition of dentin. Conversely, Adper Single Bond 2 showed significantly lower bond strength values when bonded to simulated caries-affected dentin. Load-cycling did not influence bond strength for any of the tested materials, while carious challenge resulted in a significant decrease in microtensile bond strengths of Adper Single Bond 2, but not of Vitremer restorations.
To evaluate the bond strength (microTBS) of self-etching adhesives in different solvent evaporati... more To evaluate the bond strength (microTBS) of self-etching adhesives in different solvent evaporation conditions. 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. 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. The use of a warm air-dry stream seems to be a clinical tool to improve the bond strength to self-etching adhesives.
To evaluate the influence of CAD/CAM scanning method (wax-up digitization vs. direct scanning of ... more To evaluate the influence of CAD/CAM scanning method (wax-up digitization vs. direct scanning of tooth preparation) and finish line type (chamfer vs. shoulder) on the vertical fit of zirconia frameworks for three-unit posterior-lower bridges. 30 sets of two stainless steel master dies were prepared with different marginal designs (chamfer and shoulder) around the contour of each abutment. Over these samples, 30 structures for three-unit posterior-lower bridges were made with Cercon Smart Ceramics CAD/CAM system (Dentsply). An optical laser digitized the wax patterns of 15 bridge structures, and 15 pairs of master dies were directly scanned for designing by computer the remaining half of frames. All zirconia milled structures were luted onto the metallic models with a special clamp made-up to maintain constant seating pressure. Vertical discrepancy around the margins was assessed under scanning electron microscopy (SEM). Misfit data was analyzed using two-way ANOVA and Tukey's test for multiple comparisons at a = 0.05. Vertical discrepancy of the wax-up/digitized bridge structures was significantly higher than that of the computer-designed frameworks (P < 0.0001). No statistically significant differences were found between the chamfer and shoulder vertical misfit values assessed around the metallic models margins (P = 0.55).
To evaluate resin-dentine bond degradation after 1 year of water storage. Human dentine surfaces ... more To evaluate resin-dentine bond degradation after 1 year of water storage. 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. 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. 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.
Journal of the mechanical behavior of biomedical materials, Jan 19, 2017
The aim of this study was to ascertain the effect of Zn-doping of dental adhesives and mechanical... more 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 aim of this study was to evaluate the changes in the mechanical behavior and bonding capabili... more The aim of this study was to evaluate the changes in the mechanical behavior and bonding capability of Zn-doped resin-infiltrated caries-affected dentin interfaces. Dentin surfaces were treated with 37% phosphoric acid (PA) followed by application of a dentin adhesive, single bond (SB) (PA+SB) or by 0.5 M ethylenediaminetetraacetic acid (EDTA) followed by SB (EDTA+SB). ZnO microparticles of 10 wt. % or 2 wt. % ZnCl2 was added into SB, resulting in the following groups: PA+SB, PA+SB-ZnO, PA+SB-ZnCl2, EDTA+SB, EDTA+SB-ZnO, EDTA+SB-ZnCl2. Bonded interfaces were stored for 24 h, and tested or submitted to mechanical loading. Microtensile bond strength was assessed. Debonded surfaces were evaluated by scanning electron microscopy and elemental analysis. The hybrid layer, bottom of the hybrid layer, and peritubular and intertubular dentin were evaluated using a nanoindenter. The load/displacement responses were used for the nanodynamic mechanical analysis III to estimate complex modulus, tan delta, loss modulus, and storage modulus. The modulus mapping was obtained by imposing a quasistatic force setpoint to which a sinusoidal force was superimposed. Atomic force microscopy imaging was performed. Load cycling decreased the tan delta at the PA+SB-ZnCl2 and EDTA+SB-ZnO interfaces. Tan delta was also diminished at peritubular dentin when PA+SB-ZnO was used, hindering the dissipation of energy throughout these structures. Tan delta increased at the interface after using EDTA+SB-ZnCl2, lowering the energy for recoil or failure. After load cycling, loss moduli at the interface decreased when using ZnCl2 as doping agent, increasing the risk of fracture; but when using ZnO, loss moduli was dissimilarly affected if dentin was EDTA-treated. The border between intertubular and peritubular dentin attained the highest discrepancy in values of viscoelastic properties, meaning a risk for cracking and breakdown of the resin-dentin interface. PA used on dentin provoked differences in complex and storage modulus values at the intertubular and peritubular structures, and these differences were higher than when EDTA was employed. In these cases, the long-term performance of the restorative interface will be impaired.
The aim of this study was to investigate if load cycling affects interfacial integrity of glass i... more The aim of this study was to investigate if load cycling affects interfacial integrity of glass ionomer cements bonded to sound- or caries-affected dentin. A conventional glass ionomer, Ketac Bond, and a resin-modified glass ionomer (Vitrebond Plus), were applied to dentin. Half of the specimens were load cycled. The interfaces were submitted to dye-assisted confocal microscopy evaluation. The unloaded specimens of sound and carious dentin were deficiently hybridized when Ketac Bond was used. Ketac Bond samples showed an absorption layer and an adhesive layer that were scarcely affected by fluorescein penetration (nanoleakage), in sound dentin. Nevertheless, a higher degree of micropermeability was found in carious dentin. In Ketac Bond specimens, load cycling improves the sealing capability and remineralization at the cement-dentin interface as porosity and nanoleakage was reduced. In contrast, samples treated with Vitrebond Plus exhibited a Rhodamine B-labeled absorption layer with scarce nanoleakage in both sound and carious unloaded dentin. The adhesive layer was affected by dye sorption throughout the porous cement-dentin interface. Samples treated with Vitrebond Plus had significant increases in nanoleakage and cement-dye sorption after load cycling. Within the limitations of an in vitro study, it is expected that conventional glass ionomers will provide major clinical efficacy when applied to carious-affected or sound dentin.
Journal of the Mechanical Behavior of Biomedical Materials, 2017
The aim of this study was to evaluate changes in the mechanical and chemical behavior, and bondin... more 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.
Microscopy and microanalysis : the official journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada, Jan 29, 2016
The aim of this research was to assess the ability of amalgam restorations to induce amorphous mi... more The aim of this research was to assess the ability of amalgam restorations to induce amorphous mineral precipitation at the caries-affected dentin substrate. Sound and caries-affected dentin surfaces were subjected to both Zn-free and Zn-containing dental amalgam restorations. Specimens were submitted to thermocycling (100,000 cycles/5°C-55°C, 3 months). Dentin surfaces were studied by atomic force microscopy (nanoroughness), X-ray diffraction, field emission scanning electron microscopy, and energy-dispersive analysis, for physical and morphological surface characterization. Zn-containing amalgam placement reduced crystallinity, crystallite size, and grain size of calcium phosphate crystallites at the dentin surface. Both microstrain and nanoroughness were augmented in caries-affected dentin restored with Zn-containing amalgams. Caries-affected dentin showed the shortest mineral crystallites (11.04 nm), when Zn-containing amalgams were used for restorations, probably leading to a d...
The purposes of this study were to (1) evaluate the shear bond strength of brackets fixed to enam... more The purposes of this study were to (1) evaluate the shear bond strength of brackets fixed to enamel that has been etched for 15 or 60 seconds, (2) correlate etch time with amount of resin remaining on the enamel after debonding; and (3) evaluate enamel morphology after acid etching. Sixty recently extracted human premolars were randomly divided into two groups. Group 1 was etched for 15 seconds, and group 2 for 60 seconds. A 37% phosphoric acid solution was used for etching. The brackets were Mini-Taurus, and the bonding system was Mono-Lok2. After bonding, the teeth were held at 37 degrees C and 100% humidity for at least 48 hours. To debond, a blade was placed at the ligature groove of the bracket. The force in Newtons required to dislodge the bracket was measured, employing a crosshead speed of 1 mm/min. Bond strength was calculated on the basis of bracket area. Immediately after removal of the bracket, the teeth were rinsed and dried using an air-water syringe, and the adhesive remnant index (ARI) was assessed. Enamel surfaces were analyzed using a scanning electron microscope (SEM). The results showed that shear bond strength was greater (p=0.016) when the enamel was etched for 60 seconds, and the amount of adhesive remaining on the teeth was also greater (p=0.001). There was no significant correlation between shear bond strength and the ARI calculated in the total sample (n=60, r=0.017; p>0.05). SEM evaluation revealed that the shorter etching time created a less retentive enamel surface. Absolute enamel loss also decreased.
To evaluate the microtensile bond strength (MTBS) of a resin-based composite to smear layer-cover... more To evaluate the microtensile bond strength (MTBS) of a resin-based composite to smear layer-covered dentin using a self-etching primer, Clearfil SE Bond (CSEB), under two different hydration states. Surface roughness and wettability (contact angle measurements) of water and the CSEB primer were also evaluated on this substrate. Contact angle (CA) measurements were performed on four caries-free extracted human third molars. The specimens were sectioned parallel to the occlusal surface to expose the moderately deep dentin and ground flat (180-grit SiC) under water to provide uniform flat surfaces. In two samples, the smear layer was completely air-dried; in the other two specimens, the smear layer was briefly air-dried. Contact angle measurements were performed to assess wettability of water and CSEB primer using the Axisymmetric Drop Shape Analysis technique. Surface roughness (SR) was determined with a contact profilometer. In another four molars, CSEB was applied to the smear layer-covered dentin with both hydration states. Resin build-ups were performed incrementally with Tetric Ceram. After storage for 24 hours in water at 37 degrees C, the teeth were sectioned to obtain bonded beams with an average cross-sectional area of 1.0 mm2. Each beam was tested in tension in an Instron machine at 0.5 mm/minute. Kolmogorov-Smirnov and Student t-tests were performed at a 95% significance level. Observed water contact angles were lower on the hydrated smear layer but no differences were found between contact angles on completely and briefly air-dried smear layer when the primer was used for CA measurements. SR was similar for both substrates and MTBS was greater when the adhesive was applied on the completely air-dried smear layer.
To investigate the surface roughness and the initial adhesion of Streptococcus mutans on seven de... more To investigate the surface roughness and the initial adhesion of Streptococcus mutans on seven dental resin-based restorative materials. Five cylinder specimens, with 5 mm diameter and 3 mm height, of three resin composites (Z100, Prodigy and Tetric), three polyacid modified composite resins (Compoglass, Compoglass F and Dyract AP) and a resin modified glass ionomer (Vitremer) were made. Materials were handled following manufacturer's instructions. The materials were polished up to 1200 grit SiC abrasive paper under running water in an automatic polisher. Surface roughness measurements were carried out by a profilometer. Five diametrical measurements were made and Ra was calculated in microm. The bacterial initial cell adhesion assay was performed with S. mutans ATCC 25175. The initial adhesion of Streptococcus mutans on the materials tested was observed by SEM. ANOVA and Student-Newman-Keuls multiple comparisons were used. The statistical analyses showed no significant differences in initial cell adhesion among tested materials, even when the resin-modified glass inonomer showed a rougher surface than the rest of the materials.
Journal of the Mechanical Behavior of Biomedical Materials, 2016
The purpose of this study was to evaluate the remineralization ability of an etch-and-rinse Zn-do... more 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.
To investigate the resistance to degradation of resin modified glass-ionomer cement (RMGIC) and a... more To investigate the resistance to degradation of resin modified glass-ionomer cement (RMGIC) and adhesive/composite restorations in sound and simulated caries-affected dentin of primary teeth subjected to carious challenge using a pH-cycling model and load-cycling, by means of a microtensile test. Occlusal cavities were prepared in 60 sound exfoliated primary second molars. Half the specimens were submitted to pH-cycling to induce simulated caries lesion. The teeth were randomly restored with one of the two materials: (1) a RMGIC (Vitremer) and (2) a total-etch adhesive system (Adper Single Bond 2) followed by resin composite (Filtek Z100). After storage in distilled water at 37 degrees C for 24 hours, control group specimens were subjected to test procedures while the specimens in the experimental groups were subjected to two different aging methods: load-cycling (50,000 cycles, 90N, 3Hz) or carious challenge (pH-cycling: alternately 8 hours in demineralizing and 16 hours in remineralizing solutions, for 10 days). Teeth were sectioned into 1 mm2 beams and tested to failure under tension. ANOVA and multiple-comparisons tests were used (P<0.05). Vitremer bond strength was not altered by the condition of dentin. Conversely, Adper Single Bond 2 showed significantly lower bond strength values when bonded to simulated caries-affected dentin. Load-cycling did not influence bond strength for any of the tested materials, while carious challenge resulted in a significant decrease in microtensile bond strengths of Adper Single Bond 2, but not of Vitremer restorations.
To evaluate the bond strength (microTBS) of self-etching adhesives in different solvent evaporati... more To evaluate the bond strength (microTBS) of self-etching adhesives in different solvent evaporation conditions. 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. 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. The use of a warm air-dry stream seems to be a clinical tool to improve the bond strength to self-etching adhesives.
To evaluate the influence of CAD/CAM scanning method (wax-up digitization vs. direct scanning of ... more To evaluate the influence of CAD/CAM scanning method (wax-up digitization vs. direct scanning of tooth preparation) and finish line type (chamfer vs. shoulder) on the vertical fit of zirconia frameworks for three-unit posterior-lower bridges. 30 sets of two stainless steel master dies were prepared with different marginal designs (chamfer and shoulder) around the contour of each abutment. Over these samples, 30 structures for three-unit posterior-lower bridges were made with Cercon Smart Ceramics CAD/CAM system (Dentsply). An optical laser digitized the wax patterns of 15 bridge structures, and 15 pairs of master dies were directly scanned for designing by computer the remaining half of frames. All zirconia milled structures were luted onto the metallic models with a special clamp made-up to maintain constant seating pressure. Vertical discrepancy around the margins was assessed under scanning electron microscopy (SEM). Misfit data was analyzed using two-way ANOVA and Tukey's test for multiple comparisons at a = 0.05. Vertical discrepancy of the wax-up/digitized bridge structures was significantly higher than that of the computer-designed frameworks (P < 0.0001). No statistically significant differences were found between the chamfer and shoulder vertical misfit values assessed around the metallic models margins (P = 0.55).
Uploads
Papers by Raquel Osorio