Measurement of the full-field polymerization shrinkage and depth of cure of dental composites using digital image correlation

ObjectivesThe aim of this study was to measure the full-field polymerization shrinkage of dental composites using optical image correlation method.MethodsBar specimens of cross-section 4 mm × 2 mm and length 10 mm approximately were light cured with two irradiances, 450 mW/cm² and 180 mW/cm², respectively. The curing light was generated with Optilux 501 (Kerr) and the two different irradiances were achieved by adjusting the distance between the light tip and the specimen. A single-camera 2D measuring system was used to record the deformation of the composite specimen for 30 min at a frequency of 0.1 Hz. The specimen surface under observation was sprayed with paint to produce sufficient contrast to allow tracking of individual points on the surface. The curing light was applied to one end of the specimen for 40 s during which the painted surface was fully covered. After curing, the cover was removed immediately so that deformation of the painted surface could be recorded by the camera. The images were then analyzed with specialist software and the volumetric shrinkage determined along the beam length.ResultsA typical shrinkage strain field obtained on a specimen surface was highly non-uniform, even at positions of constant distance from the irradiation surface, indicating possible heterogeneity in material composition and shrinkage behavior in the composite. The maximum volumetric shrinkage strain of ～1.5% occurred at a subsurface distance of about 1 mm, instead of at the irradiation surface. After reaching its peak value, the shrinkage strain then gradually decreased with increasing distance along the beam length, before leveling off to a value of approximately 0.2% at a distance of 4–5 mm. The maximum volumetric shrinkage obtained agreed well with the value of 1.6% reported by the manufacturer for the composite examined in this work. Using irradiance of 180 mW/cm² resulted in only slightly less polymerization shrinkage than using irradiance of 450 mW/cm².SignificanceCompared to the other measurement methods, the image correlation method is capable of producing full-field information about the polymerization shrinkage behavior of dental composites.     

Thickness and surface structure of a ceramic layer created on three indirect resin composites with aerosol deposition

PurposeAerosol deposition is a technology for coating ceramics with impact consolidation at room temperature. The aim of the present study was to investigate the thickness and the microstructure of the aluminium oxide layer on different three dental resin composite materials created by means of aerosol deposition.MethodsDisk-shaped specimens were fabricated with three resin composites (Estenia C&B, Targis, and Gradia). The specimens were ground flat, and then subjected to aerosol deposition using aluminium oxide submicron particles without inducing a localized temperature rise. The average thickness (AVH) and maximum thickness (Hmax) of the aluminium oxide layer deposited on the resin composite material were measured using a profilometer. Data were analyzed by ANOVA and post hoc Tukey compromise test at α = 0.05. The specimen surfaces were also observed using a scanning electron microscope.ResultsThe aluminium oxide layer formed on Estenia C&B (AVH 8.1 μm, Hmax 9.1 μm) and Targis (AVH 7.7 μm, Hmax 8.9 μm) were significantly thicker than that on Gradia (AVH 4.2 μm, Hmax 5.4 μm). The micrograph showed that the aluminium oxide layer on Estenia C&B was similar to that on Targis. However, the aerosol deposition area of Gradia was seen relatively rough and partly caved.ConclusionsThe type of resin composite affected the microstructure of the deposited aluminium oxide layer. The highly filled light- and heat-cured resin composites are advantageous as a target material rather than the lower filled light-cured resin composite.     

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.     

The effect of resin composite pre-heating on monomer conversion and polymerization shrinkage

ObjectivesTo determine monomer conversion and polymerization shrinkage of a resin composite after different pre-heating procedures and storage intervals.MethodsFor a commercial resin-based composite the immediate (5 min) and final (24 h) degree of conversion was measured on top and bottom surfaces utilizing FTIR spectroscopy. Composite pre-heating temperatures were selected between 10 and 68 °C. Polymerization shrinkage was measured according to Archimedes’ principles of buoyancy after 5 min at respective pre-heating temperatures and after 24 h dark and wet storage at 37 °C. Intra-cavity temperature development was monitored using a K-type thermocouple.ResultsNo significant increase in immediate as well as in final degree of conversion were measured from composite pre-heating at 68 °C compared to 54 and 39 °C. Linear correlations were detected immediately after photo-polymerization and on the top surface after 24 h storage. Polymerization shrinkage as a function of pre-heating temperatures exhibited a linear correlation after 5 min, but no statistically different behavior after 24 h.SignificancePre-heating of resin composites does not increase degree of conversion over time. It can be clinically beneficial, due to a superior marginal adaptation. This advantageous effect of reduced material paste viscosity has to be clinically addressed, since temperature rapidly drops to the physiological level upon removal from the pre-heating device.     

Vertical and horizontal polymerization shrinkage in composite restorations

ObjectivePolymerization shrinkage developed in vertical and horizontal directions after light activation of light-curing composite restorative materials. The purpose of this study was to examine the effects of vertical and horizontal polymerization shrinkage on: (a) dimensional changes of resin composites in tooth cavities; (b) shear bond strengths to enamel and dentin; and (c) marginal gap width in a non-reacting Teflon mold.MethodsVertical and horizontal polymerization shrinkage in tooth cavities were measured immediately (3 min) after light activation. With the same time lapse, shear bond strengths to enamel and dentin and marginal gap widths in Teflon mold were also measured.ResultsThere was a significant correlation between vertical and horizontal polymerization shrinkage (r = 0.647, p = 0.043) in the tooth cavity. Composite materials which produced small vertical shrinkage also produced smaller horizontal shrinkage. Composite materials which produced small vertical shrinkage in the tooth cavity exhibited greater shear bond strengths to both enamel (r = −0.697, p = 0.025) and dentin (r = −0.752, p = 0.012). Composite materials which produced smaller horizontal shrinkage produced smaller marginal gap widths in the Teflon mold (r = 0.829, p = 0.003). No relationships were observed between horizontal shrinkage in the tooth cavity and shear bond strengths to both enamel and dentin (p > 0.05).SignificanceDuring the early stage of setting (<3 min) in tooth cavities, the vertical shrinkage of light-activated composite restorative materials was correlated with horizontal shrinkage.     

Conversion kinetics of rapid photo-polymerized resin composites

ObjectiveTo measure the degrees of conversion (DC), conversion kinetics, and the effect of post-irradiation time on rapid photo-polymerized bulk-fill resin composites under conditions equivalent to clinical depths of 1 and 4 mm.Methods36 specimens (n = 3), based on two resin composites incorporating PowerCure rapid-polymerization technology in two consistencies (PFill; PFlow) and two comparators with matching consistencies (Eceram; EFlow), were investigated from the same manufacturer (Ivoclar AG, Liechtenstein). Specimens were prepared within 4 mm diameter cylindrical molds, of either 1 mm or 4 mm depths respectively, to simulate near-surface and deep locations in a bulk-fill restoration. The independent variables in this study were: materials, thickness and time. Two high irradiance polymerization protocols were utilized for PowerCure materials: 2000 and 3050 mW/cm² for 5 and 3 s, respectively. A standard (1200 mW/cm²) polymerization protocol was used with control materials. FTIR was utilized to measure DC in real-time for 24 h post-irradiation. The data were analyzed using Welch’s-ANOVA, Games-Howell post-hoc test, kinetic dual-exponential sum function and independent sample t-tests (p = 0.05).ResultsThe DC of the materials ranged between 44.7–59.0 % after 5 min, which increased after 24 h reaching 55.7–71.0 % (p < 0.05). Specimen thickness did not influence the overall DC. At 5 min, the highest DC was shown in EFlow. But PFlow, irradiated for 3 s and 5 s exhibited comparable results (p > 0.05). PFill composite irradiated with the 3 s and 5 s protocols did not differ from ECeram (p > 0.05). Specimen thickness and material viscosity affected polymerization kinetics and rate of polymerization (RP_max). Faster polymerization occurred in 1 mm specimens (except PFill-5 s and ECeram). PFill and PFlow exhibited faster conversion than the controls. RP_max varied across the specimen groups between 4.3–8.8 %/s with corresponding DC _RPmax between 22.2–45.3 %.SignificancePolymerization kinetics and RP_max were influenced by specimen thickness and material viscosity. PFill and PFlow materials produced an overall comparable conversion at 5 min and 24 h post-irradiation, despite the ultra-short irradiation times, throughout the 4 mm specimen thickness.     

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.     

Volumetric polymerization shrinkage and its comparison to internal adaptation in bulk fill and conventional composites: A μCT and OCT in vitro analysis

ObjectiveTo quantify the volumetric polymerization shrinkage (VPS) of different conventional and bulk fill resin composites, through micro-computed tomography (μCT), and qualitative comparison of gap formation through optical coherence tomography (OCT).MethodsBox-shaped class I cavities were prepared in 30 third-molars and divided into 5 groups (n = 6): G1- Filtek Z100 (Z100); G2- Tetric Evoceram Bulk Fill (TEC); G3- Tetric EvoFlow Bulk fill (TEF); G4- Filtek Bulk fill (FBU); and G5- Filtek Bulk fill Flowable (FBF). All groups were treated with Adper Single Bond Plus adhesive and light cured (Bluephase 20i). Each tooth was scanned three times using a μCT apparatus: after cavity preparation (empty scan); after cavity filling (uncured scan) and after light curing of the restorations (cured scan). The μCT images were imported into a three-dimensional rendering software, and volumetric polymerization shrinkage percentage was calculated (%) for each sample. In the same images, interfacial gaps in the pulpal floor were qualitatively evaluated. After μCT evaluation, the pulpal floor from each tooth was polished until a thin tooth structure was obtained and OCT images were obtained by scanning the pulpal portion. Gap formation was observed and qualitatively compared to the μCT images.ResultsVPS means ranged from 2.31 to 3.96% for the studied resin composites. The bulk fill materials, either high viscosity or flowable, were not statistically different from each other (p > 0.05). The conventional resin composite Z100 presented statistically higher VPS than both high viscosity bulk fill materials studied (p < 0.05), although it was statistically similar to the flowable bulk fill materials studied (p > 0.05). Both μCT and OCT methodologies enabled gap formation visualization, and images from both technologies could be associated. Gap formation was mostly observed for G1-Z100, G4-FBU, and G5-FBF. VPS% and pulpal gap formation could not be completely associated with each other for all groups and samples. Voids were observed in most of the resin composite fillings, and most VPS were observed in the occlusal area of the samples.SignificanceVolumetric polymerization shrinkage was material-dependent, although bulk fill materials did not differ from each other. Both μCT and OCT enabled interfacial pulpal gap formation visualization. VPS and gap formation cannot be completely associated with one another.     

Effect of delivering light in specific narrow bandwidths from 394 to 515 nm on the micro-hardness of resin composites

ObjectivesThis study investigated the wavelength-dependent photosensitivity of eleven resin composites (Admira A2, Heliomolar A2, Herculite XRV A2, Pyramid Dentin A2, Solitaire 2 A2, Z250 A2, Ælite LS A2, Vit-l-escence A2, Tetric Ceram Bleach XL, Tetric Ceram A2, Pyramid Enamel Neutral).MethodsResin composites 1.6 mm thick were exposed to narrow bandwidths of light at the following peak wavelengths: 394, 400, 405, 410, 415, 420, 430, 436, 442, 450, 455, 458, 467, 470, 480, 486, 493, 500, 505, and 515 ± 5 nm. A spectroradiometer was used to ensure that the same irradiance (mW/cm²) and total energy density (J/cm²) was delivered through each filter. For each resin composite, three specimens were exposed through each filter. The Knoop micro-hardness at the top and bottom of the composites was then measured. The wavelength-dependent photosensitivity of each resin composite was analyzed by plotting the mean hardness achieved at each wavelength.ResultsThe composites responded variably when they received light through the narrow bandpass filters. Six resin composites had a single peak of wavelength-dependent photosensitivity at ～470 nm. Four resin composites had two peaks of wavelength-dependent photosensitivity at ～470 and ～405 nm. One resin composite had a single peak of wavelength-dependent photosensitivity at ～405 nm and was only sensitive to light below 436 nm.SignificanceUsing light delivered through narrow bandpass filters is a convenient method to determine the wavelength-dependent photosensitivity of resins and can be used to predict the performance of dental curing lights.     

Color and contrast ratio of resin composites for whitened teeth

ObjectivesThe purpose of this study was to determine the optical properties, color and contrast ratio (CR) of commercially available resin composites marketed for the restoration of whitened teeth.MethodsTwenty-six resin composites designed for restoration of whitened teeth and four shade B1 (control) were evaluated. Five resin composite disks (d = 12 mm, h = 1.54 mm) were fabricated for each shade of composite and were stored in water at 37 °C for at least 24 h. A colorimeter was used to measure specimen color over both white and black backgrounds. CIELAB and CIExyY color spaces were used. The CIELAB color notation system provides values for L*a*b*. The CIExyY system provides lightness and chromaticity values, where Y represents lightness and xy chromaticity. The contrast ratio (CR) was assessed using, CIE xyY, of the specimens against black (Yb) and white (Yw) backgrounds, with CR = Yb/Yw. The data for L*, a*, b* and CR were analyzed by one-way ANOVA, Tukey's test, and the correlation L* and CR was analyzed by Pearson correlation test (α = 0.05).ResultsSignificantly different L*, a*, b* values and CR were observed. Premise XL2 had the highest L* and CR values and Vit-l-escence PS had the lowest. Vit-l-escence PS had the highest a* value and Point 4XL2 had the lowest, Premise XL1 had the highest b* value and Supreme WB the lowest. The L* and CR correlation was positive and statistically significant.ConclusionsComposites designated for whitened teeth have different levels of color and contrast ratio. Awareness of the optical properties of the composites allows the operator to choose the appropriate materials to mimic the remaining tooth structure.     

Response of composite resins to preheating and the resulting strengthening of luted feldspar ceramic

ObjectiveThis study evaluated the influence of preheating different composite resins on their viscosity and strengthening yielded to ceramic.MethodsModulus of elasticity, Poisson’s ratio, and degree of CC conversion were measured for three restorative composite resins (Z100–microhybrid; Empress Direct–nanohybrid; Estelite Omega–supranano) and one photoactivated resin cement (RelyX Veneer). Viscosity was measured during a heating-cooling curve (25 °C–69 °C–25 °C) and also using isothermal analyses at 25 °C and 69 °C. Feldspar ceramic disks simulating veneers were bonded with the luting materials. Biaxial flexural strength, characteristic strength, and Weibull modulus were calculated at axial positions (z = 0 and z = −t₂) of the bilayers. Film thickness was measured and morphology at the bonded interfaces was observed. Data were statistically analyzed (α = 0.05).ResultsA gradual decrease in viscosity was noticed as the rheometer temperature gradually increased. Viscosity differences between the composite resins were large at the beginning of the analysis, but minor at 69 °C. At 25 °C, the composites were up to 38 times more viscous than the resin cement; at 69 °C the difference was 5-fold. CC conversion was similar between all resin-based agents. The resin cement yielded lower film thickness than the composites. All resin-based agents were able to infiltrate the ceramic porosities at the interface and strengthen the ceramic. However, the magnitude of the strengthening effect was higher for the preheated composite resins, particularly at z = −t₂.SignificanceSelection of composite resin impacts its response to preheating and the resulting viscosity, film thickness, and magnitude of ceramic strengthening.     

Influence of TiO2 nanoparticles on the optical properties of resin composites

ObjectivesTo determine the influence of titanium dioxide (TiO₂) nanoparticle addition on the opalescence, color, translucency and fluorescence of experimental resin composites.MethodsA light curing resin matrix was made by mixing 60 wt.% Bis-GMA and 40 wt.% TEGDMA. Silane coated glass filler (mean particle size: 1.55 μm) was added in the ratio of 50 wt.% of the resin composites. A fluorescent whitening agent was also added (0.05 wt.%). TiO₂ nanoparticles (<40 nm) were added with the concentrations of 0, 0.1, 0.25 and 0.5 wt.%. Reflected and transmitted colors of 1 and 2 mm thick specimens were measured relative to the illuminant D65 with reflection spectrophotometers. Opalescence parameter (OP), color difference (ΔE*_ab), translucency parameter (TP), fluorescence parameter (FL), and fluorescence and opalescence spectra were calculated.ResultsFor the 1 mm thick specimens measured with 3 mm × 8 mm rectangular aperture, when the concentration of TiO₂ increased from 0% to 0.5%, OP increased from 2.4 to 18.0, TP decreased from 35.4 to 13.1, and fluorescence spectra remained unchanged. Color difference between these specimens was in the range of 3.4–6.6 ΔE*_ab units. OP values were significantly influenced by the thickness of the specimens and the configuration of the spectrophotometers (p < 0.05).SignificanceAddition of TiO₂ nanoparticles significantly increased the opalescence of resin composites while leaving the fluorescence spectra unchanged; however, it significantly decreased the translucency and also changed the color (p < 0.05). Resin composites with 0.1–0.25% TiO₂ nanoparticle would simulate the opalescence of human enamel.     

Viscosity and stickiness of dental resin composites at elevated temperatures

ObjectiveTo investigate the influence of pre-heating different classes of dental resin composites on viscosity and stickiness at five different temperatures.MethodsSix flowable, five conventional packable, and one thermo-viscous bulk-fill resin composites were heated up to 54 °C in a plate-plate rheometer to determine their complex viscosity. Normal force measurements were carried out for the six packable materials to determine the unplugging force and unplugging work (stickiness) over the same temperature range. Data were analyzed using Kolmogorov–Smirnoff test, one-way ANOVA and Tukey Post Hoc test with α = 0.05 as level of significance.ResultsAt 23 °C packable composites showed viscosity between 6.75 and 19.14 kPa s, while flowable composites presented significantly lower viscosities between 1.31 and 2.20 kPa s. Pre-heating led to a drop of 30–82% in the viscosity of packable materials. The thermo-viscous material dropped to the level of flowables at 45 and 54 °C thus behaving as a packable composite at room temperature with flowable-like viscosity at higher temperatures. No statistically significant differences for viscosity were observed among flowable composites at any temperature.The unplugging force decreased for packable composites, while their unplugging work generally increased at elevated temperature. At 23 °C unplugging force was measured between 7.50 and 19.18 N, while pre-heating up to 54 °C led to values between 2.9 and 6.2 N. Regarding unplugging work at 23 °C the calculated values were between 3.0 and 8.9 × 10^?3 J and at 54 °C between 8.8 and 13.0 × 10^?3 J.SignificancePre-heating significantly reduced viscosity of highly viscous resin composites, while no influence was shown for flowable composites. In general stickiness, measured as unplugging work, increased at elevated temperatures. The thermo-viscous material showed low viscosity comparable to flowable composites at 45 and 54 °C, yet its stickiness did not increase significantly compared to the values at 23 °C.     

Mathematical model for assessing true irradiance received by luting materials while curing through modern CAD/CAM resin composites

Statement of problemMeasurement of irradiance passing through a dental restoration for properly curing a dual- or light-polymerized luting composite is imprecise due to surface reflection.ObjectiveTo provide a mathematical correction of measured transmitted irradiance for predicting true transmitted light intensity through CAD/CAM restorations.MethodsA total of 432 specimens were fabricated. Seven modern CAD/CAM resin-based composites (RBCs) and one CAD/CAM glass-ceramic (control group) were sectioned and polished into specimens of 0.5–5 mm thickness (in 0.5 mm steps, n = 6). Irradiance of a violet-blue LED light curing unit (LCU) (power modes: Standard, High and Plasma) was measured after passing through each specimen with a spectrometer. Data was compared based on 95% confidence intervals and using univariate ANOVA followed by Tukey HSD (α = 0.05).ResultsThe measured transmitted irradiance passing through the specimens decreased exponentially. Significantly highest values of transmitted irradiance were measured for 0.5 mm thick specimens for all materials (p < 0.05). The decadic absorption coefficient for CAD/CAM-RBCs ranged from 0.292 mm⁻¹ to 0.387 mm⁻¹ while the control group (glass-ceramic) reached a significantly lower value of 0.283 mm⁻¹. The reflection ratio for all materials ranged from 12.6% to 18.5%.SignificanceA correction can be implemented to predict the true transmitted irradiance after passing through a dental restoration as function of initial irradiance, specimen thickness and material specific parameters. For a practitioner, this model may be applied depending on the specific treatment conditions, the individual LCU's radiant emittance and restoration thickness for the tested materials.     

Flowability of composites is no guarantee for contraction stress reduction

ObjectivesThe purpose of this study was to measure the contraction stress development of three flowable resin-composite materials (Grandio Flow, VOCO GmbH, Cuxhaven, Germany; Tetric Flow, Ivoclar Vivadent, Schaan, Liechtenstein; Filtek Supreme XT Flowable Restorative, 3 M ESPE, ST. Paul, MN, USA) and an universal micro-hybrid composite resin (Filtek Z250, 3 M ESPE, St. Paul, MN, USA) during photopolymerization with a halogen curing light, using a novel stress-measuring gauge.MethodsCuring shrinkage stress was measured using a stress-analyzer. Composites were polymerized with a halogen curing unit (VIP, Bisco Inc., Schaumburg, IL, USA) for 40 s. The contraction force (N) generated during polymerization was continuously recorded for 180 s after photo-initiation. Contraction stress (MPa) was calculated at 20 s, 40 s, 60 s, 120 s and 180 s. Data were statistically analyzed.ResultsFiltek Supreme XT Flowable Restorative exhibited the highest stress values compared to other materials (p < 0.05), while the lowest values were recorded with Tetric Flow (p < 0.05). Tetric Flow was also the only flowable composite showing stress values lower than the conventional composite Filtek Z250 (p < 0.05).SignificanceFlowable composites investigated with this experimental setup showed shrinkage stress comparable to conventional resin restorative materials, thus supporting the hypothesis that the use of flowable materials do not lead to marked stress reduction and the risk of debonding at the adhesive interface as a result of polymerization contraction is similar for both type of materials.     

Effects of monomer ratios and highly radiopaque fillers on degree of conversion and shrinkage-strain of dental resin composites

ObjectivesThe degree of conversion (DC) and polymerization shrinkage of resin composites are closely related manifestations of the same process. Ideal dental composite would show an optimal degree of conversion and minimal polymerization shrinkage. These seem to be antagonistic goals, as an increase in monomer conversion leads to a high polymerization shrinkage. This paper aims to determine the effect of opaque mineral fillers and monomer ratios on the DC and the shrinkage-strain of experimental composites based on (BisGMA/TEGDMA) monomers (traditionally used monomers). A relationship between the shrinkage-strain and the degree of conversion values was also investigated. The radiopacity of these experimental composites has been investigated in a previous paper.MethodsExperimental resin composites were prepared by mixing different monomer ratios of (BisGMA/TEGDMA) with Camphoroquinone and dimethyl aminoethyl methacrylate (DMAEMA) as photo-initiator system. Five different radiopacifying filler agents: La₂O₃, BaO, BaSO₄, SrO and ZrO₂ at various volume fractions ranging from 0 to 80 wt.% were added to the mixture. The degree of conversion of experimental composites containing different opaque fillers contents was measured using FTIR/ATR spectroscopy. The shrinkage-strain of specimens, photopolymerized at circa 500 mW/cm², was measured using the bonded-disk technique at room temperature with respect to time.ResultsThe result revealed that the DC and the shrinkage-strain decrease slightly with the increasing of opaque fillers loadings, but this decrease is not significant. However, these two properties are closely related to the monomer concentration of the organic matrix. The results have also showed a linear correlation between the shrinkage-strain and DC of experimental composites investigated.SignificanceThe nature and the volume effects of the opaque fillers on the DC and shrinkage of the experimental composites investigated were not significant. However, this study has confirmed the importance of viscosity in the system and shrinkage behavior of dimethacrylate monomers studied. Then we confirmed that direct relationships linked the shrinkage and the DC of filled dental resin composites.     

Adhesion procedures for CAD/CAM indirect resin composite block: A new resin primer versus a conventional silanizing agent

PurposeThe purpose of this study was to evaluate the effectiveness of both a resin primer containing methyl methacrylate (MMA) and a silanizing agent on bonding to indirect resin composite blocks, using two types of build-up hybrid resin composites.MethodsSHOFU BLOCK HC (Shofu) specimens were blasted with alumina, after which one of two surface treatments was applied: CERA RESIN BOND (Shofu, the Silane group) or HC primer (Shofu, the MMA group). Resin composites made using either Solidex Hardura (SDH, Shofu) or Ceramage Duo (CMD, Shofu) were built up and micro-tensile bond strength (μTBS) values were measured after storage in water for either 24 h or 6 months (n = 24 per group). The fracture surfaces after μTBS measurements and the resin block/build-up resin interfaces were observed by scanning electron microscopy (SEM).ResultsThe bond strength of the Silane/SDH group significantly decreased after 6 months (p < 0.001), whereas in the MMA group there was no significant loss after 24 h or 6 months (p = 0.99). In the CMD group, the bond strength after 6 months was significantly lowered in both the Silane group (p < 0.001) and the MMA group (p < 0.001), but the latter still showed greater adhesion. SEM images demonstrated that the matrix resin was partially destroyed at the fracture surfaces of the MMA group and fracture surface unevenness was observed.ConclusionsA primer containing MMA produced stronger bonding to CAD/CAM resin even after long-term aging compared to a silane treatment.     

Reinforcement of experimental composite materials based on amorphous calcium phosphate with inert fillers

ObjectivesThe aim of this study was to examine the influence of the addition of glass fillers with different sizes and degrees of silanization percentages to remineralizing composite materials based on amorphous calcium phosphate (ACP).MethodsFour different materials were tested in this study. Three ACP based materials: 0-ACP (40 wt% ACP, 60 wt% resin), Ba-ACP (40 wt% ACP, 50 wt% resin, 10 wt% barium-glass) and Sr-ACP (40 wt% ACP, 50 wt% resin, 10 wt% strontium-glass) were compared to the control material, resin modified glass ionomer (Fuji II LC capsule, GC, Japan). The fillers and composites were characterized using scanning electron microscopy. Flexural strength and modulus were determined using a three-point bending test. Calcium and phosphate ion release from ACP based composites was measured using inductively coupled plasma atomic emission spectroscopy.ResultsThe addition of barium-glass fillers (35.4 (29.1–42.1) MPa) (median (25–75%)) had improved the flexural strength in comparison to the 0-ACP (24.8 (20.8–36.9) MPa) and glass ionomer control (33.1 (29.7–36.2) MPa). The admixture of strontium-glass (20.3 (19.5–22.2) MPa) did not have any effect on flexural strength, but significantly improved its flexural modulus (6.4 (4.8–6.9) GPa) in comparison to 0-ACP (3.9 (3.4–4.1) GPa) and Ba-ACP (4.6 (4.2–6.9) GPa). Ion release kinetics was not affected by the addition of inert fillers to the ACP composites.SignificanceIncorporation of barium-glass fillers to the composition of ACP composites contributed to the improvement of flexural strength and modulus, with no adverse influence on ion release profiles.     

Composite resin reinforced with fluorescent europium-doped hydroxyapatite nanowires for in-situ characterization

ObjectiveThe object is to find an easy but efficient way to illustrate the in-situ dispersion of nano-scaled one-dimensional fillers in composite resins, and to correlate their dispersion status with the properties of composite resins.MethodsFluorescent europium-doped hydroxyapatite nanowires (HANW:Eu) were synthesized via the hydrothermal method. The HANW:Eu was mixed into Bis-GMA/TEGDMA (60/40, w/w) at different contents (1–5 wt.%), and different processing methods (kneading, grinding, stirring) were tested to achieve good dispersion of HANW:Eu with the aid of fluorescent imaging system. Then, the mixtures of HANW:Eu and barium glass powder (BaGP) were kneaded into resin at a fixed content (70 wt.%) while at different mixing ratios. In addition to the 3D fluorescent imaging, characterizations were carried out on mechanical properties, fractured surface, wear resistance and polymerization shrinkage, to correlate the composite properties of with the dispersion status of the incorporated HANW:Eu.ResultsBy doping calcium with 5 mol.% of europium, the obtained HANW:Eu displayed strong fluorescence, which made the illustration of its in-situ dispersion status within composites being possible. And this helped to judge that kneading was more efficient to homogeneously disperse HANW:Eu than grinding and stirring. However, it was illustrated vividly that HANW:Eu aggregated severely when it was co-incorporated with BaGP into composites at the total content of 70 wt.%, which had not been previously revealed by other microscope observations. In comparison with composites containing 70 wt.% of BaGP, improvements in the mechanical properties of resulting composites were identified for the cases containing 3 wt.% of HANW and 67 wt.% of BaGP, however, their wear volume loss and the polymerization shrinkage did not decrease as expected due to the HANW aggregations.SignificanceThe fluorescent filler prepared in this study provides a feasible strategy to illustrate the in-situ dispersion status of inorganic fillers, which provides guidance for the processing of composite resins.