Thermal shrinkage reveals the feasibility of pulse-delay photocuring technique

ObjectivesTo resolve the feasibility of the pulse-delay photocuring technique as a clinical strategy for reducing the detrimental polymerization stress induced in dental composites during the photocuring process.MethodsModel dental composites with high and low-filler contents were cured with the pulse-delay photocuring technique using different combinations of photocuring variables (irradiance, exposure time, and delay time). Irradiance used ranged from 0.1 W/cm² to 4 W/cm². The exposure time of the first pulse varied from 0.2 s to 27.2 s and the delay times ranged from 10 s to 120 s. The radiant exposure was varied from 4 J/cm² to 20 J/cm². A cantilever-beam based instrument (NIST Standards Reference Instrument 6005) was used to implement the photocuring technique for the measurement of the polymerization properties (the degree of monomer conversion, polymerization stress induced due to shrinkage, and temperature change due to the reaction exotherm and curing light absorbance) simultaneously in real-time. These properties were compared with those obtained using the conventional photocuring technique (i.e., using a constant irradiance for a fixed exposure time, a uniform exposure).ResultsThere exists a minimum radiant exposure, such that a reduction in the polymerization stress can be achieved without sacrificing the degree of monomer conversion by using the pulse-delay over the conventional photocuring technique. More specifically, stress reductions of up to 19% and 32% was observed with the pulse-delay when compared with the conventional photocuring technique at an irradiance of 0.5 W/cm² and 4 W/cm², respectively. The reduction occurred when the exposure time of the first pulse was greater than, but closer to, the gelation time (i.e., lower than the vitrification time) of the composite, regardless of the delay time used. Lower thermal shrinkage (contraction) during the post-curing time, rather than the stress relaxation during the delay time or lower degree of monomer conversion as claimed in the literature, is the cause of the reduction in the polymerization stress.SignificanceThe study clarifies a long-standing confusion and controversy on the applicability of the pulse-delay photocuring technique for reducing the polymerization stress and promotes its potential clinical success for dental restorative composites.     

Bis(4-methyl phenyl)iodonium as an alternative component to diphenyliodonium in camphorquinone-based ternary initiating systems

ObjectiveTo evaluate the influence of different co-initiators (diphenyliodonium hexafluorophosphate - DPI - and bis(4-methyl phenyl)iodonium hexafluorophosphate – BPI) on chemical and mechanical properties of resins.MethodsNine experimental resins (50% Bis-GMA and 50% TEGDMA, w/w) with 60 wt% filler particles were formulated. The initiating system used was camphorquinone (CQ-1 mol%) and ethyl dimethylaminobenzoate (EDAB-2 mol%). Experimental groups were established according to DPI and BPI quantities (0.25, 0.5, 0.75, and 1 mol%). The control group was a resin containing only CQ-EDAB. Light transmission through the resin during polymerisation was analysed with a UV–vis spectrophotometer. Real-time polymerisation of the systems was evaluated using an FTIR spectrometer. Real-time polymerisation shrinkage strain was evaluated, and the flexural strength and modulus of materials were obtained by 3-point bending. Experimental groups were statistically analysed by Analysis of Variance and Tukey’s test (α = 0.05). Dunnett’s test was applied to compare experimental groups with control.ResultsLight transmission rapidly increased initially for resins containing DPI or BPI. After 30 s cure, the irradiance on the lower surface of resin specimens was similar for all groups. After 10 s of light irradiation, groups containing DPI and BPI had higher conversion than the control. However, conversion after 120 s post-irradiation was similar for all groups. The rate of polymerisation, shrinkage strain, and the maximum strain rate were higher for groups containing DPI/BPI. The use of iodonium salts increased the flexural strength and flexural moduli of resins.SignificanceDPI and BPI increased resin reactivity similarly. Increased rate of polymerization influenced light transmission through the resin in the first seconds of polymerisation and increased resin shrinkage and rate of shrinkage, as well as flexural strength and moduli.     

Mechanical properties of new self-adhesive resin-based cement

PurposeThe aim of this study was to compare the bonding strength, flexural strength, elastic modulus, water absorption and the expansion after water storage of new self-adhesive resin cements to commercially available dental cements.MethodsTwo types (hand-mix and auto-mix) of new self-adhesive resin cements (SAC-H and SAC-A, Kuraray Medical), one conventional resin cement (Panavia F2.0), three self-adhesive resin cements (Relyx Unicem, Maxcem and G-Cem), and two resin-modified glass-ionomer cements (Fuji Luting S and Vitremer) were used. Shear bond strengths, flexural strengths and elastic moduli (ISO 4049), water absorption (ISO 4049), and the expansion rate after water storage were investigated.ResultsBoth SAC-H and SAC-A provided adhesion to enamel and dentin, and had the same bond strength to gold alloy and zirconia as conventional resin cements. SAC-H and SAC-A had greater flexural strengths (86.4–93.5 MPa) than commercial self-adhesive resin cements or glass-ionomer cements. The elastic moduli of self-adhesive and glass-ionomer cements were 5.2–7.4 GPa and 2.3–3.4 GPa, respectively. The water absorption of SAC-H and SAC-A (26.3–27.7 μg/mm³) were significantly lower than commercial self-adhesive resin cements. SAC-H and SAC-A showed significantly lower expansion rates (0.17–0.26%) than commercial self-adhesive cements and glass-ionomer cements after 4 weeks water storage.ConclusionsIt is suggested that the new self-adhesive resin cements exhibited a favorable bonding capability and mechanical properties.     

Resin viscosity determines the condition for a valid exposure reciprocity law in dental composites

ObjectiveTo provide conditions for the validity of the exposure reciprocity law as it pertains to the photopolymerization of dimethacrylate-based dental composites.MethodsComposites made from different mass ratios of resin blends (Bis-GMA/TEGDMA and UDMA/TEGDMA) and silanized micro-sized glass fillers were used. All the composites used camphorquinone and ethyl 4-dimethylaminobenzoate as the photo initiator system. A cantilever beam-based instrument (NIST SRI 6005) coupled with NIR spectroscopy and a microprobe thermocouple was used to simultaneously measure the degree of conversion (DC), the polymerization stress (PS) due to the shrinkage, and the temperature change (TC) in real time during the photocuring process. The instrument has an integrated LED light curing unit providing irradiances ranging from 0.01 W/cm² to 4 W/cm² at a peak wavelength of 460 nm (blue light). Vickers hardness of the composites was also measured.ResultsFor every dental composite there exists a minimum radiant exposure required for an adequate polymerization (i.e., insignificant increase in polymerization with any further increase in the radiant exposure). This minimum predominantly depends on the resin viscosity of composite and can be predicted using an empirical equation established based on the test results. If the radiant exposure is above this minimum, the exposure reciprocity law is valid with respect to DC for high-fill composites (filler contents >50% by mass) while invalid for low-fill composites (that are clinically irrelevant).SignificanceThe study promotes better understanding on the applicability of the exposure reciprocity law for dental composites. It also provides a guidance for altering the radiant exposure, with the clinically available curing light unit, needed to adequately cure the dental composite in question.     

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.     

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.     

Limited reciprocity in curing efficiency of bulk-fill resin-composites

ObjectiveThe aim of the study was to identify experimental limits of the general reciprocity hypothesis that the same photo-cure outcomes will result from applying essentially constant energy densities, despite reciprocal variations in the irradiance and irradiation time-period, for a representative set of bulk fill (BF) and non-BF resin composites.MethodsSix BF and two non-BF resin-composites were selected. The unset pastes were inserted into white acetal molds (5 mm id) with (n = 6) depths (1, 2, 3, 4, 5 and 6 mm). Three light curing units (LCUs) of increasing radiant emittance capability: 1200, 2000 and 3200 mW/cm² were used. Composite specimen groups (n = 3, per depth, per LCU) were irradiated on the upper surface only. For each specific composite, the irradiation times for each LCU were reduced reciprocally, as the LCU irradiance increased, to deliver a constant energy density (J/cm²) to that composite. However, the required energy density for a given composite differed in accordance with each composite manufacturer recommendations. After storing for 24 h at 37 °C, light transmission measurements were made through each specimen and re-expressed as Apparent Absorbance (A′). Vickers hardness (H_V) measurements (n = 10) were made on both top and bottom surfaces, for each specimen, and H_V versus “depth” profile plots created. From the top-surface data, a Depth-of-Cure parameter could be derived. Data were statistically evaluated for differences between top and bottom H_V values and for other predefined variables of interest.ResultsIrradiation with the LCU of 1200 mW/cm² generally gave the highest H_V/depth for most materials tested compared to the other curing lights with higher power output, regardless of top and bottom measurements (p < 0.001). However, this difference was material-dependent. With one BF composite, 1200 and 2000 mW/cm² irradiance did not show a significant difference between top and bottom H_V. Composites with higher translucency showed reduced differences in top/bottom H_V than more opaque composites.SignificanceReciprocity was found to be limited with most materials examined, such that irradiance periods of 10 s, gave generally better H_V outcomes than by using LCUs of superior radiant emittance while reciprocally reducing irradiance time to maintain constant dose of energy density.     

Microhardness of resin cements in the intraradicular environment: Effects of water storage and softening treament

ObjectivesTo analyze the microhardness of four dual-cure resin cements used for cementing fiber-reinforced posts under the following conditions: after 7 days of storage in water, after additional 24 h of immersion in 75% ethanol, and after 3 months of storage in water. Hardness measurements were taken at the cervical, middle and apical thirds along the cement line.MethodsRoot canals of 40 bovine incisors were prepared for post space. Fibrekor^® glass fiber-reinforced posts (Jeneric/Pentron) of 1 mm in diameter were cemented using Panavia F 2.0 (Kuraray), Variolink (Ivoclar-Vivadent), Rely X Unicem (3M ESPE) or Duolink (Bisco) (N = 10). After 7 days of water storage at 37 °C, half the sample (N = 5) was longitudinally sectioned and the initial microhardness measured along the cement line from cervical to apex. These same samples were further immersed in 75% ethanol for 24 h and reassessed. The remaining half (N = 5) was kept unsectioned in deionized water at 37 °C for 3 months, followed by sectioning and measuring. Data were analyzed by a series of two-way ANOVA and Tukey tests at α = 5%.ResultsStatistically significant differences were identified among the cements, thirds and conditions. Significant interactions were also observed between cements and thirds and between cements and conditions. Panavia F exhibited significantly higher initial microhardness than the other three cements, which showed no statistical difference among themselves. Variolink and Duolink showed significantly higher microhardness values in the cervical third, without significant difference among the thirds for the other cements. Immersion in ethanol significantly reduced the hardness values for all cements, regardless of the thirds. Storage in water for 3 months had no influence on the hardness of most of the cements, with the exception of Unicem that showed a significant increase in the hardness values after this period.SignificanceResults showed heterogeneity in the microhardness of the cements inside the canal. All cements presented some degree of softening after ethanol treatment, which suggests instability of the polymer. The quality of curing of resin cements in the root canal environment seems unpredictable and highly material dependent.     

Curing efficiency of four self-etching,self-adhesive resin cements

ObjectivesTo evaluate the degree of cure (%DC) of four self-etching, self-adhesive resin cements, and one conventional resin cement, in their self- and dual-curing mode.MethodsThe self-etching, self-adhesive resin cements studied were RelyX? Unicem (3M? ESPE? AG), Maxcem? (Kerr Corporation), Biscem? (Bisco, Inc.) and Multilink^® Sprint (Ivoclar Vivadent^® AG) and the classic resin cement was Multilink^® Automix (Ivoclar Vivadent^® AG). Twelve specimens of each material (1.8 mm × 4 mm × 4 mm) were prepared in room temperature (23 ± 1) °C following the manufacturers’ instructions. Six of them were treated as dual-cured, thus irradiated for 20 s with a halogen light curing unit and left undisturbed for 5 min. The other six were treated as self-cured and were not irradiated, but left in dark and dry conditions for 10 min. The assessment of the %DC was made using micro-ATR FTIR spectrometry.ResultsThe %DC in their self-curing mode was very low (10.82–24.93%), with Multilink Sprint exhibiting the highest values among the five. In the dual-curing mode the values obtained were also low (26.40–41.52%), with the exception of Multilink Automix (61.36%). Maxcem was found to have the lowest DC.SignificanceThe low %DC found raises questions as to whether these materials can be successfully used in clinical applications, where light attenuation takes place. Increased irradiation times could potentially lead to higher %DC, in applications where light is not completely blocked by the overlying restoration.     

A comparison of stress relaxation in temporary and permanent luting cements

PurposeThe stress relaxation and compressive strength of resin, resin-modified glass ionomer, glass ionomer, polycarboxylate, and zinc oxide eugenol cements were measured to determine the characteristics of these materials after setting.MethodsA total of 19 luting cements including 12 permanent cements and 7 temporary cements were used. Cylindrical cement specimens (10 mm long and 6 mm in diameter) were obtained by chemical setting or light curing. The specimens were stored for 24–36 h in water at 37 °C and were then used for the stress relaxation and compression tests. The stress relaxation test was carried out using three constant cross-head speeds of 5, 50, and 100 mm/min. Upon reaching the preset dislocation of 0.5 mm, the cross-head movement was stopped, and the load was recorded for 60 s. Fractional stress loss at 1 s was calculated from the relaxation curves. The compressive strength and modulus were measured at a cross-head speed of 1 mm/min. Data were analyzed with the Kruskal–Wallis test and Holm's test.ResultsA zinc oxide eugenol cement [TempBOND NX] exhibited the largest fractional stress loss. A resin cement [ResiCem] showed the largest compressive strength, while a glass ionomer cement [HY-BOND GLASIONOMER CX] showed the largest compressive modulus among all tested cements (p < 0.05).ConclusionThe fractional stress loss could not be classified by the cement type. Two implant cements [Multilink Implant and IP Temp Cement] showed similar properties with permanent resin cements and temporary glass ionomer cements, respectively. Careful consideration of the choice of cement is necessary.     

Determination of the optimal photoinitiator concentration in dental composites based on essential material properties

ObjectivesThe aim of this study was to determine the concentrations of the photosensitizer (camphoroquinone, CQ) and coinitiator (ethyl-4-dimethylaminobenzoate, EDMAB) that resulted in maximum conversion but generated minimum contraction stress in experimental composites.MethodsExperimental composites were prepared with an identical resin formulation [TEGDMA:UDMA:bis-GMA of 30.25:33.65:33.65]. Five groups of resin were prepared at varied CQ concentrations (0.1, 0.2, 0.4, 0.8 and 1.6 wt% of the resin). Five subgroups of resin were prepared at each level of CQ concentration, by adding EDMAB at 0.05, 0.1, 0.2, 0.4 and 0.8 wt% of the resin, resulting in 25 experimental resins. Finally, strontium glass (～3 μm) and silica (0.04 μm) were added at 71.5 and 12.6 wt% of the composite, respectively. Samples (n = 3) were then evaluated for Knoop hardness (KHN), degree of conversion (DC), depth of cure (DoC) and contraction stress (CS).ResultsThere was an optimal CQ and EDMAB concentration that resulted in maximum DC and KHN, beyond which increased concentration resulted in a decline in those properties. KHN testing identified two regions of maxima with best overlaps occurring at CQ:EDMAB ratio of 1.44:0.42 and 1.05:1.65 mol%. DC evaluation showed one region of maximum, the best overlap occurring at CQ:EDMAB ratio of 2.40:0.83 mol%. DoC was 4 mm. Overall, maximum CS was attained before the system reached the maximum possible conversion and hardness.Significance(1) Selection of optimal photoinitiator/amine concentration is critical to materials’ formulation, for excessive amounts can compromise materials’ properties. (2) There was no sufficient evidence to suggest that contraction stress can be reduced by lowering CQ/EDMAB concentration without compromising DC and KHN.     

Evaluation of light-curing units in rural and urban areas

ObjectivesTo evaluate the distribution of light-curing units (LCU) used in an urban area (Riyadh) and a rural area (Kharj) of Saudi Arabia, and to compare their irradiance values.MethodsThe study involved three dental centers in urban areas and two in rural areas, all of which were parts of a single healthcare institution providing dental services. The light outputs (power mW) from 140 LCUs were measured by laboratory-grade spectrometry, and the irradiance (mW/cm²) was calculated from the tip area of each LCU. The minimum acceptable irradiance outputs for the quartz-tungsten-halogen (QTH) and light-emitting diode (LED) units were set at 300 and 600 mW/cm², respectively. The ages of these units and the protocol used to light-cure the resins were also determined.ResultsThe total number of LCUs was 140, 112 (78%) in urban areas, and 28 (22%) in rural areas. In rural areas, only 7 of the 22 (32%) QTH units delivered irradiances greater than 300 mW/cm² and were therefore considered clinically acceptable, whereas 4 of the 6 (66.7%) LED units delivered values greater than 600 mW/cm². In urban centers, 43 of 61 (70.5%) LED units and 25 of 61 (49%) QTH units were considered clinically acceptable. Irradiance values for both QTH (P < 0.01) and LED (P < 0.05) units were significantly better in urban than in rural areas.ConclusionsUrban areas had a greater distribution of LCUs than rural areas. Overall, irradiance values were significantly higher in urban areas.     

Initial fracture resistance and curing temperature rise of ten contemporary resin-based composites with increasing radiant exposure

ObjectivesThe principal objective of this study was to determine whether the bulk fracture resistance of ten light activated composites varied over a clinically realistic range of radiant exposures between 5 and 40 J/cm².MethodsTen operators were tested for clinically simulated radiant exposure delivery from a Bluephase^® (Ivoclar Vivadent, Schaan, Liechtenstein) LED light to an occlusal cavity floor in tooth 27 in a mannequin head using a MARC^®-Patient Simulator (Bluelight Analytics Inc., Halifax, NS) device. Notch disc test samples were prepared to determine the torque resistance to fracture (T) of the composites. Samples were irradiated with the same monowave Bluephase^® light for 10 s, 20 s or 40 s at distances of 0 mm or 7 mm. After 24 h, storage samples were fractured in a universal testing machine and torque to failure was derived.ResultsRadiant exposure delivered in the clinical simulation ranged from 14.3% to 69.4% of maximum mean radiant exposure deliverable at 0 mm in a MARC^®-Resin Calibrator (Bluelight Analytics Inc., Halifax, NS) test device. Mean torque to failure increased significantly (P < 0.05) with radiant exposure for 8 out of 10 products. The micro-fine hybrid composite Gradia Direct anterior (GC) had the lowest mean (S.D.) T between 10.3 (1.8) N/mm and 13.7 (2.2) N/mm over the tested radiant exposure range. Three heavily filled materials Majesty Posterior, Clearfil APX and Clearfil Photo-Posterior (Kuraray) had mean T values in excess of 25 N/mm following 40 J/cm² radiant exposure. Mean T for Z100 (3MESPE) and Esthet-X (Dentsply) increased by 10% and 91% respectively over the tested range of radiant exposures.ConclusionsIndividual products require different levels of radiant exposure to optimize their fracture resistance. Light activated composites vary in the rate at which they attain optimal fracture resistance.Clinical significanceUnless the clinician accurately controls all the variables associated with energy delivery, there is no way of predicting that acceptable fracture resistance will be achieved intra-orally.     

Effect of proanthocyanidins and photo-initiators on photo-polymerization of a dental adhesive

ObjectivesTo evaluate the effects of proanthocyanidins (PA) and photoinitiator type on the degree of conversion (DC) and polymerization rate (PR) of a model dental adhesive.MethodsThree types of photo-initiation systems were introduced into the Bis-GMA/HEMA co-monomer mixture, resulting in four resin formulations including CQ/A (0.5 wt% CQ and EDMAB), CQ/A/I-1 (0.5 wt% CQ, EDMAB and DPIHP), CQ/A/I-2 (1.0 wt% CQ, EDMAB and DPIHP), and TPO (2.1 wt% TPO). For each resin formulation, adhesives containing 0%, 2.5%, 5% and 10% of PA with respect to the weight of resin were produced after mixing the resin with various amount of PA/ethanol solution. When light-cured, the RP and DC of each adhesive was determined using ATR-FTIR spectroscopy.ResultsAcross and within the initiator groups, the DC followed the general trend of CQ/A < CQ/A/I-1 < CQ/A/I-2 < TPO and 0-PA > 2.5-PA > 5-PA > 10-PA, respectively. The change of PR with respect to photo-initiation systems and PA content was in a similar but less pronounced pattern.ConclusionPA hampered the polymerization of all adhesives regardless of photoinitiators used. The initiator formulations CQ/A/I-2 and TPO are better fit for PA-containing adhesives, both leading to >65% DC in the presence of 5% PA.Clinical significanceThe inclusion of PA in dental adhesives has been limited by its interference with the light-curing of adhesive resins. This study found photo-initiation formulations that could maintain a satisfactory degree of monomer conversion while a significant amount of PA is incorporated.     

Effect of pulpal pressure on the microtensile bond strength of luting resin cements to human dentin

ObjectivesThe objectives of this study were to examine the effect of pulpal pressure on the microtensile bond strength (mTBS) of luting resin cements to human dentin and the permeability of dentin surfaces pre-treated with an adhesive and a self-etching primer.MethodsCylindrical composite blocks were luted with resin cements (RelyX ARC, 3M ESPE: ARC; Panavia F, Kuraray Medical Inc.: PF; RelyX Unicem, 3M ESPE: UN) in the absence or presence of simulated pulpal pressure. The application of Adper Single Bond 2 (3M ESPE) and ED primer 2.0 (Kuraray) was performed under 0 cm H₂O. After each resin cement was applied, the pulpal pressure group was subjected to 20 cm H₂O of hydrostatic pressure for 10 min during the initial setting period. Testing for mTBS was performed on 0.9 mm × 0.9 mm sectioned beams after 24 h water-storage. Scanning electron microscopy was performed to investigate the fractured surfaces after mTBS testing and additional dentin surfaces that were treated by an etchant, ED primer 2.0 and UN. Fluid permeability was measured on dentin surfaces that were applied with Adper Single Bond 2 and ED primer 2.0.ResultsApplication of pulpal pressure reduced mTBS significantly in groups ARC and PF. Porous bonding interfaces due to water permeability through the cured adhesive were observed on fractured surfaces. Dentin surfaces that were applied with the adhesive and the primer were more permeable than smear layer-covered dentin. The mTBS of UN was significantly lower than ARC and PF regardless of the absence/presence of pulpal pressure.SignificanceFluid permeation during the initial setting period deteriorated the bonding quality of resin cements.     

Effects of residual ethanol on the rate and degree of conversion of five experimental resins

ObjectivesThis study examined the extent of ethanol retention in five comonomer blends of experimental methacrylate-based dental adhesives, containing (10, 20, or 30 wt.%) ethanol, after solvent evaporation, as well as observing the effect of residual ethanol and exposure duration on degree of conversion (DC). The null hypothesis that was tested was that residual, unevaporated ethanol has no effect on the rate or extent of DC of polymerized adhesive resins.MethodsA known mass of each mixture was placed in glass wells and evaporated for 60 s. The mass of the mixtures before and after evaporation was measured, allowing calculation of the gravimetric ethanol loss/retention.ResultsThe concentration of retained ethanol increased significantly with ethanol concentration (p < 0.01): 1.1–1.9 mole/L for 10% ethanol/90% comonomers, 2.2–3.5  mole/L for 20% ethanol, and 2.6–3.7 mole/L for 30% ethanol/70% comonomers. As ethanol is evaporated from solvated comonomer mixtures, the molar concentration of comonomers increases, reducing the vapor pressure of the remaining ethanol. Thus, the fractional loss of ethanol solvent decreases as the comonomer concentration increases. The DC of 10, 20, and 30 wt.% ethanol blends increased with ethanol concentration in four of the five experimental resins (p < 0.05), increasing by 30–45% when 10 or 20 wt.% ethanol was added to neat resins, regardless of exposure duration. Depending on the resin system, inclusion of 30% ethanol lowered DC at 20 s but increased DC after 40–60 s of light exposure.SignificanceSince 10 and 20 wt.% ethanol–resin blends increased the DC of solvated resins by 30–45% over neat resins, the test null hypothesis is rejected. Even with prolonged evaporation, 4–9% residual ethanol concentration can remain in 90/10 (wt./wt.) comonomer–ethanol mixtures. This is thought to be because comonomers lower the vapor pressure of ethanol. This amount of residual ethanol facilitates DC but lowers the rate of polymerization.     

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.     

Influence of composition on setting kinetics of new injectable and/or fast setting tricalcium silicate cements

ObjectivesNew commercial tricalcium silicate based cements were elaborated to improve handling properties and setting time. The goals of the present work were: (i) to determine the composition of the new injectable and/or fast setting calcium silicate based cements, and (ii) to investigate the impact of the differences in composition on their setting kinetics.MethodsThe materials considered were Angelus MTA™, Biodentine™, MM-MTA™, MTA-Caps™, and ProRoot MTA™ as control.Elemental composition of materials was studied by Inductively Coupled Plasma-Atomic Emission Spectroscopy and X-ray Energy Dispersive analysis, whereas phases in presence were analyzed by Micro-Raman spectroscopy and X-ray Diffraction analysis and cement surface by Scanning Electron Microscope. Setting kinetics was evaluated using rheometry.ResultsElemental analysis revealed, for all cements, the presence of three major components: calcium, silicon and oxygen. Chlorine was detected in MM-MTA, MTA-Caps and Biodentine. Different radio-opacifiers were identified: bismuth oxide in ProRoot MTA, Angelus MTA and MM-MTA, zirconium oxide in Biodentine and calcium tungstate (CaWO₄) in MTA-Caps. All cements were composed of di- and tri-calcium silicate, except Biodentine for which only the latter was detected. Major differences in setting kinetics were observed: a modulus of 8 × 10⁸ Pa is reached after 12 min for Biodentine, 150 min for MM-MTA, 230 min for Angelus MTA and 320 min for ProRoot MTA. The maximum modulus reached by MTA-Caps was 7 × 10⁸ Pa after 150 min.SignificanceEven if these cements possess some common compounds, major differences in their composition were observed between them, which directly influence their setting kinetics.     

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.     

Cytotoxicity of polymerized resin cements on human dental pulp cells in vitro

ObjectivesThis study was designed to evaluate the cytotoxicity of several resin-based cements (Panavia F, Super-Bond C&B, Chemiace II) after polymerization on cultured human dental pulp cells.MethodsAfter polymerization, specimens from three resin-based cements were eluted with fresh Dulbecco's modified Eagle's medium (DMEM) without serum for 72 h, at 37 °C, using 0.4 g of each substance per milliliter of fresh medium. Elutes obtained during this step were passed through a 0.22-μm filter and diluted with the culture medium by a ratio of 75%, 50%, 25% (v/v). Cytotoxicity of elutes were evaluated by the relative growth rates (RGR) of pulp cells with a modified 3-(4, 5-dimethyl-thiazol-2-yl)-2, 5-diphenyl-tetrazolium bromide (MTT) assay. The RGR of pulp cells were statistic analyzed by the one-way analysis of variance among the groups.ResultsThe RGR of cells exposed to 100% concentration of elution of Panavia F, Super-Bond C&B, and Chemiace II were 74.42%, 85.54%, and 82.39%, respectively. The RGR increased along with the elution of cements diluted. There was significant difference between the Panavia F group and Super-Bond C&B group (p < 0.01), but there was no significant difference in the cytotoxicity between Chemiace II and Super-Bond C&B.ConclusionsAfter polymerization, three resin-based cements (Panavia F, Super-Bond C&B, Chemiace II) induced slight cytotoxicity. The sensitivity of cytotoxicity to human pulp cells depended on the resin-based cements and the concentration of the elution. Super-Bond C&B is the least cytotoxic agent among the three resin-based cements.