Polymerization stress, shrinkage and elastic modulus of current low-shrinkage restorative composites

Objective. To compare currently available low-shrinkage composites with others regarding polymerization stress, volumetric shrinkage (total and post-gel), shrinkage rate and elastic modulus. Methods. Seven BisGMA-based composites (Durafill/DU, Filtek Z250/FZ, Heliomolar/HM, Aelite LS Posterior/AP, Point 4/P4, Filtek Supreme/SU, ELS/EL), a silorane-based (Filtek LS, LS), a urethane-based (Venus Diamond, VD) and one based on a dimethacrylate-derivative of dimer acid (N`Durance, ND) were tested. Polymerization stress was determined in 1-mm high specimens inserted between two PMMA rods attached to a universal testing machine. Total volumetric shrinkage was measured using a mercury dilatometer. Maximum shrinkage rate was used as a parameter of the reaction speed. Post-gel shrinkage was measured using strain-gages. Elastic modulus was obtained by three-point bending. Data were submitted to one-way ANOVA/Tukey test (p = 0.05), except for elastic modulus (Kruskal-Wallis). Results. Composites ranked differently for total and post-gel shrinkage. Among the materials considered as ""low-shrinkage"" by the respective manufacturers, LS, EL and VD presented low post-gel shrinkage, while AP and ND presented relatively high values. Polymerization stress showed a strong correlation with post-gel shrinkage except for LS, which presented high stress. Elastic modulus and shrinkage rate showed weak relationships with polymerization stress. Significance. Not all low-shrinkage composites demonstrated reduced polymerization shrinkage. Also, in order to effectively reduce polymerization stress, a low post-gel shrinkage must be associated to a relatively low elastic modulus. (C) 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Influence of matrix composition on polymerization stress development of experimental composites

Objective. Stress development at the tooth/restoration interface is one of the most important reasons for failure of adhesive restorations. The aim of this study was to evaluate the influence of BisGMA/TEGDMA (B/T) and UDMA/TEGDMA (U/T) ratios on polymerization stress (PS) and on the variables related to its development: degree of conversion (DC), polymerization maximum rate (Rp(max)), volumetric shrinkage (VS), elastic modulus (E), stress relaxation (SR) and viscosity of experimental composites. Method. Composites were formulated containing B/T or U/T in mol% ratios of 2: 8, 3: 7, 4: 6, 5: 5, 6: 4, 7: 3 and 8: 2, and 15 wt% of fumed silica. PS was determined with a universal testing machine. VS was measured with a linometer. E and SR were obtained in three-point bending. DC and Rp(max) were determined by real time NIR spectroscopy and viscosity was measured in viscometer. Data were submitted to one-way ANOVA, Tukey test (alpha = 0.05%) and regression analyses. Results. PS, VS, E and DC decreased and viscosity and Rp(max) increased with base monomer content in both series. PS showed strong correlation with VS, DC and viscosity. PS, VS and DC were higher and viscosity was lower for UDMA-based materials. Significance. Reduced viscosity, kinetics parameters and molecular characteristics led UDMA-based composites to elevated conversion and relatively lower PS at lower TEGDMA contents, compared to B/T composites. (C) 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Contraction stress related to composite inorganic content

Objectives. The role of inorganic content on physical properties of resin composites is well known. However, its influence on polymerization stress development has not been established. The aim of this investigation was to evaluate the influence of inorganic fraction on polymerization stress and its determinants, namely, volumetric shrinkage, elastic modulus and degree of conversion. Methods. Eight experimental composites containing 1:1 BisGMA (bisphenylglycidyl dimethacrylate): TEGDMA (triethylene glycol dimethacrylate) (in mol) and barium glass at increasing concentrations from 25 to 60 vol.% (5% increments) were tested. Stress was determined in a universal test machine using acrylic as bonding substrate. Nominal polymerization stress was obtained diving the maximum load by the cross-surface area. Shrinkage was measured using a water picnometer. Elastic modulus was obtained by three-point flexural test. Degree of conversion was determined by FT-Raman spectroscopy. Results. Polymerization stress and shrinkage showed inverse relationships with filler content (R(2) = 0.965 and R(2) = 0.966, respectively). Elastic modulus presented a direct correlation with inorganic content (R(2) = 0.984). Degree of conversion did not vary significantly. Polymerization stress showed a strong direct correlation with shrinkage (R(2) = 0.982) and inverse with elastic modulus (R(2) = 0.966). Significance. High inorganic contents were associated with low polymerization stress values, which can be explained by the reduced volumetric shrinkage presented by heavily filled composites. (C) 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Shrinkage stress and mechanical properties of photoactivated composite resin using the argon ion laser

The objective of this study was to verify the influence of photoactivation with the argon ion laser on shrinkage stress (SS), followed by evaluation of Vickers microhardness (VM), percentage of maximum hardness (PMH), flexural strength (FS), and flexural modulus (FM) of a composite resin. The study groups were: L1-laser at 200 mW for 10 seconds; L2-laser at 200 mW for 20 seconds; L3-laser at 250 mW for 10 seconds; L4-laser at 250 mW for 20 seconds; H-halogen light at 275 mW for 20 seconds. Data were analyzed by ANOVA/Tukey`s test (alpha=5%). The values of SS (MPa) were statistically lower for the group L3 (1.3)c, followed by groups L1 (2.7)b, L4 (3.4)a, b, L2 (3.7)a, and H (4.5)a. There was no difference in the values of VM when the same time of photoactivation was used, with respective values being L1=70.1a, L2=78.1b, L3=69.9a, L4=78.1b and H=79.9b. All groups showed a PMH of at least 80%. Only the group L1 showed differences in FS (MPa) and FM (GPa), the respective values of 86.2 and 5.4 being lower. Therefore, the use of argon ion laser had influenced the composite resin polymerization. The L3 group presented adequate mechanical properties and minimum SS, reducing the clinical working time for photoactivation of restorations with the tested resin by 50%.

Factors Affecting Photopolymerization Stress in Dental Composites

Polymerization stress development results from the complex interplay of volumetric shrinkage, reaction kinetics, and viscoelastic properties. The objective of this study was to examine the relationships among volumetric shrinkage, degree of conversion, rate of polymerization (RPmax), and stress development for 2 model bis-GMA-based composites. Three irradiances were used 220, 400, or 600 mW/cm(2) - with exposure times adjusted to deliver the same radiant energy. Volumetric shrinkage was determined with a mercury dilatometer, degree of conversion and RPmax by differential scanning calorimetry (DSC), and polymerization stress with a low-compliance device (Sakaguchi et al., 2004b). Results indicated that polymerization reaction rate and shrinkage were not correlated. Irradiance was directly related to polymerization reaction rate and to stress development. The group with the highest stress/degree of conversion exhibited the lowest RPmax, so it can be assumed, within the limitations of this study, that the conversion was most closely related to stress development.

Contraction stress determinants in dimethacrylate composites

The influence of composite organic content on polymerization stress development remains unclear. It was hypothesized that stress was directly related to differences in degree of conversion, volumetric shrinkage, elastic modulus, and maximum rate of polymerization encountered in composites containing different BisGMA (bisphenylglycidyl dimethacrylate) concentrations and TEGDMA ( triethylene glycol dimethacrylate) and/or BisEMA ( ethoxylated bisphenol-A dimethacrylate) as co-monomers. Stress was determined in a tensilometer. Volumetric shrinkage was measured with a mercury dilatometer. Elastic modulus was obtained by flexural test. We used fragments of flexural specimens to determine degree of conversion by FT-Raman spectroscopy. Reaction rate was determined by differential scanning calorimetry. Composites with lower BisGMA content and those containing TEGDMA showed higher stress, conversion, shrinkage, and elastic modulus. Polymerization rate did not vary significantly, except for the lower value of the 66% TEGDMA composite. We used linear regressions to evaluate the association between polymerization stress and conversion (R-2 = 0.905), shrinkage ( R-2 = 0.825), and modulus ( R-2 = 0.623).

BisGMA/TEGDMA ratio and filler content effects on shrinkage stress

Objective. To investigate the contributions of BisGMA:TEGDMA and filler content on polymerization stress, along with the influence of variables associated with stress development, namely, degree of conversion, reaction rate, shrinkage, elastic modulus and loss tangent for a series of experimental dental composites. Methods. Twenty formulations with BisGMA: TEGDMA ratios of 3: 7, 4: 6, 5: 5, 6: 4 and 7: 3 and barium glass filler levels of 40, 50, 60 or 70 wt% were studied. Polymerization stress was determined in a tensilometer, inserting the composite between acrylic rods fixed to clamps of a universal test machine and dividing the maximum load recorded by the rods cross-sectional area. Conversion and reaction rate were determined by infra-red spectroscopy. Shrinkage was measured by mercury dilatometer. Modulus was obtained by three-point bending. Loss tangent was determined by dynamic nanoindentation. Regression analyses were performed to estimate the effect of organic and inorganic contents on each studied variable, while a stepwise forward regression identified significant variables for polymerization stress. Results. All variables showed dependence on inorganic concentration and monomeric content. The resin matrix showed a stronger influence on polymerization stress, conversion and reaction rate, whereas filler fraction showed a stronger influence on shrinkage, modulus and loss tangent. Shrinkage and conversion were significantly related to polymerization stress. Significance. Both the inorganic filler concentration and monomeric content affect polymerization stress, but the stronger influence of the resin matrix suggests that it may be possible to reduce stress by modifying resin composition without sacrificing filler content. The main challenge is to develop formulations with low shrinkage without sacrificing degree of conversion. (C) 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Adhesive Temperature: Effects on Adhesive Properties and Resin-Dentin Bond Strength

Objectives: To evaluate the effect of adhesive temperature on the resin-dentin bond strength (mu TBS), nanoleakage (NL), adhesive layer thickness (AL), and degree of conversion (DC) of ethanol/water- (SB) and acetone-based (PB) etch-and-rinse adhesive systems. Methods: The bottles of the two adhesives were kept at each temperature (5 degrees C, 20 degrees C, 37 degrees C, and 50 degrees C) for 2 hours before application to demineralized dentin surfaces of 40 molars. Specimens were prepared for mu TBS testing. Bonded sticks (0.8 mm(2)) were tested under tension (0.5 mm/min). Three bonded sticks from each tooth were immersed in silver nitrate and analyzed by scanning electron microscopy. The DC of the adhesives was evaluated by Fourier transformed infrared spectroscopy. Results: Lower mu TBS was observed for PB at 50 degrees C. For SB, the mu TBS values were similar for all temperatures. DC was higher at 50 degrees C for PB. Higher NL and thicker AL were observed for both adhesives in the 5 degrees C and 20 degrees C groups compared to the 37 degrees C and 50 degrees C groups. The higher temperatures (37 degrees C or 50 degrees C) reduced the number of pores within the adhesive layer of both adhesive systems. Conclusions: It could be useful to use an ethanol/water-based adhesive at 37 degrees C or 50 degrees C and an acetone-based adhesive at 37 degrees C to improve adhesive performance.

Patients with oral squamous cell carcinoma are characterized by increased frequency of suppressive regulatory T cells in the blood and tumor microenvironment

Oral squamous cell carcinoma (OSCC) is a cancerous lesion with high incidence worldwide. The immunoregulatory events leading to OSCC persistence remain to be elucidated. Our hypothesis is that regulatory T cells (Tregs) are important to obstruct antitumor immune responses in patients with OSCC. In the present study, we investigated the frequency, phenotype, and activity of Tregs from blood and lesions of patients with OSCC. Our data showed that > 80% of CD4(+)CD25(+) T cells isolated from PBMC and tumor sites express FoxP3. Also, these cells express surface Treg markers, such as GITR, CD45RO, CD69, LAP, CTLA-4, CCR4, and IL-10. Purified CD4(+)CD25(+) T cells exhibited stronger suppressive activity inhibiting allogeneic T-cell proliferation and IFN-gamma production when compared with CD4(+)CD25(+) T cells isolated from healthy individuals. Interestingly, approximately 25% of CD4(+)CD25(-) T cells of PBMC from patients also expressed FoxP3 and, although these cells weakly suppress allogeneic T cells proliferative response, they inhibited IFN-gamma and induced IL-10 and TGF-beta secretion in these co-cultures. Thus, our data show that Treg cells are present in OSCC lesions and PBMC, and these cells appear to suppress immune responses both systemically and in the tumor microenvironment.

In vitro wear, surface roughness and hardness of propanal-containing and diacetyl-containing novel composites and copolymers based on bis-GMA analogs

Objective. To evaluate the effect of two additives, aldehyde or diketone, on the wear, roughness and hardness of bis-GMA-based composites/copolymers containing TEGDMA, propoxylated bis-GMA (CH(3)bis-GMA) or propoxylated fluorinated bis-GMA (CF(3)bis-GMA). Methods. Fifteen experimental composites and 15 corresponding copolymers were prepared combining bis-GMA and TEGDMA, CH3bis-GMA or CF3bis-GMA, with aldehyde (24mol% and 32 mol%) or diketone (24 mol% and 32 mol%) totaling 30 groups. For composites, hybrid treated filler (barium aluminosilicate glass/pyrogenic silica; 60 wt%) was added to monomer mixtures. Photopolymerization was affected by 0.2 wt% each of camphorquinone and N,N-dimethyl-p-toluidine. Wear (W) test was conducted in a toothbrushing abrasion machine (n = 6) and quantified using a profilometer. Surface roughness (R) changes, before and after abrasion test, were determined using a rugosimeter. Microhardness (H) measurements were performed for dry and wet samples using a Knoop microindenter (n = 6). Data were analyzed by one-way ANOVA and Tukey`s test (alpha = 0.05). Results. Incorporation of additives led to improved W and H values for bis-GMA/TEGDMA and bis-GMA/CH(3)bis-GMA systems. Additives had no significant effect on the W and H changes of bis-GMA/CF(3)bis-GMA. With regard to R changes, additives produced decreased values for bis-GMA/CH3bis-GMA and bis-GMA/CF3bis-GMA composites. Bis-GMA/TEGDMA and bis-GMA/CH(3)bis-GMA copolymers with additives became smoother after abrasion test. Significance. The findings correlate with additives ability to improve degree of conversion of some composites/copolymers thereby enhancing mechanical properties. Published by Elsevier Ltd on behalf of Academy of Dental Materials

Influence of differently oriented dentin surfaces and the regional variation of specimens on adhesive layer thickness and bond strength

Statement of the Problem: Adhesive systems can spread differently onto a substrate and, consequently, influence bonding. Purpose: The purpose of this study was to evaluate the effect of differently oriented dentin surfaces and the regional variation of specimens on adhesive layer thickness and microtensile bond strength (MTBS). Materials and Methods: Twenty-four molars were sectioned mesiodistally to expose flat buccal and lingual halves. Standardized drop volumes of adhesive systems (Single Bond [SB] and Prime & Bond 2.1 [PB2.1]) were applied to dentin according to the manufacturer`s instructions. Teeth halves were randomly divided into groups: 1A-SB/parallel to gravity; 1B-SB/perpendicular to gravity; 2A-PB2.1/parallel to gravity; and 2B-PB2.1/perpendicular to gravity. The bonded assemblies were stored in 37 degrees C distilled water for 24 hours and then sectioned to obtain dentin sticks (0.8 mm(2)). The adhesive layer thickness was determined in a light microscope (x200), and after 48 hours the specimens were subjected to MTBS test. Data were analyzed by one-way and two-way analysis of variance and Student-Newman-Keuls tests. Results: Mean values (MPa +/- SD) of MTBS were: 39.1 +/- 12.9 (1A); 32.9 +/- 12.4 (1B); 52.9 +/- 15.2 (2A); and 52.3 +/- 16.5 (2B). The adhesive systems` thicknesses (mu m +/- SD) were: 11.2 +/- 2.9 (1A); 18.1 +/- 7.3 (1B); 4.2 +/- 1.8 (2A); and 3.9 +/- 1.3 (2B). No correlation between bond strength and adhesive layer thickness for both SB and PB2.1 (r = -0.224, p = 0.112 and r = 0.099, p = 0.491, respectively) was observed. Conclusions: The differently oriented dentin surfaces and the regional variation of specimens on the adhesive layer thickness are material-dependent. These variables do not influence the adhesive systems` bond strength to dentin. CLINICAL SIGNIFICANCE Adhesive systems have different viscosities and spread differently onto a substrate, influencing the bond strength and also the adhesive layer thickness. Adhesive thickness does not influence dentin bond strength, but it may impair adequate solvent evaporation, polymer conversion, and may also determine water sorption and adhesive degradation over time. In the literature, many studies have shown that the adhesive layer is a permeable membrane and can fail over timebecause ofits continuous plasticizing and degradation when in contact with water. Therefore, avoiding thick adhesive layers may minimize these problems and provide long-term success for adhesive restorations.

Network structures of Bis-GMA/TEGDMA resins differ in DC, shrinkage-strain, hardness and optical properties as a function of reducing agent

Objectives. To evaluate the influence of different tertiary amines on degree of conversion (DC), shrinkage-strain, shrinkage-strain rate, Knoop microhardness, and color and transmittance stabilities of experimental resins containing BisGMA/TEGDMA (3: 1 wt), 0.25wt% camphorquinone, 1wt% amine (DMAEMA, CEMA, DMPT, DEPT or DABE). Different light-curing protocols were also evaluated. Methods. DC was evaluated with FTIR-ATR and shrinkage-strain with the bonded-disk method. Shrinkage-strain-rate data were obtained from numerical differentiation of shrinkage-strain data with respect to time. Color stability and transmittance were evaluated after different periods of artificial aging, according to ISO 7491: 2000. Results were evaluated with ANOVA, Tukey, and Dunnett`s T3 tests (alpha = 0.05). Results. Studied properties were influenced by amines. DC and shrinkage-strain were maximum at the sequence: CQ < DEPT < DMPT <= CEMA approximate to DABE < DMAEMA. Both DC and shrinkage were also influenced by the curing protocol, with positive correlations between DC and shrinkage-strain and DC and shrinkage-strain rate. Materials generally decreased in L* and increased in b*. The strong exception was the resin containing DMAEMA that did not show dark and yellow shifts. Color varied in the sequence: DMAEMA < DEPT < DMPT < CEMA < DABE. Transmittance varied in the sequence: DEPT approximate to DABE < DABE approximate to DMPT approximate to CEMA < DMPT approximate to CEMA approximate to DMAEMA, being more evident at the wavelength of 400 nm. No correlations between DC and optical properties were observed. Significance. The resin containing DMAEMA showed higher DC, shrinkage-strain, shrinkage-strain rate, and microhardness, in addition to better optical properties. (C) 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of curing protocol on the polymerization of dual-cured resin cements

Objectives. The purpose of this study was to evaluate how curing protocol affects the extent of polymerization of dual-cured resin cements. Methods. Four commercial resin cements were used (DuoLink, Panavia F 2.0, Variolink II and Enforce). The extent of polymerization of the resin cements cured under different conditions was measured using a (1)H Stray-Field MRI method, which also enabled to probe molecular mobility in the kHz frequency range. Results. Resin cements show well distinct behaviours concerning chemical cure. Immediate photo-activation appears to be the best choice for higher filler loaded resin cements (Panavia F 2.0 and Variolink). A photo-activation delay (5 min) did not induce any significant difference in the extent of polymerization of all cements. Significance. The extent of polymerization of dual-cured resin cements considerably changed among products under various curing protocols. Clinicians should optimize the materials choice taking into account the curing characteristics of the cements. (C) 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

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

Objectives. To 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. Methods. Root canals of 40 bovine incisors were prepared for post space. Fibrekor (R) 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 degrees 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 degrees C for 3 months, followed by sectioning and measuring. Data were analyzed by a series of two-way ANOVA and Tukey tests at alpha = 5%. Results. Statistically 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. Results 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. (C) 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Bond strength of Epiphany (TM) Sealer combined with different adhesive systems photo-activated with LED and QTH

The Epiphany (TM) Sealer is a new dual-curing resin-based sealer and has been introduced as an alternative to gutta-percha and traditional root canal sealers. The canal filling is claimed to create a seal with the dentinal tubules within the root canal system producing a `monoblock` effect between the sealer and dentinal tubules. Therefore, considering the possibility to incorporate the others adhesive systems, it is important to study the bond strength of the resulting cement. Forty-eight root mandibular canines were sectioned 8-mm below CEJ. The dentine discs were prepared using a tapered diamond bur and irrigated with 1% NaOCl and 17% EDTA. Previous the application Epiphany (TM) Sealer, the Epiphany (TM) Primer, AdheSE, and One Up Bond F were applied to the root canal walls. The LED and QTH (Quartz Tungsten Halogen) were used to photo-activation during 45 s with power density of 400 and 720 mW/cm(2), respectively. The specimens were performed on a universal testing machine at a cross-head speed of 1 mm/min until bond failure occurred. The force was recorded and the debonding values were used to calculate Push-out bond strength. The analysis of variance (ANOVA) and Tukey`s post-hoc tests showed significant statistical differences (P < 0.05) to Epiphany (TM) Sealer/Epiphany (TM) Primer/QTH and EpiphanyTM Sealer/AdheSE/QTH, which had the highest mean values of bond strength. The efficiency of resin-based filling materials are dependent the type of light curing unit used including the power density, the polymerization characteristics of these resin-based filling materials, depending on the primer/adhesive used.