Polymerization stress of resin composites as a function of system compliance

Objectives. Evaluate the effect of testing system compliance on polymerization stress and stress distribution of composites. Methods. Composites tested were Filtek Z250 (FZ), Herculite (HL), Tetric Ceram (TC), Helio Fill-AP (HF) and Heliomolar (HM). Stress was determined in 1-mm thick specimens, inserted between two rods of either poly(methyl methacrylate), PMMA, or glass. Experimental nominal stress (sigma(exp)) was calculated by dividing the maximum force recorded 5 min after photoactivation by the cross-sectional area of the rod. Composites` elastic modulus (E) was obtained by three-point bending. Data were submitted to one-way ANOVA/Tukey`s test (alpha = 0.05). Stress distribution on longitudinal (sigma(y)) and transverse (sigma(x)) axes of models representing the composites with the highest and lowest E (FZ and HM, respectively) were evaluated by finite element analysis (FEA). Results. sigma(exp) ranged from 5.5 to 8.8 MPa in glass and from 2.6 to 3.4 MPa in PMMA. Composite ranking was not identical in both substrates, since FZ showed or sigma(exp) statistically higher than HM in glass, while in PMMA FZ showed values similar to the other composites. A strong correlation was found between stress reduction (%) from glass to PMMA and composite`s E (r(2) = 0.946). FEA revealed that system compliance was influenced by the composite (FZ led to higher compliance than HM). sigma(x) distribution was similar in both substrates, while cry distribution showed larger areas of compressive stresses in specimens built on PMMA. Significance. sigma(exp) determined in PMMA was 53-68% lower than in glass. Composite ranking varied slightly due to differences in substrates` longitudinal and transverse deformation. (c) 2007 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

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).

The role of surface sealants in the roughness of composites after a simulated toothbrushing test

Objectives: To evaluate the influence of two surface sealants (BisCover/Single Bond) and three application techniques (unsealed/conventional/co-polymerization) on the roughness of two composites (Filtek Z250/Z350) after the toothbrushing test. Methods: Seventy-two rectangular specimens (5 mm x 10 mm x 3 mm) were fabricated and assigned into 12 groups (n = 6). Each sample was subjected to three random roughness readings at baseline, after 100,000 (intermediate), and 200,000 (final) toothbrushing strokes. Roughness (R) at each stage was obtained by the arithmetic mean of the reading of each specimen. Sealant removal was qualitatively examined (optical microscope) and classified into scores (0-3). Data were analyzed by Student`s paired t-test, two-way ANOVA/Tukey`s test, and by Wilcoxon, Kruskal-Wallis and Miller`s test (alpha = 0.05). Results: Z250 groups at baseline did not differ statistically from each other. Unsealed Z350 at baseline had lower R values. All the unsealed groups presented gradual decrease in R from baseline to final brushing. From baseline to the inter-mediate stage, Z250 co-polymerized groups presented a significant reduction in R (score 3). Conventionally sealed groups had no significant changes in R (scores 2-0.8). From baseline to the intermediate stage, the conventionally sealed Z350 Single Bond group had an increase in R (score 1.5). In the final stage, all the conventionally sealed groups presented a reduction in R (scores 0.7-0). Co-polymerized Single Bond groups had a significant reduction in R (scores 2.5-2.7), and co-polymerized BisCover groups an increase in R (scores 2.8-3). Conclusions: At any brushing stage, sealed composites presented superior performance when compared with unsealed composites. (C) 2009 Elsevier Ltd. All rights reserved.

Effect of different surface treatments on the repair bond strength of indirect composites

Purpose: To evaluate the tensile bond strength of indirect composites repaired with different surface treatments and direct composites. Methods: 180 specimens were prepared with Targis, belleGlass HP and Sculpture indirect composites, light-activated and post-cured according to the manufacturers` recommendations. The specimens were stored in distilled water for 24 hours at 37 degrees C. The bonding surfaces were prepared with air abrasion, hydrofluoric acid or hydrofluoric acid followed by a neutralizing solution. All the treated surfaces were subject to the application of a silane and a bonding agent before the repair procedures with Tetric Ceram and Tetric Flow for the Targis specimens, Herculite XRV and Revolution for the belleGlass HP specimens and Sculp-It and Flow-It for Sculpture specimens. The tensile bond strength tests were carried out using a universal testing machine at cross-head speed of 0.5 mm/minute. The type of fracture was observed under a light microscope at x40 magnification. Data were analyzed by a two-way ANOVA and Tukey`s post-hoc tests (P<0.05). Results: Targis showed a statistically higher repair bond strength than belleGlass HP and Sculpture, which were not significantly different from each other. Air abrasion increased the repair bond strength of belleGlass HP and Sculpture. For Targis, all the surface treatments resulted in similar repair bond strength. The different viscosity of repair composites did not affect the repair of indirect composites. Fractured surfaces showed mostly adhesive failures, mainly with hydrofluoric acid treatment.

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

Clinical evaluation of two packable posterior composites A five-year follow-up

Background. Research has suggested that packable resin-based composites inserted with a placement technique similar to amalgam condensation can reduce the sensitivity associated with posterior restorations. The authors evaluated the clinical performance, including associated sensitivity, of two packable composites in a randomized five-year clinical trial. Methods. A single operator randomly placed two restorations in each of 33 patients: one restoration consisting of Alert (Jeneric/Pentron, Wallingford, Conn.) and the other consisting of SureFil (Dentsply/Caulk, Milford, Del.). There were 30 Class I and 36 Class II restorations. Two independent evaluators evaluated the restorations by using modified U.S.; Public Health Service criteria. The authors analyzed data by means of the Fisher, chi(2) and McNemar tests at P < .05. Results. Of 60 restorations evaluated at five years, two Class II restorations (one SureFil, one Alert) failed. All other restorations received the highest score possible for sensitivity and vitality. The only difference between the composites at the five-year recall was the significantly better surface texture of SureFil. The authors observed significantly different scores between the baseline and at five years for marginal discoloration (Alert and SureFil), surface texture (Alert and SureFil) and color (SureFil). Conclusions. Both packable resin-based composites showed excellent durability during the five-year follow-up. Clinical Implications. The investigated resin-based composites are suitable for posterior restorations.

Color stability of silorane-based composites submitted to accelerated artificial ageing-An in situ study

Objectives: To assess the in situ color stability, surface and the tooth/restoration interface degradation of a silorane-based composite (P90, 3M ESPE) after accelerated artificial ageing (AAA), in comparison with other dimethacrylate monomer-based composites (Z250/Z350, 3M ESPE and Esthet-X, Dentsply). Methods: Class V cavities (25 mm(2) x 2 mmdeep) were prepared in 48 bovine incisors, which were randomly allocated into 4 groups of 12 specimens each, according to the type of restorative material used. After polishing, 10 specimens were submitted to initial color readings (Easyshade, Vita) and 2 to analysis by scanning electronic microscopy (SEM). Afterwards, the teeth were submitted to AAA for 384 h, which corresponds to 1 year of clinical use, after which new color readings and microscopic images were obtained. The values obtained for the color analysis were submitted to statistical analysis (1-way ANOVA, Tukey, p < 0.05). Results: With regard to color stability, it was verified that all the composites showed color alteration above the clinically acceptable levels (Delta E >= 3.3), and that the silorane-based composite showed higher Delta E (18.6), with a statistically significant difference in comparison with the other composites (p < 0.05). The SEM images showed small alterations for the dimethacrylate-based composites after AAA and extensive degradation for the silorane-based composite with a rupture at the interface between the matrix/particle. Conclusion: It may be concluded that the silorane-based composite underwent greater alteration with regard to color stability and greater surface and tooth/restoration interface degradation after AAA. (C) 2011 Elsevier Ltd. All rights reserved.

Effect of accelerated carbonation on cementitious roofing tiles reinforced with lignocellulosic fibre

The present work evaluated the effects of accelerated carbonation on mechanical and physical characteristics of cementitious roofing tiles reinforced with vegetable fibre. The maximum load and toughness of the tiles have increased approximately 25% and 80% respectively as a consequence of the accelerated carbonation. Water absorption and apparent porosity decreased with carbonation while bulk density increased as a clear indication of the densification of the composite. The improvement on the mechanical performance suggests that the fibres retained their tensile strength in the inorganic matrix. Results of specimens extracted from the tested tiles after approximately 480 days in laboratory environment and further aged indicate that soak and dry cycles promoted some leaching of hydration products and more voids and lower density when performed before carbonation. The results indicate the utilization of accelerated carbonation as an effective procedure to mitigate the degradation suffered by the cellulose fibres in the less aggressive medium. (C) 2009 Elsevier Ltd. All rights reserved.

EPR in the Characterization of the Shade Effect on Translucence, Remaining Free Radicals, and Polymerization Depth of Commercially Available Resin Composites

The aim of this study was to assess the relation between the number of free radicals generated and the polymerization depth in two different commercial brands of resin composites with different colors and translucence. Electron paramagnetic resonance quantified the radical populations through relative intensity (I (r)) of free radicals generated, and radical decay was monitored. Sample translucence and the classical polymerization depth were measured. The analysis indicated that resin with more color pigments (MA4, I (r) = 0.73 a.u) or more opacity components (ODA2, I (r) = 0.84 a.u) generated smaller populations of free radicals and have the lower polymerization depth than clearer (M, I (r) = 1.20 a.u and MA2, I (r) = 1.02) or more translucent (OEA2, I (r) = 1.00 a.u) composites for the same light-curing time. It seems that irradiation doses have to be adequate to more colored and less translucent resins.

Stability and interface properties of thin cellulose ester films adsorbed from acetone and ethyl acetate solutions

Stability and interface properties of cellulose acetate propionate (CAP) and cellulose acetate butyrate (CAB) films adsorbed from acetone or ethyl acetate onto Si wafers have been investigated by means of contact angle measurements and atomic force microscopy (AFM). Surface energy (gamma(total)(S)) values determined for CAP adsorbed from acetone are larger than those from ethyl acetate. In the case of CAB films adsorbed from ethyl acetate and acetone were similar. Dewetting was observed by AFM only for CAP films prepared from ethyl acetate. Positive values of effective Hamaker constant (A(eff)) were found only for CAP prepared from ethyl acetate, corroborating with dewetting phenomena observed by AFM. Oil the contrary, negative values of A(eff) were determined for CAP and CAB prepared from acetone and for CAB prepared from ethyl acetate, Corroborating with experimental observations. Sum frequency generation (SFG) vibrational spectra indicated that CAP and CAB films prepared from ethyl acetate present more alkyl groups oriented perpendicularly to the polymer-air interface than those films prepared from acetone. Such preferential orientation corroborates with macroscopic contact angle measurements. Moreover, SFG spectra showed that acetone hinds strongly to Si wafers, creating a new surface for CAP and CAB films. (C) 2008 Elsevier Inc. All rights reserved.

A Morphological View of the Sodium 4,4 `-Distyrylbiphenyl Sulfonate Fluorescent Brightness Distribution on Regenerated Cellulose Fibers

Evidence of the sorption of the whitening agent sodium 4,4`-distyrylbiphenyl sulfonate in the presence of the anionic surfactant sodium dodecylsulfate or the cationic surfactant dodecyl trimethyl ammonium chloride on regenerated cellulose fibers is given by several microscopy techniques. Scanning electron microscopy provided images of the cylindrical fibers with dimensions of 3.5 cm (length) and 13.3 mu m (thickness), with empty cores of 1 mu m diameter and a smooth surface. Atomic force microscopy showed a fiber surface with disoriented nanometric domains using both tapping-mode height and phase image modes. Atomic force microscopy also showed that the whitening agent and surfactant molecules were sorbed onto the fiber surface, in agreement with the adsolubilization sorption model. Transmission electron microscopy showed fibers with nanometric parallel cylinders, surrounded by holes where the fluorescent whitening molecules accumulated. On the basis of these techniques, we conclude that the sorption process occurs preferentially on the fiber surface in contact with the water solution, and under saturated conditions, the whitening agent penetrates into the pores and are simultaneously sorbed on the pore walls bulk, forming molecular aggregates. (C) 2010 Wiley Periodicals, Inc. J Appl Polym Sci 2321-2327, 2010

Elastomeric Composites Based on Ethylene-Propylene-Diene Monomer Rubber and Conducting Polymer-Modified Carbon Black

Thermally stable elastomeric composites based on ethylene-propylene-diene monomer (EPDM) and conducting polymer-modified carbon black (CPMCB) additives were produced by casting and crosslinked by compression molding. CPMCB represent a novel thermally stable conductive compound made via ""in situ"" deposition of intrinsically conducting polymers (ICP) such as polyaniline or polypyrrole on carbon black particles. Thermogravimetric analysis showed that the composites are thermally stable with no appreciable degradation at ca. 300 degrees C. Incorporating CPMCB has been found to be advantageous to the processing of composites, as the presence of ICP lead to a better distribution of the filler within the rubber matrix, as confirmed by morphological analysis. These materials have a percolation threshold range of 5-10 phr depending on the formulation and electrical dc conductivity values in the range of 1 x 10(-3) to 1 x 10(-2) S cm(-1) above the percolation threshold. A less pronounced reinforcing effect was observed in composites produced with ICP-modified additives in relation to those produced only with carbon black. The results obtained in this study show the feasibility of this method for producing stable, electrically conducting composites with elastomeric characteristics. POLYM. COMPOS., 30:897-906, 2009. (C) 2008 Society of Plastics Engineers

Highly Stable, Edible Cellulose Films Incorporating Chitosan Nanoparticles

The need for biodegradable polymers for packaging has fostered the development of novel, biodegradable polymeric materials from natural sources, as an alternative to reduce amount of waste and environmental impacts. The present investigation involves the synthesis of chitosan nanoparticles-carboxymethylcellulose films, in view of their increasing areas of application in packaging industry. The entire process consists of 2-steps including chitosan nanoparticles preparation and their incorporation in carboxymethylcellulose films. Uniform and stable particles were obtained with 3 different chitosan concentrations. The morphology of chitosan nanoparticles was tested by transmission electron microscopy, revealing the nanoparticles size in the range of 80 to 110 nm. The developed film chitosan nanoparticles-carboxymethylcellulose films were characterized by Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis, solubility tests, and mechanical analysis. Improvement of thermal and mechanical properties were observed in films containing nanoparticles, with the best results occurring upon addition of nanoparticles with 110 nm size in carboxymethylcellulose films. Practical Application Carboxymethylcellulose films containing chitosan nanoparticles synthesized and characterized in this article could be a potential material for food and beverage packaging applications products due to the increase mechanical properties and high stability. The potential application of the nanocomposites prepared would be in packaging industry to extend the shelf life of products.

Luminescence characteristics of YAP:Ce scintillator powders and composites

Cerium doped yttrium aluminate perovskite YAlO(3) (YAP) powders are pursued as interesting alternatives to bulk crystals for application in scintillating devices. The emissions of these materials in the near-UV and visible spectral regions originate from electric dipole transitions between 4f and 5d energy levels of Ce(3+) and largely depend on the environment occupied by the ion. In search for improved synthesis conditions that can lead to phase pure powders with optimized structural and spectroscopic characteristics, in this work we have employed the polymeric precursor (Pechini) method to prepare crystalline and amorphous YAP:Ce powders doped with 1-10 mol% Ce(3+). Interesting composite materials were also obtained by dispersing some of the YAP:Ce powders in silica xerogels. A comparative structural and spectroscopic study of all the samples was done by XRD, FT-IR, emission, excitation and excited state lifetime measurements. In agreement with previous reports, excitation at 296 nm results in intense emission in the range 315-425 nm with an average decay time of 30 ns. (c) 2010 Elsevier B.V. All rights reserved.

Thermal characterization of dental composites by TG/DTG and DSC

Dental composites can be improved by heat treatment, as a possible way to increase mechanical properties due to additional cure (post-cure). Direct dental composites are essentially similar to the indirect ones, supposing they have the same indication. Therefore, to establish a heat treatment protocol for direct composites, using as indirect (photoactivated by continuous and pulse-delay techniques), a characterization (TG/DTG and DSC) is necessary to determine parameters, such as mass loss by thermal decomposition, heat of reaction and glass transition temperature (T (g)). By the results of this study, a heat treatment could be carried out above 160 A degrees C (above T (g), and even higher than the endset exothermic event) and under 180 A degrees C (temperature of significant initial mass loss).