Effect of pre-heating resin composite and light-curing units on monomer conversion

The purpose of this study was to evaluate the effect of pre-heating resin composite photo-cured with light-curing units (LCU) by FT-IR. Twenty specimens were made in a metallic mold (4 mm diameter × 2 mm thick) from composite resin-Tetric Ceram® (Ivoclar/Vivadent) at room temperature (25°C) and pre-heated to 37, 54, and 60°C. The specimens were cured with halogen curing light (QTH) and light emitted by diodes (LED) during 40 s. Then, the specimens were pulverized, pressed with KBr and analyzed with FT-IR. The data were submitted to statistical analysis of variance and Kruskal-Wallis test. Study data showed no statistically significant difference to the degree of conversion for the different light curing units (QTH and LED) (p > 0.05). With the increase of temperature there was significant increase in the degree of conversion (p < 0.05). In this study were not found evidence that the light curing unit and temperature influenced the degree of conversion. © 2010 Pleiades Publishing, Ltd.

Effect of light energy density on conversion degree and hardness of dual-cured resin cement

This study evaluated the effect of different light energy densities on conversion degree (CD) and Knoop hardness number (KHN) of RelyX ARC (RLX) resin cement. After manipulation according to the manufacturer's instructions, RLX was inserted into a rubber mold (0.8 mm X 5 mm) and covered with a Mylar strip. The tip of the lightcuring unit (LCU) was positioned in contact with the Mylar surface. Quartz-tungsten-halogen (QTH) and light-emitting diode (LED) LCUs with light densities of 10, 20 and 30 J/cm2 were used to light-cure the specimens. After light curing, the specimens were stored dry in lightproof containers at 37°C. After 24 hours, the CD was analyzed by FT-Raman and, after an additional 24-hours, samples were submitted to Knoop hardness testing. The data of the CD (%) and KHN were submitted to two-way ANOVA and the Tukey's test (α=0.05). QTH and LED were effective light curing units. For QTH, there were no differences among the light energy densities for CD or KHN. For LED, there was a significant reduction in CD with the light energy density set at 10 J/cm2. KHN was not influenced by the lightcuring unit and by its light energy density. © Operative Dentistry.

Temperature rise during adhesive and composite polymerization with different light-curing sources

AIM: This study evaluated the temperature rise of the adhesive system Single Bond (SB) and the composite resins Filtek Z350 flow (Z) and Filtek Supreme (S), when polymerized by light-emitting diode (LED XL 3000) and quartz-tungsten halogen (QTH Biolux). METHODS: Class V cavities (3 yen2 mm) were prepared in 80 bovine incisors under standardized conditions. The patients were divided as follows: G1: Control; G2: SB; G3: SB + Z; G4: SB + S. The groups were subdivided into two groups for polymerization (A: QTH, B: LED). Light curing was performed for 40 s and measurement of temperature changes during polymerization was performed with a thermocouple positioned inside the pulp chamber. Data were statistically analyzed using ANOVA and Tukey tests. RESULTS: The factors material (P<0.00001) and curing unit (P<0.00001) had significant influence on temperature rise. The lowest temperature increase (0.15 degrees C) was recorded in G2 B and the highest was induced in G1 A (0.75 degrees C, P<0.05). In all groups, lower pulp chamber temperature measurements were obtained when using LED compared to QTH (P<0.05). CONCLUSION: QTH caused greater increases in tooth temperature than LED. However, both sources did not increase pulpal temperature above the critical value that may cause pulpal damage.

Effect of thickness of indirect restoration and distance from the light-curing unit tip on the hardness of a dual-cured resin cement

This study evaluated the Knoop hardness and polymerization depth of a dual-cured resin cement, light-activated at different distances through different thicknesses of composite resin. One bovine incisor was embedded in resin and its buccal surface was flattened. Dentin was covered with PVC film where a mold (0.8-mm-thick and 5 mm diameter) was filled with cement and covered with another PVC film. Light curing (40 s) was carried out through resin discs (2, 3, 4 or 5 mm) with a halogen light positioned 0, 1, 2 or 3 mm from the resin surface. After storage, specimens were sectioned for hardness measurements (top, center, and bottom). Data were subjected to split-plot ANOVA and Tukey's test (α=0.05). The increase in resin disc thickness decreased cement hardness. The increase in the distance of the light curing tip decreased hardness at the top region. Specimens showed the lowest hardness values at the bottom, and the highest at the center. Resin cement hardness was influenced by the thickness of the indirect restoration and by the distance between the light-curing unit tip and the resin cement surface.

Kinetic parameters for thermal decomposition of supramolecular polymers derived from diclofenac-meglumine supramolecular adducts

Meglumine is an aminocarbohydrate able to form supramolecular adducts with organic acids. The recognition is based on hydrogen bonds and the structures resulting from the complexation have high solubility in water. This property has been exploited by the pharmaceutical industry in the improvement of existing drugs, and the successful example of this approach involves the poorly soluble non-steroidal anti-inflammatory drugs (NSAIDs). Investigation of the thermal behavior of adduct obtained from meglumine and the NSAID diclofenac revealed that a polymer-like material is formed from the self-assembly of diclofenac-meglumine adducts in the melt. This polymer showed a high molecular weight around 2.0×105kDa. The kinetic parameters for the thermal decomposition step of the polymer were determined by the Capela-Ribeiro non-linear isoconversional method. From data for the TG curves in nitrogen atmosphere and heating rates of 5, 10, 15 and 20°Cmin-1, the Eα and Bα terms could be determined, and consequently the pre-exponential factor, Aα, as well as the kinetic model, g(α). © 2012 Elsevier B.V.

Effects of cement-curing mode and light-curing unit on the bond durability of ceramic cemented to dentin

The aim of this study was to evaluate the effects of different light-curing units and resin cement curing types on the bond durability of a feldspathic ceramic bonded to dentin. The crowns of 40 human molars were sectioned, exposing the dentin. Forty ceramic blocks of VITA VM7 were produced according to the manufacturer's recommendations. The ceramic surface was etched with 10% hydrofluoric acid/60s and silanized. The dentin was treated with37% phosphoric acid/15s, and the adhesive was applied. The ceramic blocks were divided and cemented to dentin according to resin cement/RC curing type(dual-and photocured), light-curing unit (halogen light/QTH and LED), and storage conditions (dry and storage/150 days + 12,000 cycles/thermocycling). All blocks were stored in distilled water (37°C/24h) and sectioned (n = 10): G1-QTH + RC Photo, G2-QTH + RC Dual, G3-LED + RC Photo, G4-LED + RC Dual. Groups G5, G6, G7, and G8 were obtained exactly as G1 through G4, respectively, and then stored and thermocycled. Microtensile bond strength tests were performed (EMIC), and data were statistically analyzed by ANOVA and Tukey's test (5%). The bond strength values (MPa) were: G1-12.95 (6.40)ab; G2-12.02 (4.59)ab; G3-13.09 (5.62)ab; G4-15.96 (6.32)a; G5-6.22 (5.90)c; G6-9.48 (5.99)bc; G7-12.78 (11.30)ab; and G8-8.34 (5.98)bc. The same superscript letters indicate no significant differences. Different light-curing units affected the bond strength betweenceramic cemented to dentin when the photocured cement was used, and only after aging (LED>QTH). There was no difference between the effects of dual-and photo-cured resin-luting agents on the microtensile bond strength of the cement used in this study.

Effect of light curing modes on mechanical properties of direct and indirect composites

Objective. To evaluate the degree of conversion (DC), flexural strength (FS) and Knoop microhardness (KHN) of direct and indirect composite resins polymerized with different curing systems. Materials and methods. Specimens of direct (Z250, 3M/Espe) and indirect (Sinfony, 3M/Espe) restorative materials were made and polymerized using two light curing units: XL2500 (3M/Espe) and Visio system (3M/Espe). Absorption spectra of both composites were obtained on a FTIR spectrometer in order to calculate the DC. FS was evaluated in a universal testing machine and surface microhardness was performed in a microhardness tester (50gf/15s). DC, FS and KHN data were submitted to two-way ANOVA and Tukey's test (α = 0.05). Results. Z250 showed higher DC, FS and KHN compared with Sinfony when the polymerization was carried out with XL2500 (p < 0.05). However, there is no statistical difference in DC between the materials when Visio was used (p > 0.05). Visio showed higher DC and KHN for Z250 and Sinfony than the values obtained using XL2500 light curing (p < 0.05). For FS, no significant difference between curing units was found (p > 0.05). Conclusion. Even though the Visio system could increase DC and KHN for some direct and indirect composites, compared with the conventional halogen curing unit, a high number of monomers did not undergo conversion during the polymerization. © 2013 Informa Healthcare.

Thermal stability of ionene polymers

Two different cationic polymers of the same chemical type and with very similar chemical structures were reacted with a natural bentonite over a wide range of polymer/clay ratios. This study involved the synthesis of cationic aliphatic ammonium polyionenes, specifically 3,6-ionene and 3,6-dodecylionene. Ionenes are ion-containing polymers that contain quaternary nitrogen atoms in the main macromolecular chain as opposed to a pendant chain. The CHN content, basal spacing, and elemental composition of each of the polymer-clay complexes were analyzed by X-ray diffraction, X-ray fluorescence, and thermogravimetry. All the polycations reacted to form interlayer complexes with clay, which displaced more Na+ and little Ca2+. Sodium and calcium were both present as interlayer cations in the clay and its complexes. The TG/DTG curves show that both polymers underwent thermal degradation in more than one stage. Specifically, 3,6-ionene was found to undergo two stages of decomposition and 3,6-dodecylionene undergo three stages. The behavior of the TG/DTG curves and the activation energy values suggest that 3,6-dodecylionene (E = 174,85 kJ mol-1) complexes have greater thermal stability than 3,6-ionene (E = 115,52 kJ mol-1) complexes. The mechanism of degradation suggests a direct interaction with the dodecyl chain containing 12 carbons, which are present in 3,6-dodecylionene but not in 3,6-ionene. © 2012 Akadémiai Kiadó, Budapest, Hungary.

Subcutaneous tissue reaction and cytotoxicity of polyvinylidene fluoride and polyvinylidene fluoride-trifluoroethylene blends associated with natural polymers

Cytotoxicity and subcutaneous tissue reaction of innovative blends composed by polyvinylidene fluoride and polyvinylidene fluoride-trifluoroethylene associated with natural polymers (natural rubber and native starch) forming membranes were evaluated, aiming its applications associated with bone regeneration. Cytotoxicity was evaluated in mouse fibroblasts culture cells (NIH3T3) using trypan blue staining. Tissue response was in vivo evaluated by subcutaneous implantation of materials in rats, taking into account the presence of necrosis and connective tissue capsule around implanted materials after 7, 14, 21, 28, 35, 60, and 100 days of surgery. The pattern of inflammation was evaluated by histomorphometry of the inflammatory cells. Chemical and morphological changes of implanted materials after 60 and 100 days were evaluated by Fourier transform infrared (FTIR) absorption spectroscopy and scanning electron microscopy (SEM) images. Cytotoxicity tests indicated a good tolerance of the cells to the biomaterial. The in vivo tissue response of all studied materials showed normal inflammatory pattern, characterized by a reduction of polymorphonuclear leukocytes and an increase in mononuclear leukocytes over the time (p < 0.05 Kruskal-Wallis). On day 60, microscopic analysis showed regression of the chronic inflammatory process around all materials. FTIR showed no changes in chemical composition of materials due to implantation, whereas SEM demonstrated the delivery of starch in the medium. Therefore, the results of the tests performed in vitro and in vivo show that the innovative blends can further be used as biomaterials. © 2013 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater 101B: 1284-1293, 2013. Copyright © 2013 Wiley Periodicals, Inc.

In vitro analysis of shear bond strength and adhesive remnant index comparing light curing and self-curing composites

OBJETIVO: Avaliar in vitro a resistência ao cisalhamento de compósitos autopolimerizáveis (Concise e Alpha Plast) e fotopolimerizáveis (Transbond XT e Natural Ortho) utilizados na colagem de braquetes metálicos da marca Morelli, analisando o índice de adesivo remanescente (ARI) e da integridade da superfície do esmalte por meio de microscopia eletrônica de varredura (MEV). MÉTODOS: foram utilizados 40 pré-molares humanos extraídos. As raízes dos dentes foram incluídas em gesso-pedra especial, no interior de tubos de PVC usados para a confecção dos corpos de prova. Esses corpos de prova foram divididos em quatro grupos: grupo G1, braquetes associados ao compósito Concise; grupo G2, braquetes associados ao compósito Alpha Plast; grupo G3, braquetes associados ao compósito Transbond XT; e grupo G4, braquetes associados ao compósito Natural Ortho. Os grupos foram submetidos ao teste de cisalhamento em máquina universal de ensaios, a uma velocidade de 0,5mm por minuto. RESULTADOS: houve diferença estatística entre os grupos G3 e G4, sendo os valores de G4 superiores; no entanto, não foram encontradas diferenças estatisticamente significativas entre os grupos G1, G2 e G3 e G1, G2 e G4. Na análise do ARI não foram encontradas diferenças estatísticas entre os grupos, predominando escores baixos. De acordo com a análise da MEV, constatou-se o rompimento dos compósitos e a integridade do esmalte entre os grupos. CONCLUSÃO: a resistência ao cisalhamento foi satisfatória e semelhante entre os compósitos utilizados, sendo que a resina Natural Ortho apresentou-se superior à Transbond XT.

Influence of light intensity and curing cycle on microleakage of Class V composite resin restorations

O objetivo deste estudo foi determinar o efeito da polimerização gradual, mediante a utilização de aparelhos de Quartzo-Tungustênio-Halógena (QTH) e Arco de Plasma de Xenônio (PAC), no selamento marginal de restaurações classe V em resina composta com margens localizadas em dentina. Setenta e cinco incisivos bovinos receberam preparos de cavidades classe V, na raiz, com o intuito de situar as margens cavitárias em dentina. Os dentes foram divididos em cinco grupos de acordo com o método de fotoativação. As cavidades, depois de condicionadas, foram tratadas com o sistema adesivo Single Bond (3M Dental) e restauradas com a resina composta Z100 (3M Dental) pela técnica incremental. A fotoativação foi realizada para cada grupo como descrito a seguir: Grupo I: PAC pelo método de fotoativação constante: 1600mW/cm² – 3s; Grupo II: PAC pelo método de fotoativação por passos (800mW/cm² – 2s, subindo automaticamente para 1600mW/cm² – 4s); Grupo III: QTH pelo método de fotoativação constante: 400 mW/cm² – 40s; Grupo IV: QTH pelo método de fotoativação em rampa: 100 a 600 mW/cm² – 15s, permanecendo a 600mW/cm² por mais 25s; Grupo V: QTH pelo método de fotoativação por pulso: 200 mW/cm² – 3s, tempo de espera de 3min.e a seguir 600mW/cm² – 30s. Os dentes foram armazenados em água destilada a 37ºC por 30 dias e então submetidos à ciclagem térmica, por 500 ciclos à 5 ºC e 55 ºC. Os ápices dos dentes foram selados com resina composta e os dentes foram cobertos com duas camadas de esmalte para unha, antes da sua imersão em fucsina básica a 0,5%. Os dentes foram seccionados e os cortes foram escaneados para avaliação da área infiltrada por corante por um programa de computador (Image Tools). Os cortes foram também visualizados com lupa para a determinação do grau de penetração do corante na interface dente-restauração por escores. Diferenças estatisticamente significantes foram observadas entre os grupos quanto ao grau e à área de penetração de corante (p < 0,05). Os grupos I e II apresentaram valores significantemente mais altos de infiltração e penetração do corante que os grupos III, IV e V. Em conclusão, o uso da fonte de PAC, no modo constante e por passos, resultou em valores significantemente maiores de infiltração marginal quando comparados com a intensidade de luz média emitida pelos aparelhos de QTH. Os métodos de fotoativação por pulso, rampa e continuo com a fonte de QTH resultaram num grau similar de microinfiltração.

Production and evaluation of recycled polymers from açaí fibers

The possibility of recycling and the favorable mechanical properties of the products have encouraged the study and production of thermoplastic composites from natural fibrous waste. Açaí (cabbage palm) fiber, which is removed from the seed, has been slightly investigated, as compared to what is already known about the fruit pulp. In this study, the influence of açaí fiber as an element of reinforcement in recycled everyday usage thermoplastics using simple, low cost methodology was evaluated. Recycled matrixes of high impact polystyrene and polypropylene were molded by hot compression from which the fiber composites were obtained. The FTIR technique showed that the process was efficient in preventing degradation of the açaí fibers. The influence of the fiber on the mechanical behavior of the recycled matrixes was investigated by microscopic images of compression and impact tests. The results showed better impact performance for the fiber combined with the polymeric matrixes.

Structural and optical properties of brominated plasma polymers

Novel brominated amorphous hydrogenated carbon (a-C:H:Br) films were produced by the plasma polymerization of acetylene-bromoform mixtures. The main parameter of interest was the degree of bromination, which depends on the partial pressure of bromoform in the plasma feed, expressed as a percentage of the total pressure, R-B. When bromoform is present in the feed, deposition rates of up to about 110 nm min(-1) may be obtained. The structure and composition of the films were characterized by Transmission Infrared Reflection Absorption Spectroscopy (IRRAS) and X-ray Photo-electron Spectroscopy (XPS). The latter revealed that films with atomic ratios Br:C of up to 0.58 may be produced. Surface contact angles, measured using goniometry, could be increased from similar to 63 degrees (for an unbrominated film) to similar to 90 degrees for R-B of 60 to 80%. Film surface roughness, measured using a profilometer, does not depend strongly on R-B. Optical properties the refractive index, n, absorption coefficient, alpha(E), where E is the photon energy, and the optical gap, E-g, were determined from film thicknesses and data obtained by Transmission Ultraviolet-Visible Near Infrared Spectroscopy (UVS). Control of n was possible via selection of R-B. The measured optical gap increases with increasing F-BC, the atomic ratio of Br to C in the film, and semi-empirical modeling accounts for this tendency. A typical hardness of the brominated films, determined via nano-indentation, was similar to 0.5 GPa. (C), 2013 Elsevier B.V. All rights reserved.

Light-curing Time and Aging Effects on the Nanomechanical Properties of Methacrylate- and Silorane-based Restorations

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Time reduction of light curing: Influence on conversion degree and microhardness of orthodontic composites

Introduction: The aim of this study was to assess the influence of curing time and power on the degree of conversion and surface microhardness of 3 orthodontic composites. Methods: One hundred eighty discs, 6 mm in diameter, were divided into 3 groups of 60 samples according to the composite used-Transbond XT (3M Unitek, Monrovia, Calif), Opal Bond MV (Ultradent, South Jordan, Utah), and Transbond Plus Color Change (3M Unitek)-and each group was further divided into 3 subgroups (n = 20). Five samples were used to measure conversion, and 15 were used to measure microhardness. A light-emitting diode curing unit with multiwavelength emission of broad light was used for curing at 3 power levels (530, 760, and 1520 mW) and 3 times (8.5, 6, and 3 seconds), always totaling 4.56 joules. Five specimens from each subgroup were ground and mixed with potassium bromide to produce 8-mm tablets to be compared with 5 others made similarly with the respective noncured composite. These were placed into a spectrometer, and software was used for analysis. A microhardness tester was used to take Knoop hardness (KHN) measurements in 15 discs of each subgroup. The data were analyzed with 2 analysis of variance tests at 2 levels. Results: Differences were found in the conversion degree of the composites cured at different times and powers (P < 0.01). The composites showed similar degrees of conversion when light cured at 8.5 seconds (80.7%) and 6 seconds (79.0%), but not at 3 seconds (75.0%). The conversion degrees of the composites were different, with group 3 (87.2%) higher than group 2 (83.5%), which was higher than group 1 (64.0%). Differences in microhardness were also found (P < 0.01), with lower microhardness at 8.5 seconds (35.2 KHN), but no difference was observed between 6 seconds (41.6 KHN) and 3 seconds (42.8 KHN). Group 3 had the highest surface microhardness (35.9 KHN) compared with group 2 (33.7 KHN) and group 1 (30.0 KHN). Conclusions: Curing time can be reduced up to 6 seconds by increasing the power, with a slight decrease in the degree of conversion at 3 seconds; the decrease has a positive effect on the surface microhardness.