Abstract This in vitro study synthesized hybrid nanofibers embedded in graphene oxide (GO) and incorporated them into experimental resin composite monomers to evaluate their physical-mechanical properties. Inorganic-organic hybrid nanofibers were produced with precursor solutions of 1% wt. GO-filled Poly (d,l-lactide, PLA) fibers and scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS) characterized the morphology and chemical composition of the spun fibers. Resin composite monomers were developed and a total of 5% nanofibers were incorporated into the experimental materials. Three groups were developed: G1 (control resin monomers), G2 (resin monomers/PLA nanofibers), and G3 (resin monomers/inorganic-organic hybrid nanofibers). Contact angle (n=3), flexural strength (n=22), elastic modulus (n=22), and Knoop hardness (n=6) were evaluated. The mean of the three indentations was obtained for each sample. The normality of data was assessed by QQ Plot with simulated envelopes and analyzed by Welch's method (p<0.05). Overall, SEM images showed the regular shape of nanofibers but were non-aligned. Compositional analysis from EDS (n=6) revealed the presence of carbon and oxygen (present in GO composition) and Si from the functionalization process. The results of contact angle (°) and hardness (Kg/mm2) for each group were as follow, respectively: G1 (59.65±2.90; 37.48±1.86a), G2 (67.99±3.93; 50.56±1.03b) and G3 (62.52±7.40; 67.83±1.01c). The group G3 showed the highest Knoop hardness values (67.83 kg/mm2), and the flexural strength of all groups was adversely affected. The experimental resin composite composed of hybrid nanofibers with GO presented increased hardness values and hydrophilic behavior.

Resumo Este estudo in vitro sintetizou nanofibras híbridas embebidas em óxido de grafeno (GO), incorporando-as à uma resina composta experimental de monômeros para avaliar suas propriedades físico-mecânicas. Nanofibras híbridas inorgânica-orgânicas foram produzidas com soluções precursoras de fibras poli (d, l-lactídeo, PLA) preenchidas com GO a 1% em peso e microscopia eletrônica de varredura (MEV) e espectroscopia de raio-X de energia dispersiva (EDS) caracterizaram a morfologia e composição química das fibras. Monômeros de resina composta foram desenvolvidos e um total de 5% de nanofibras foi incorporado aos materiais experimentais. Três grupos foram desenvolvidos: G1 (monômeros de resina controle), G2 (monômeros de resina/ nanofibras de PLA) e G3 (monômeros de resina/nanofibras híbridas inorgânico-orgânicas). Ângulo de contato (n=3), resistência à flexão (n=22), módulo de elasticidade (n=22) e dureza Knoop (n=6) foram avaliados. A média das três endentações foi obtida para cada amostra. A normalidade dos dados foi avaliada pelo QQ Plot com envelopes simulados e analisada pelo método de Welch (p<0,05). No geral, as imagens de MEV mostraram forma regular de nanofibras, mas não alinhadas. A análise composicional de EDS (n=6) revelou a presença de carbono e oxigênio (presentes na composição do GO) e Si resultante do processo de funcionalização. Os resultados do ângulo de contato (°) e dureza (Kg/mm2) para cada grupo foram os seguintes, respectivamente: G1 (59,65±2,90; 37,48±1,86a), G2 (67,99±3,93; 50,56±1,03b) e G3 (62,52±7,40; 67,83±1,01c). G3 apresentou os maiores valores de dureza Knoop (67,83 kg/mm2), e a resistência à flexão de todos os grupos foi prejudicada. A resina composta experimental composta por nanofibras híbridas com GO apresentou maiores valores de dureza e comportamento hidrofílico.

Resumo O presente estudo teve como objetivo avaliar as propriedades de polimerização de materiais bulk-fill (baixa e alta viscosidade) utilizando luz contínua de alta intensidade e fotoativação intermitente em relação ao estresse de contração de polimerização e grau de conversão (DC). As seguintes resinas compostas Bulk-fill e nanohíbridas convencionais foram avaliadas: Filtek Z350XT Flow (3M/ESPE), SureFil SDR Flow (Dentsply), Filtek Bulk Fill Flow (3M/ESPE), Filtek Z350XT (3M/ESPE) e Filtek Bulk Fill Posterior (3M/ESPE). Um dispositivo de LED (DB 685, Dabi Atlante) foi utilizado nos dois protocolos: fotoativação contínua e intermitente contínua (ciclos de liga e desliga) com exposição idêntica (14 J/cm2). A tensão de contração de polimerização (n=6) foi avaliada através da inserção de um incremento único de 12 mm3 entre duas placas de aço inoxidável (6×2 mm) adaptadas a uma Máquina de Ensaio Universal (UTM), em tempos diferentes. As medições foram registradas após a fotoativação. O grau de conversão foi avaliado por FTIR-ATR (n=5). Os dados foram analisados pelos testes ANOVA a três fatores e teste de Tukey (α=0,05). A resina Bulk Fill Posterior apresentou maiores valores de tensão de contração quando fotoativadas com a técnica intermitente (p<0,05). A fotoativação intermitente aumentou o grau de conversão nas resinas bulk-fill de baixa viscosidade (p<0,05). Portanto, o uso de fotoativação modulada (intermitente) deve ser indicado com cautela, uma vez que seu uso pode influenciar a tensão de contração e o grau de conversão dos compósitos, o que varia de acordo com as formulações da resina.

Abstract This study aimed to evaluate the polymerization properties of bulk-fill materials (low and high-viscosity) by using high-intensity continuous light and intermittent photo-activation in terms of polymerization shrinkage stress and degree of conversion (DC). The following Bulk-fill and Conventional nanofilled resin composites were evaluated: Filtek Z350XT Flow (3M/ESPE), SureFil SDR Flow (Dentsply), Filtek Bulk Fill Flow (3M/ESPE), Filtek Z350XT (3M/ESPE) and Filtek Bulk Fill Posterior (3M/ESPE). A LED device (DB 685, Dabi Atlante) was used for both protocols: continuous uniform and intermittent photo-activation (light-on and light-off cycles) with identical radiant exposure (14 J/cm2). The polymerization shrinkage stress (n=6) was evaluated by inserting a single increment of 12 mm3 between two stainless steel plates (6×2 mm) adapted to a Universal Testing Machine (UTM), at different times. Measurements were recorded after photo-activation. The degree of conversion was evaluated by Fourier transformed infrared spectroscope (FTIR) with an attenuated total reflectance (ATR) accessory (n=5). Data were analyzed by three-way ANOVA and Tukey’s HSD (α=0.05) tests. Bulk Fill Posterior presented higher shrinkage stress values when photo-activated with the intermittent technique (p<0.05). The intermittent photo-activation increased the degree of conversion for the low-viscosity bulk-fills (p<0.05). Therefore, the use of modulated photo-activation (intermittent) must be indicated with caution since its use can influence the shrinkage stress and degree of conversion of composites, which varies according to the resin formulations.

Abstract We assessed the effect of a new coating material based on resin-modified glass-ionomer with calcium (Ca) in inhibiting the demineralization of underlying and adjacent areas surrounding caries-like lesions in enamel. The measures used were surface hardness (SH) and cross-sectional hardness (CSH). Thirty-six bovine enamel specimens (3 × 6 × 2 mm) were randomly allocated into three groups (n = 12): No treatment (NT); resin-modified glass-ionomer with Ca (Clinpro XT Varnish, 3M ESPE) (CL), and fluoride varnish (Duraphat, Colgate) (DU). The specimens were subjected to alternated immersions in demineralizing (6 h) and remineralizing solutions (18 h) for 7 days. SH measurements were conducted at standard distances of 150, 300, and 450 µm from the treatment area. CSH evaluated the mean hardness profile over the depth of the enamel surface and at standard distances from the materials. The energy-dispersive X-ray spectroscopy analysis was conducted to evaluate the demineralization bands created on the sublayer by % of calcium (Ca), phosphorus (P), and fluoride (F). Ca/P weight ratio was also calculated. Based on SH and CSH measurements, there was no difference between groups at the distances 150 µm (p = 0.882), 300 µm (p = 0.995), and 450 µm (p = 0.998). Up to 50 µm depth (at 150 µm from the treatment area), CL showed better performance than DU ( p< 0.05). NT presented higher loss of Ca and P than CL and DU (p < 0.05). There was no significant difference in the % of F ion among the three groups. The new coating material was similar to F varnish in attenuating enamel demineralization.

Abstract This study evaluated the effect of adding the hydrophobic monomer 1,12 dodecanediol dimethacrylate (DDDMA) to experimental sealants with and without thermocycling on degree of conversion (DC), water sorption (WS), water solubility (WSB), color stability (ΔE), and micro-shear bond strength (μSBS). Five experimental and one commercially available sealant (Bisco - BIS) were tested. The experimental sealants were formulated by mixing different percentages of DDDMA monomers and urethane dimethacrylate (UDMA). The photoinitiator system was composed by camphorquinone (CQ) and tertiary amine 4-ethyl benzoate dimetilamiono (EDBA). Ethanol was used as a solvent. The experimental groups were named sequentially according to the monomeric content (DDDMA/UDMA): S40/40 (40/40), S50/30 (50/30), S60/20 (60/20), S70/10 (70/10) and S80/0 (80/0). Data were analyzed separately by one-way ANOVA, followed by Tukey’s test (p<0.05). The values of DC ranged from 94.59% (S40/40) to 54.02% (S80/10). BIS showed the highest WS value (p<0.05) and S40/40, S50/30, S60/20 and S80/0 showed the lowest WS values of all tested sealants. WSB values ranged from 7.88 µg/mm3 (BIS) to 13.27 µg/mm3 (S70/10). The highest ΔE value was 11.05±2.88 for BIS and the highest μSBS value was found for S60/20. No significant difference was observed in bond strength between sealants and bovine enamel after thermocycling. Adding DDDMA to the composition of surface sealants can improve its performance, once the monomer increased the degree of conversion and the color stability.