RESUMO

Advanced Polymerization System (APS) technology in a commercial composite resin enables reduction of the concentration of camphorquinone without altering composite physicochemical properties. AIM: The aim of this study was to evaluate the degree of conversion and mechanical properties of a commercial composite with an advanced polymerization system (APS) and compare it to other composites that do not use this system. MATERIALS AND METHOD: Five groups were analyzed. Group 1 (VT: Vittra APS - FGM); G2 (AU: Aura - SDI); G3 (ES: Quick Sigma Stelite - TOKOYAMA); G4 (FZ: Filtek Z350 XT - 3M ESPE); G5 (OP: Opallis -FGM). Degree of conversion (DC, n=3) was analyzed immediately and after 24h by analysis with FTIR spectroscopy. For Knoop hardness (KHN, n=3), 5 indentations were made at the top and bottom of specimens 2 mm thick. Flexural strength (FS, n=10) was determined by the three-point method in a universal testing machine. Polymerization stress (PS) was determined by light-curing the material (1.0 mm high) between polymethylmethacrylate rods in a universal testing machine. Light curing was performed with a Valo Cordless LED (1,000 mW/cm2 x 20 s: 20J). The results were analyzed using ANOVA and complemented by Tukey's test (α=0.05). RESULTS: The highest DC values (immediate and 24h after) were observed for VT and OP resins, followed by FZ, AU and ES. FZ (top and bottom) had the highest KHN values, similar to VT top. AU, ES, OP and VT had statistically different KHN between their top and bottom surfaces. The highest RF values were observed for FZ, followed by OP/VT, ES and AU. The highest TP values were observed for FZ, OP and VT. CONCLUSION: The Vittra APS resin with a new polymerization system presents satisfactory performance for the parameters evaluated.

A tecnologia Advanced Polymerization System (APS) presente em uma resina composta comercial permite reduzir a concentração de canforoquinona sem alterar as propriedades físico-químicas do compósito. Objetivo: o objetivo deste estudo foi avaliar o grau de conversão e as propriedades mecânicas de um compósito comercial com sistema avançado de polimerização (SAP) e comparálo com outros compósitos que não utilizam esse sistema. Materiais e Método: cinco grupos foram analisados. Grupo 1 (VT: Vittra APS - FGM); G2 (AU: Aura ­ SDI); G3 (ES: Quick Sigma Stelite ­ TOKOYAMA); G4 (FZ: Filtek Z350 XT ­ 3M ESPE); G5 (OP: Opallis -FGM). O grau de conversão (GC, n=3) foi analisado imediatamente e após 24h através da análise com espectroscopia FTIR; para dureza Knoop (DK, n=3), foram feitas 5 indentações no topo e na base de corpos de prova de 2 mm de espessura; para determinar a resistência à flexão (RF, n=10), o método de três pontos foi realizado em uma máquina universal de ensaios; a tensão de polimerização (TP) foi determinada pela fotopolimerização do material (1,0 mm de altura) entre hastes de polimetilmetacrilato em uma máquina de teste universal. A fotopolimerização foi realizada com um Valo Cordless LED (1.000 mW/cm2 x 20 s: 20J). Os resultados foram analisados por ANOVA e complementados pelo teste de Tukey (α=0,05). Resultados: os maiores valores de GC (imediato e 24h após) foram observados para as resinas VT e OP, seguidas de FZ, AU e ES. A resina FZ (superior e inferior) apresentou os maiores valores de DK, semelhante ao VT superior. As resinas AU, ES, OP e VT apresentaram DK estatisticamente diferente entre suas superfícies de topo e base. Os maiores valores de RF foram observados para FZ, seguido de OP/VT, ES e AU. Os maiores valores de TP foram observados para FZ, OP e VT. Conclusão: com base nos resultados, pode-se concluir que a resina Vittra APS com um novo sistema de polimerização apresenta desempenho satisfatório para os parâmetros avaliados.

RESUMO

ABSTRACT Advanced Polymerization System (APS) technology in a commercial composite resin enables reduction of the concentration of camphorquinone without altering composite physicochemical properties. Aim: The aim of this study was to evaluate the degree of conversion and mechanical properties of a commercial composite with an advanced polymerization system (APS) and compare it to other composites that do not use this system. Materials and Method: Five groups were analyzed. Group 1 (VT: Vittra APS - FGM); G2 (AU: Aura - SDI); G3 (ES: Quick Sigma Stelite - TOKOYAMA); G4 (FZ: Filtek Z350 XT - 3M ESPE); G5 (OP: Opallis -FGM). Degree of conversion (DC, n=3) was analyzed immediately and after 24h by analysis with FTIR spectroscopy. For Knoop hardness (KHN, n=3), 5 indentations were made at the top and bottom of specimens 2 mm thick. Flexural strength (FS, n=10) was determined by the three-point method in a universal testing machine. Polymerization stress (PS) was determined by light-curing the material (1.0 mm high) between polymethylmethacrylate rods in a universal testing machine. Light curing was performed with a Valo Cordless LED (1,000 mW/cm2 x 20 s: 20J). The results were analyzed using ANOVA and complemented by Tukey's test (α=0.05). Results: The highest DC values (immediate and 24h after) were observed for VT and OP resins, followed by FZ, AU and ES. FZ (top and bottom) had the highest KHN values, similar to VT top. AU, ES, OP and VT had statistically different KHN between their top and bottom surfaces. The highest RF values were observed for FZ, followed by OP/VT, ES and AU. The highest TP values were observed for FZ, OP and VT. Conclusion: The Vittra APS resin with a new polymerization system presents satisfactory performance for the parameters evaluated.

RESUMO A tecnologia Advanced Polymerization System (APS) presente em uma resina composta comercial permite reduzir a concentração de canforoquinona sem alterar as propriedades físico-químicas do compósito. Objetivo: o objetivo deste estudo foi avaliar o grau de conversão e as propriedades mecânicas de um compósito comercial com sistema avançado de polimerização (SAP) e comparálo com outros compósitos que não utilizam esse sistema. Materiais e Método: cinco grupos foram analisados. Grupo 1 (VT: Vittra APS - FGM); G2 (AU: Aura - SDI); G3 (ES: Quick Sigma Stelite - TOKOYAMA); G4 (FZ: Filtek Z350 XT - 3M ESPE); G5 (OP: Opallis -FGM). O grau de conversão (GC, n=3) foi analisado imediatamente e após 24h através da análise com espectroscopia FTIR; para dureza Knoop (DK, n=3), foram feitas 5 indentações no topo e na base de corpos de prova de 2 mm de espessura; para determinar a resistência à flexão (RF, n=10), o método de três pontos foi realizado em uma máquina universal de ensaios; a tensão de polimerização (TP) foi determinada pela fotopolimerização do material (1,0 mm de altura) entre hastes de polimetilmetacrilato em uma máquina de teste universal. A fotopolimerização foi realizada com um Valo Cordless LED (1.000 mW/cm2 x 20 s: 20J). Os resultados foram analisados por ANOVA e complementados pelo teste de Tukey (α=0,05). Resultados: os maiores valores de GC (imediato e 24h após) foram observados para as resinas VT e OP, seguidas de FZ, AU e ES. A resina FZ (superior e inferior) apresentou os maiores valores de DK, semelhante ao VT superior. As resinas AU, ES, OP e VT apresentaram DK estatisticamente diferente entre suas superfícies de topo e base. Os maiores valores de RF foram observados para FZ, seguido de OP/VT, ES e AU. Os maiores valores de TP foram observados para FZ, OP e VT. Conclusão: com base nos resultados, pode-se concluir que a resina Vittra APS com um novo sistema de polimerização apresenta desempenho satisfatório para os parâmetros avaliados.

RESUMO

Abstract The objective of this study was to evaluate the effect of the exposure reciprocity law of a multi-wave light-emitting diode (LED) on the light transmittance (LT), depth of cure (DOC) and degree of conversion in-depth (DC) of a bulk fill composite. A bulk fill composite (EvoCeram® bulk fill, Ivoclar Vivadent) was photoactivated using the multi-wave LED (VALO™ Cordless, Ultradent). The LED was previously characterized using a spectrophotometer to standardize the time of exposure when using the Standard or Xtra-Power modes with the same radiant exposure of 20J/cm2. LT was evaluated through samples of the bulk fill composite every millimeter till 4 mm in-depth. DOC was evaluated according to the ISO 4049. DC of the central longitudinal cross-section from each sample of the DOC test was mapped using FT-NIR microscopy. Data were statistically analyzed according to the experimental design (α=0.05; ß=0.2). The radiant exposure in the violet wavelength range for Standard and Xtra-Power was 4.5 and 5.0 J/cm2, respectively; for the blue wavelength range the radiant exposure for Standard and Xtra-Power was 15.5 and 15.0 J/cm2, respectively. There was no statistical difference in the DOC using Standard or Xtra-Power light-curing modes, but the DOC was lower than the claimed by the manufacturer (4 mm). The DC was not significantly affected by the light-curing mode up to 4 mm in depth (p>0.05). According to exposure reciprocity law, the reduction in exposure time using the same radiant exposure did not affect the depth of cure of the bulk fill composite.

Resumo O objetivo deste estudo foi avaliar o efeito da lei de reciprocidade de um diodo emissor de luz (LED) multi-wave na transmitância de luz (LT), profundidade de cura (DOC) e grau de conversão em profundidade (DC) de um compósito bulk fill. Material e Métodos: Um compósito bulk fill (EvoCeram®, Ivoclar Vivadent) foi fotoativado utilizando um LED multi-wave (VALO ™ Cordless, Ultradent). O LED foi previamente caracterizado usando um espectrofotômetro para padronizar o tempo de exposição utilizando os modos Standard ou Xtra-Power com a mesma dose de energia de 20 J/cm 2. A LT foi avaliada através de amostras do compósito bulk fill a cada milímetro até 4 mm de profundidade. O DOC foi avaliado de acordo com a ISO 4049. O DC foi realizado em forma de mapeamento da seção transversal longitudinal central de cada amostra do teste de DOC utilizando microscopia FT-NIR. Os dados foram analisados estatisticamente de acordo com o delineamento experimental (α=0,05; ß=0,2). A exposição radiante na faixa de comprimento de onda violeta para os modos Standard e Xtra-Power foi de 4,5 e 5,0 J/cm2, respectivamente; e para a faixa de comprimento de onda azul, a exposição radiante para os modos Standard e Xtra-Power foi de 15,5 e 15,0 J/cm2, respectivamente. Não houve diferença estatística no DOC utilizando os modos de fotopolimerização Standard ou Xtra-Power, mas o DOC foi menor do que o reivindicado pelo fabricante (4 mm). O DC não foi afetado significativamente pelo modo de fotopolimerização até 4 mm de profundidade (p>0,05). De acordo com a lei de reciprocidade da exposição, a redução no tempo de exposição utilizando a mesma exposição radiante não afetou a profundidade de cura do compósito bulk fill.

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Abstract The aim in this study was to evaluate the influence of different ratio of camphorquinone/tertiary amine concentration on the flexural strength (FS), elastic modulus (EM), degree of conversion (DC), yellowing (YL), water sorption (WS) and water solubility (WSL) of experimental composites. Thus, acrylate blends were prepared with different camphorquinone (CQ) and amine (DABE) concentrations and ratios by weight: (CQ/DABE%): 0.4/0.4% (C1), 0.4/0.8% (C2), 0.6/0.6% (C3), 0.6/1.2% (C4), 0.8/0.8% (C5), 0.8/1.6% (C6), 1.0/1.0% (C7), 1.0/2.0% (C8), 1.5/1.5% (C9), 1.5/3.0% (C10). For the FS and EM, rectangular specimens (7x2x1 mm, n=10) were photo-activated by single-peak LED for 20 s and tested at Instron (0.5 mm/min). Then, the same specimens were evaluated by FTIR for DC measurement. For YL, disks (5x2 mm, n=10) were prepared, light-cured for 20 s and evaluated in spectrophotometer using the b aspect of the CIEL*a*b* system. For WS and WSL, the volume of the samples was calculated (mm³). For WS and WSL, composites disks (5x0.5 mm, n=5) were prepared. After desiccation, the specimens were stored in distilled water for 7 days and again desiccated, in order to measure the WS and WSL. Data were submitted to one-way ANOVA and Tukey's test (5%). The groups C8, C9 and C10 showed higher DC, EM and YL means, compared to other composites. Therefore, the FS and WS values were similar among all groups. Also, C1, C2 and C3 presented higher WSL in 7 days, compared to other composites. In general, higher concentrations of camphorquinone promoted higher physical-mechanical properties; however, inducing higher yellowing effect for the experimental composites

Resumo O objetivo foi avaliar a influência da concentração e proporção de canforoquinona (CQ)/amina terciária (DABE) na resistência à flexão (RF), módulo flexural (MF), grau de conversão (GC), amarelamento (AM), sorpção (SA) e solubilidade em água (SL) de compósitos experimentais. Blendas acrilatas foram preparadas com diferentes concentrações e proporções de CQ/DABE em peso, como segue: (CQ/DABE%): 0,4/0,4% (C1); 0,4/0,8% (C2); 0,6/0,6% (C3); 0,6/1,2% (C4); 0,8/0,8% (C5); 0,8/1,6% (C6); 1,0/1,0% (C7); 1,0/2,0% (C8); 1,5/1,5% (C9); 1,5/3,0% (C10). Para RF e MF, espécimes retangulares (7x2x1 mm, n=10) foram fotoativados com LED de pico único (Radii Cal) por 20 s e testados em máquina Instron (0,5 mm/min). Após, o GC dos mesmos espécimes (fragmentos) foi mensurado por FTIR. Para AM, discos de compósito (5x2 mm, n=10) foram preparados, fotoativados por 20 s e imediatamente avaliados em espectrofotômetro, considerando o aspecto b do sistema CIEL*a*b*. Para SA e SL, discos de compósito (5x0,5 mm, n=5) foram preparados e seus volumes calculados (mm³). Após desidratação, as amostras foram pesadas e armazenadas em água destilada por 7 dias, pesadas e novamente desidratadas e pesadas, para se calcular o SA e SL. Os dados foram submetidos a one-way ANOVA e teste de Tukey (5%). Os grupos C8, C9 e C10 mostraram maior GC, MF e AM, comparado aos outros grupos. No entanto, RF e SA foram similares entre todos os grupos. Ainda, C1, C2 e C3 apresentaram maior SL em 7 dias comparado aos outros grupos. Em geral, maiores concentrações de CQ promoveram melhores propriedades físico-mecânicas; no entanto, levaram ao maior amarelamento dos compósitos.

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OBJECTIVES: To investigate the influence of camphorquinone (CQ):amine ratio on the degree of CC conversion (DC) and color stability of experimental dental composites formulated with different co-monomer viscosities, indirectly determined by variations in the co-monomer ratios. MATERIALS AND METHODS: Experimental composites were formulated in two different BisGMA:TEGDMA molar ratios (50:50 and 70:30). Viscosities were assessed with a viscometer. For each composite formulation, four different CQ:amine ratios were added: 1:1, 1:2, 1:3 or 1:4 mol%. Materials were loaded with 40 wt% of silanized glass particles. DC was determined by Fourier-transformed infrared spectroscopy with attenuated reflectance mode (ATR-FTIR). A spectrophotometer was used to measure the CIE L*a*b* color coordinates 24h after polymerization and after 2 months stored in water. Color changes (ΔE) were calculated. Data were statistically analyzed using analyses of variance (ANOVA), Tukey's and Student-t tests (α=0.05). RESULTS: The 50:50 BisGMA:TEGDMA co-monomer showed lower viscosity than 70:30. DC was affected by CQ:amine ratio, and not by the co-monomer viscosity, but the interaction between these two factors was significant. a* and b* coordinates were dependent on CQ:amine or BisGMA:TEGDMA ratios, while L* was not. b* values were directly related to the amount of amine in the formulation, regardless of co-monomer viscosity. ΔE was dependent on the amount of amine, but not on the viscosity of the material. SIGNIFICANCE: DC was influenced by the CQ:amine ratio. The influence of viscosity on DC was dependent on the CQ:amine ratio and exhibited distinguished behavior. a* and b* coordinates were affected by CQ:amine and BisGMA:TEGDMA ratios. The color change (ΔE) was affected by CQ:amine ratio, but not by viscosity.

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OBJECTIVES: To evaluate conversion, bulk mechanical properties and camphorquinone (CQ) consumption in methacrylate resins, comprising a range of overall initiator concentrations and CQ/amine ratios. METHODS: BisGMA (Bisphenol-A glycidyl dimethacrylate), TEGDMA (triethyleneglycol dimethacrylate) and UDMA (urethane dimethacrylate) were mixed at a 1:1:1 molar ratio. CQ was used as the visible light photosensitizer, in combination with EDMAB (Ethyl p-dimethylamino benzoate), at 3:1, 2:1, 1:1, 1:2 and 1:3 weight ratios, at 0.5, 1.0, 1.5, 2.0 and 3.0 wt% overall initiator concentration. Butylhydroxytoluene was added at 0.05 wt% as an inhibitor. Unfilled resins were photoactivated with a dental light source (VIP Jr, Bisco) for 60 s at 600 mW/cm(2). Flexural strength/modulus were assessed in 2×1×10 mm bars, tested in three-point bending. Degree of conversion was assessed at the bottom of the same specimens using FT-RAMAN. CQ consumption was measured using a UV-vis spectrometer. Data were analyzed with two-way ANOVA/Tukey test (α=5%). RESULTS: Lower conversion and inferior mechanical properties were observed with lower overall initiator concentrations and higher amine/CQ ratios. The lowest overall initiator concentration (0.5%) presented the statistically lowest conversion/properties results, except for the 1:3 amine/CQ ratio. For overall concentrations equal or greater to 1.5%, the amine/CQ ratio did not influence conversion or mechanical properties. CQ consumption was less efficient for the highest overall initiator concentrations and lower amine/CQ ratios. CLINICAL RELEVANCE: Above 1.5 wt% overall initiator concentration, the conversion and general mechanical properties were independent of the initiator concentration. Therefore, there seems to be no benefit to increasing the initiator concentration above that level. At higher camphorquinone concentrations, light transmission and photosensitizer consumption becomes impaired, which could lead to decreased depth of cure and yellowing of the restoration.

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OBJECTIVES: This study evaluated the performance of phenylbis (2,4,6-trimethylbenzoyl)-phosphine oxide (BAPO) as an alternative photoinitiator in the polymerization kinetics (PK), flexural strength (σ) and elastic modulus (E) of a model dental resin. METHODS: A monomer mixture based on Bis-GMA and TEGDMA was used as model dental resin. Initially a screening was performed to evaluate BAPO concentrations (0.125, 0.25, 0.50, 1, 2, and 4 mol%). Photoinitiator systems were formed with the combination of camphorquinone (CQ), ethyl-dimethylamino benzoate (EDAB), diphenyliodonium hexafluorophosphate (DPIHFP), and BAPO. Groups with unitary photoinitiator systems (BAPO and CQ), binary (BAPO+EDAB, BAPO+DPIHFP and CQ+EDAB), ternary (BAPO+CQ+EDAB, BAPO+CQ+DPIHFP, BAPO+EDAB+DPIHFP and CQ+EDAB+DPIHFP) and quaternary (BAPO+CQ+EDAB+DPIHFP) were formulated for evaluation. Real-time Fourier transform infrared spectroscopy was used to investigate the PK and test mini-bending to evaluate σ and E. RESULTS: When only CQ was used, a slow polymerization reaction was observed and a lower monomer conversion. When only BAPO was used as photoinitiator an increase in the polymerization rate was observed and conversion was higher than CQ+EDAB. The ternary system (BAPO+EDAB+DPIHFP) showed the highest polymerization and conversion rate, in short photo-activation time. SIGNIFICANCE: BAPO it is a potential photoinitiator for the photopolymerization of dental materials.

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OBJECTIVES: The aim of this study was to formulate materials with high color stability and reduced degradation by using photoinitiator systems derived from phosphine oxides alternative to the traditional camphorquinone (CQ)/amine system. METHODS: Materials were formulated with the monomers BisGMA and TEGDMA as organic matrix. The photoinitiators tested were CQ+amine (EDMAB), phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide (BAPO), BAPO+EDMAB, diphenyl(2,4,6-trimethylbenzoyl)-phosphine oxide (TPO) and TPO+EDMAB. A 60% mass of silanated glass filler particles was added. Degree of CC conversion was evaluated by Fourier-transformed infrared spectroscopy 10min after photopolymerization. The color properties were evaluated by a digital spectrophotometer, applying the CIELab parameters, either before photoactivation, immediately after photoactivation, 24h after dry storage, and one month after water immersion. Water sorption and solubility were assessed by mass gain or loss after storage in water for 30 days. Data were analyzed using ANOVA and Tukey's test (5%). RESULTS: Degree of conversion did not differ statistically among all the tested formulations. Regarding color, only groups with TPO presented satisfactory color stability after one month of water storage (ΔE<3.3). Water sorption and water stability did not differ among the groups. CONCLUSIONS: Degree of conversion, water sorption and water solubility did not differ among all the tested groups. The TPO-based groups were the only materials with satisfactory color stability after one month of water storage. CLINICAL SIGNIFICANCE: The use of a photoinitiator system containing TPO might improve the color stability of resin composites compared with the traditional CQ/amine system while attaining similar physico-chemical properties for the composite.

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OBJECTIVE: The aim of this study was to evaluate the influence of photoinitiator concentration on marginal and internal adaptation of composites photocured by modulated methods. MATERIALS AND METHODS: Composites based on BisGMA/triethylene glycol dimethacrylate and 65 wt% of filler were prepared with different concentrations of camphorquinone/amine (C1-0.5%, C2-1%, C3-1.5%). Cavities were prepared (3 mm × 3 mm × 2 mm) on the buccal surface of 120 bovine incisors and the adhesive system Adper Single Bond 2 was applied following manufactures instruction. Specimens were then distributed according to type of composite (C1, C2, C3) and photoactivation method (high-intensity - 750 mW/cm(2) for 40 s; low intensity - 150 mW/cm(2) for 200 s; soft-start - 150 mW/cm(2) for 10 s + 750 mW/cm(2) for 38 s; pulse-delay - 150 mW/cm(2) for 10 s + 3 min dark + 750 mW/cm(2) for 38 s). Superficial and internal margins were analyzed by scanning electron microscopy, using the epoxy replica technique. The length of gaps was expressed as a percentage of the total length of the margins. Data were submitted to two-way analysis of variance and Tukey's test (α =0.05). RESULTS: Modulated curing methods did not influence gap formation regarding both superficial and internal adaptation. The composite with the lower initiator concentration (C1) presented higher gap formation when compared with those with higher concentrations (C2 and C3). CONCLUSION: Modulated photoactivation methods did not reduce gap formation for the experimental composite restorations evaluated. However, higher photoinitiator concentrations promote better marginal seal.