Mechanical Properties of Experimental Composites with Different Photoinitiator.

OBJECTIVE: The effect of different photoinitiators on mechanical properties of experimental composites was evaluated. MATERIALS AND METHODS: Resin composites were formulated by using a blend of bisphenol A-glycidyl and triethylene glycol (50/50 wt%) dimethacrylate monomers, and 65 wt% of barium aluminium silicate and silica filler particles. Photoinitiators used were 0.2% camphorquinone (CQ) and 0.8% co-initiator (DMAEMA); 0.2% phenyl-propanedione and 0.8% DMAEMA; 0.1% CQ + 0.1% phenyl propanedione and 0.8% DMAEMA; 0.42% mono(acyl)phosphine oxide (MAPO); and 0.5% bis(acyl)phosphine oxide (BAPO). Specimens (n = 10) were light cured by using a multiple-emission peak light-emitting diode for 20 seconds at 1,200 mW/cm2 of irradiance and Knoop hardness and plasticization, depth of cure, flexural strength, and elastic modulus were evaluated. Data were statiscally analyzed at significance level of α = 5%. RESULTS: Experimental composites containing MAPO and BAPO photoinitiators showed the highest values of flexural strength, elastic modulus, top surface hardness, and lower hardness reduction caused by alcohol compared with CQ. Composites containing CQ and PPD showed similar results, except for depth of cure and hardness of bottom surface. CONCLUSION: BAPO and MAPO showed higher flexural strength, elastic modulus, hardness on top surface, and lower polymer plasticization to CQ.

The effect of hydrofluoric acid and resin cement formulation on the bond strength to lithium disilicate ceramic.

To investigate how the hydrofluoric acid (HF) concentrations applied to a lithium disilicate glass-ceramic (EMX) affects the surface morphology and microtensile bond strength (µTBS) of ceramics to dentin, using light-cured resin cements with or without UDMA. Sixty-three EMX square ceramic blocks were etched for 20 seconds using different HF concentrations (1%, 5% and 10%) and luted to dentin using two types of resin cement combinations: BisGMA/TEGDMA and BisGMA/TEGDMA/UDMA (n = 10). Each bonded EMX-dentin block was sectioned to obtain 1 mm2 sticks for µTBS evaluation. Half of the sticks were tested after 24 hours and the other half was assessed after 6 months of water storage. Data were statistically assessed using split-plot three-way ANOVA and multiple comparisons were performed using the Tukey's post hoc test (α = 0.05). One EMX sample from each HF concentration was analyzed using field-emission scanning electron microscope (FE-SEM) to characterize the etching pattern. According to the FE-SEM images, increasing the concentration of HF from 1 to 5 and then to 10% led to increased removal of glassy matrix and greater exposure of lithium disilicate crystals. The 10% HF concentration yielded higher µTBS when compared to 1% for BisGMA/TEGDMA formulation (p < 0.05); whereas HF 1% and 5% showed similar µTBS values when compared to 10% HF for BisGMA/TEGDMA/UDMA resin matrix (p > 0.05) at both storage times. Water aging decreased the µTBS values (p < 0.05), except when 10% HF was associated with BisGMA/TEGDMA resin cement. Resin cement formulation and hydrofluoric acid concentrations can interfere with the immediate and long-term glass-ceramic bond strength to dentin.

Influence of light-curing unit on the network structure and mechanical properties of model resin cements containing diphenyliodonium compared with a commercial reference.

OBJECTIVE: To evaluate the effects of dyphenyliodonium hexafluorophosphate (DPI) on crosslink density (CLD), flexural strength (FS), and flexural modulus (FM) of a light-cured experimental resin cement compared with a commercial dual-cured cement. MATERIALS AND METHODS: Bis-GMA combined with TEGDMA (50-50%) was used as resin matrix. Silanated barium-aluminum-silica glass was used as inorganic filler. Camphorquinone (CQ) - 1 mol%, 2-(dimethylamino)ethyl methacrylate (DMAEMA) - 2 mol%, and two concentrations of DPI (0 or 0.5 mol%) were used as the photoinitiator system. Two light-curing units (LCUs) were used (a single-peak (Radii-Cal) and a polywave (Bluephase)). The CLD was indirectly assessed in a softening test by Knoop hardness indentation; FS and FM were measured by means of a three-point bending test. RESULTS: DPI positively influenced Knoop hardness when compared with experimental resin without DPI. The flexural strength of experimental cements was lower than that found with Variolink II. The crosslinking density (obtained by reduction of Knoop hardness) of cement with 0.5% DPI was similar to that of dual - cured Variolink II. CONCLUSIONS: DPI showed an improvement in some of the properties tested but was inferior to the commercial dual-cured resin cement. The LCUs had no influence on the flexural strength of the resin cements.

The effect of hydrofluoric acid and resin cement formulation on the bond strength to lithium disilicate ceramic

Abstract To investigate how the hydrofluoric acid (HF) concentrations applied to a lithium disilicate glass-ceramic (EMX) affects the surface morphology and microtensile bond strength (μTBS) of ceramics to dentin, using light-cured resin cements with or without UDMA. Sixty-three EMX square ceramic blocks were etched for 20 seconds using different HF concentrations (1%, 5% and 10%) and luted to dentin using two types of resin cement combinations: BisGMA/TEGDMA and BisGMA/TEGDMA/UDMA (n = 10). Each bonded EMX-dentin block was sectioned to obtain 1 mm2 sticks for μTBS evaluation. Half of the sticks were tested after 24 hours and the other half was assessed after 6 months of water storage. Data were statistically assessed using split-plot three-way ANOVA and multiple comparisons were performed using the Tukey's post hoc test (α = 0.05). One EMX sample from each HF concentration was analyzed using field-emission scanning electron microscope (FE-SEM) to characterize the etching pattern. According to the FE-SEM images, increasing the concentration of HF from 1 to 5 and then to 10% led to increased removal of glassy matrix and greater exposure of lithium disilicate crystals. The 10% HF concentration yielded higher μTBS when compared to 1% for BisGMA/TEGDMA formulation (p < 0.05); whereas HF 1% and 5% showed similar μTBS values when compared to 10% HF for BisGMA/TEGDMA/UDMA resin matrix (p > 0.05) at both storage times. Water aging decreased the μTBS values (p < 0.05), except when 10% HF was associated with BisGMA/TEGDMA resin cement. Resin cement formulation and hydrofluoric acid concentrations can interfere with the immediate and long-term glass-ceramic bond strength to dentin.

Effects of radiant exposure and wavelength spectrum of light-curing units on chemical and physical properties of resin cements.

OBJECTIVES: In this study, we evaluated the influence of different radiant exposures provided by single-peak and polywave light-curing units (LCUs) on the degree of conversion (DC) and the mechanical properties of resin cements. MATERIALS AND METHODS: Six experimental groups were established for each cement (RelyX ARC, 3M ESPE; LuxaCore Dual, Ivoclar Vivadent; Variolink, DMG), according to the different radiant exposures (5, 10, and 20 J/cm2) and two LCUs (single-peak and polywave). The specimens were made (7 mm in length × 2 mm in width × 1 mm in height) using silicone molds. After 24 hours of preparation, DC measurement was performed using Fourier transform infrared spectrometry. The same specimens were used for the evaluation of mechanical properties (flexural strength, FS; elastic modulus, E) by a three-point bending test. Data were assessed for normality, after which two-way analysis of variance (ANOVA) and post hoc Tukey's test were performed. RESULTS: No properties of the Variolink cement were influenced by any of the considered experimental conditions. In the case of the RelyX ARC cement, DC was higher when polywave LCU was used; FS and E were not influenced by the conditions evaluated. The LuxaCore cement showed greater sensitivity to the different protocols. CONCLUSIONS: On the basis of these results, both the spectrum of light emitted and the radiant exposure used could affect the properties of resin cements. However, the influence was material-dependent.

Effect of diphenyliodonium hexafluorphosphate on resin cements containing different concentrations of ethyl 4-(dimethylamino)benzoate and 2-(dimethylamino)ethyl methacrylate as co-initiators.

OBJECTIVE: The present study evaluated the influence of diphenyliodonium hexafluorphosphate (DPI) combined with two different amines [ethyl 4-(dimethylamino)benzoate (EDAB) and 2-(dimethylamino)ethyl methacrylate (DMAEMA)] on the properties of model resin cements. METHODS: A comonomer base containing a 1:1 mass ratio of 2.2-bis[4-(2-hydroxy-3-methacryloxypropoxy)phenyl]propane (bis-GMA) and triethyleneglycol dimethacrylate (TEGDMA) was obtained, after which 1mol% of camphorquinone and 0.1mol% of hydroxyl butyl toluene were added to the comonomer blend. Concentrations of co-initiators varied at 0, 0.5 or 1mol% for DPI and in 1 or 2mol% for amines (DMAEMA or EDAB). Silanated Ba-Al-Si glass (60wt%) was added as filler. The combination of each amine and DPI concentration resulted in 12 formulations, which had the following properties analyzed: degree of conversion (DC), water sorption (Wsp) and solubility (Wsl), flexural strength (FS) and flexural modulus (Ef). Data for DC, FS and Ef were analyzed by two-way ANOVA and Tukey's test (α=0.05) and Wsp and Wsl by Kruskal-Wallis and Dunn tests (α=0.05). RESULTS: EDAB promoted a higher DC than did DMAEMA; however, DPI increased DC for all materials with DMAEMA. The physical properties of resin formulations containing EDAB were significantly better than those of groups with DMAEMA; however, DPI had a positive influence on the chemical and physical properties of the model resin cement containing DMAEMA, especially with higher concentrations of amine. SIGNIFICANCE: EDAB proved to be more reactive than DMAEMA, being less influenced by DPI. Resins containing a 1:2 CQ/amine ratio had better properties than those with 1:1.

Effect of diphenyliodonium hexafluorophosphate on the physical and chemical properties of ethanolic solvated resins containing camphorquinone and 1-phenyl-1,2-propanedione sensitizers as initiators.

OBJECTIVES: To evaluate the effects of the diphenyliodonium hexafluorophosphate (DPI) on the physical and mechanical properties of solvated dental adhesive resins containing camphorquinone (CQ) and/or 1-phenyl-1,2-propanedione (PPD) as initiators. METHODS: Model solvated resins containing bisphenol glycidyl methacrylate (BisGMA); triethyleneglycol dimethacrylate (TEGDMA); 1,3-glycerol dimethacrylate (GDMA); 2-hydroxyethyl methacrylate (HEMA); dimethylaminoethyl amine benzoate (EDAB) and ethanol were prepared. The resins were divided in 24 test groups according to the incorporated initiator systems (CQ-0.5 or 1mol%; PPD-0.5 or 1mol%; CQ+PPD-0.5 or 1mol%) as well the presence of DPI (0, 0.5 or 1mol%). Degree of conversion (using Fourier-transformed near infra-red spectroscopy), flexural strength and modulus by three point bending, cohesive strength and water sorption and solubility were measured. Data were statistically analyzed by one and two way ANOVA and Tukey's test (α=0.05). RESULTS: DPI increased the degree of conversion of all materials tested. Camphorquinone promoted higher degree of conversion than resins containing only PPD or CQ+PPD. Generally, the resins containing PPD+CQ with DPI presented higher flexural strength and modulus, cohesive strength, as well lower water sorption and solubility. SIGNIFICANCE: The use of PPD combined with CQ can increase the physical properties of the solvated resins. DPI improved the monomer conversion of all experimental materials and can positively modulate most of the physical properties of the solvated resins.

The effect of surface treatment and bonding procedures on the bond strength of silorane composite repairs.

OBJECTIVE: The aim of this study was to evaluate the effect of surface treatments and adhesive protocols on the microtensile bond strength of a low-shrinkage composite repair. MATERIALS AND METHODS: Ninety-six blocks of composite resin Filtek LS were prepared using a half-hourglass-shaped silicone matrix. The specimens were storage for 24 h in distilled water and were randomly divided into the experimental (6) and negative control (2) groups (n = 12) according to the surface treatment (diamond bur and aluminum oxide sandblasting) and adhesive protocol (none; Filtek LS adhesive; phosphoric acid + Filtek LS adhesive; and phosphoric acid + silane + Filtek LS adhesive). After the adhesive procedure, the specimens were fixed in an hourglass-shaped silicone matrix and the other half of the specimen was restored. Hourglass shaped specimens (n = 12) were used as positive control (cohesive strength of the resin). The microtensile bonding test was performed at a crosshead speed of 0.5 mm/min. The data were analyzed using ANOVA, Tukey's and Dunnett's tests (α = 0.05). RESULTS: The bond strength values were similar for all experimental groups, except the groups without adhesive application. None of the experimental groups presented results similar to the positive control group. CONCLUSIONS: The repair of silorane restorations is viable; nevertheless, the different bonding procedures tested were incapable to produce bond strengths similar to the cohesive strength of the material.

Surface roughness and staining susceptibility of composite resins after finishing and polishing.

PURPOSE: The study aims to investigate the influence of filler size and finishing systems on the surface roughness and staining of three composite resins. METHODS: Three composites, classified according to their filler size, were selected: Filtek Supreme Plus/nanofill (3M ESPE, St. Paul, MN, USA), Esthet-X/minifill (Dentsply Caulk, Milford, DE, USA), and Renamel Microfill/microfill (Cosmedent Inc., Chicago, IL, USA). Composite specimens were made in stainless steel split molds and polished with Sof-Lex (3M ESPE), Enhance+PoGo (Dentsply Caulk), or FlexiDiscs+Enamelize (Cosmedent Inc.). Finishing systems were used according to the manufacturers' instructions and polished surfaces were evaluated with a profilometer and then immersed in 2% methylene blue for 24 hours. Specimens were then prepared for spectrophotometric analysis and results were statistically analyzed by two-way analysis of variance and Tukey's test. RESULTS: No significant differences in surface roughness among the composites were found when the surfaces were treated with Enhance+PoGo. In addition, no differences were observed when the Filtek Supreme Plus composite was submitted to surface staining evaluation. In general, the composites polished with the finishing systems from the same company demonstrated lower surface roughness and staining. CONCLUSION: The results of this study recommend that composite resins could be finished and polished with finishing systems supplied by the composite's manufacturer. The surface roughness and staining of composite resins were not influenced solely by filler size. CLINICAL SIGNIFICANCE: Dentists should finish and polish composite resin with the polishing agent supplied by the same manufacturer. The smallest filler size does not necessarily result in a low surface roughness and staining susceptibility.

Effect of bleaching treatment and reduced application time of an antioxidant on bond strength to bleached enamel and subjacent dentin.

PURPOSE: To evaluate the influence of bleaching on bond strength to enamel and subjacent dentin, and to determine whether a reduced application time (1 min) of the antioxidizing agent can obviate the compromised bond strength after bleaching. MATERIALS AND METHODS: One hundred twelve bovine incisors were obtained, and the enamel and dentin surfaces were standardized to a thickness of 1 mm. The specimens were divided into two control groups (enamel and dentin without treatment) and 12 experimental groups (n = 10), based on the concentration of bleaching agents (carbamide peroxide 16% and hydrogen peroxide 35%), time interval between bleaching and restorative procedures (24 h; 24 h + sodium ascorbate (SA) 10%/1 min; 14 days), and substrate (enamel or dentin). All samples were submitted to the bleaching treatment on enamel. After the stipulated interval, a microshear test was performed. RESULTS: The bleaching treatment compromised the bond strength to the enamel when the restoration was performed 24 h after the end of bleaching. The bond strength to dentin was not affected by bleaching. CONCLUSIONS: The SA 10% application for 1 min obviates the detrimental effect of bleaching on bond strength. The bleaching performed on enamel does not affect the bond strength to the subjacent dentin.

Characterization of water sorption, solubility and filler particles of light-cured composite resins.

The goals of this study were to measure the water sorption (WS) and solubility (SO) of 3 composite resins containing different filler contents. Additionally, the size, shape, type and other characteristics of fillers were analyzed by scanning electron microscopy (SEM). Three composites, classified according to filler size, were selected: Filtek Supreme nanofill (3M/ESPE), Esthet-X minifill (Dentsply/Caulk) and Renamel microfill (Cosmedent Inc.). Ten disk-shaped specimens of each resin composite were made and stored in desiccators until constant mass was achieved. Specimens were then stored in water for 7 days, and the mass of each specimen was measured. The specimens were dried again and dried specimen mass determined. The WS and SO were calculated from these measurements. Data analyzed by one-way ANOVA and Tukey's post-hoc test (alpha=0.05). Composite filler particles were observed under SEM after removal of resin matrix by organic solvents. WS values were not significantly different among the resins; however, SO values were lower for Filtek Supreme. The materials presented differences in filler contents (e.g. particle size and shape). The composite resins had similar WS, while the SO was lower for the nanofill than for mini and microfill resins. The filler characteristics varied and were different among the materials.

Characterization of water sorption, solubility and filler particles of light-cured composite resins

The goals of this study were to measure the water sorption (WS) and solubility (SO) of 3 composite resins containing different filler contents. Additionally, the size, shape, type and other characteristics of fillers were analyzed by scanning electron microscopy (SEM). Three composites, classified according to filler size, were selected: Filtek Supreme nanofill (3M/ESPE), Esthet-X minifill (Dentsply/Caulk) and Renamel microfill (Cosmedent Inc.). Ten disk-shaped specimens of each resin composite were made and stored in desiccators until constant mass was achieved. Specimens were then stored in water for 7 days, and the mass of each specimen was measured. The specimens were dried again and dried specimen mass determined. The WS and SO were calculated from these measurements. Data analyzed by one-way ANOVA and Tukey's post-hoc test (?=0.05). Composite filler particles were observed under SEM after removal of resin matrix by organic solvents. WS values were not significantly different among the resins; however, SO values were lower for Filtek Supreme. The materials presented differences in filler contents (e.g. particle size and shape). The composite resins had similar WS, while the SO was lower for the nanofill than for mini and microfill resins. The filler characteristics varied and were different among the materials.

Os objetivos deste estudo foram determinar a sorção de água (SA) e solubilidade (SO) de 3 resinas compostas que contêm diferentes conteúdos de partículas de carga. Adicionalmente, o tamanho, formato, tipo e outras características das partículas foram analisados em microscopia eletrônica de varredura (MEV). As resinas foram selecionadas de acordo com o tamanho das partículas: Filtek Supreme nanoparticulado (3M ESPE), Esthet-X microhíbrido (Dentsply Caulk) e Renamel microparticulado (Cosmedent Inc.). Dez espécimes com formato de disco de cada compósito foram confeccionados e armazenados em dessecador até obtenção de massa constante. Em seguida, os espécimes foram armazenados em água por 7 dias e a massa mensurada novamente. Os espécimes foram desidratados novamente e a massa final mensurada. A SA e a SO foram calculados a partir destas medidas. As partículas de carga dos compósitos foram observadas em MEV, após a remoção da matriz orgânica com solventes orgânicos. Os dados foram analisados por ANOVA e teste de Tukey (?=0.05). As médias de SA das resinas compostas foram semelhantes. A SO foi menor para o compósito Filtek Supreme. Os materiais contêm diferentes conteúdos de carga, em termos de formato e tamanho das partículas. As resinas compostas mostraram similar SA, enquanto o compósito nanoparticulado apresentou a menor SO. As características das partículas de carga foram diferentes entre os compósitos estudados.