Color stability of bulk‐fill composites immersed in different drinks

Bulk‐fill composites show structural differences compared to those of conventional resin composites. Their more reactive photoinitiators, monomer compositions, and increased filler content may result in higher color stability than for conventional ones. Therefore, this study aimed to assess the color stability of three different bulk‐fill composites and one conventional resin composite with a higher filler load after 1 week and 1 month of immersion in different drinks. The resin composite materials that were tested demonstrated significantly different color changes after immersion in the four solutions during both evaluation periods. Immersion in coffee and red wine showed noticeable staining of all the materials. The discoloration effect of staining solutions on the resin composites depends both on the material composition and on the pigment types found in the solutions.     

Effects of different polymerization protocols on the degree of conversion of two dual‐cured core buildup composites polymerized by light‐emitting diode and halogen light‐curing units

The aim of study was to investigate the effects of various curing protocols with quartz–tungsten halogen (QTH) or light‐emitting diode (LED) light‐curing units on the degree of conversion (% DC) of two dual‐cured core buildup resin composites. Two dual‐cured core buildup resin composites, Clearfil Dc Core Automix (CLF) and Grandio Core Dc (GR), were selected. Specimens were exposed to the polymerization protocols as follows: there was immediate photoactivation or photoactivation delayed by 2 or 5 min by a QTH or LED source, and one group was allowed to chemically polymerize and served as a control (n = 6). The % DC of the specimens was determined with attenuated total reflectance–Fourier transform infrared spectroscopy. The GR samples polymerized with QTH for the 5‐min‐delayed photoactivation had higher % DC values than those self‐cured, and the Clearfil Dc Core Automix (CLF) samples with immediate or delayed curing protocols with halogen yielded higher % DC values than the samples that were chemically polymerized. The comparison of the two resin composites polymerized with halogen showed a higher % DC for CLF than for GR in the 2‐min‐delayed photoactivation. On the other hand, when they were cured with LED, the % DC values of GR significantly increased after the 2‐min‐delayed photoactivation. In light of the results, it might be stated that CLF polymerized with QTH, could be the better option. GR provided adequate chemical polymerization; therefore, it might be useful in areas in which light curing is not possible. Clinicians should consider the polymerization characteristics of dual‐cured resin composites. The use of different composites may require the modification of the application procedures recommended by the manufacturer. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40560.     

Study of physicochemical properties of two current commercial dental self‐curing resin composites

The aim of the present work is the study of some physicochemical properties of two current commercial dental self‐curing two component composites, i.e., of Concise? (3M?, Dental Products, St. Paul, USA), and Alfacomp (VOCO GmbH, Germany). Based on their filler type Concise is characterized as “conventional” or “macrofilled” composite and Alfacomp as “hybrid.” The resin matrix of Concise is a copolymer of 2‐bis[4‐2‐hydroxy‐3‐(methacryloxy)‐propyl]phenyl propane (Bis‐GMA)/triethyleneglycol dimethacrylate, while that of Alfacomp a homopolymer of Bis‐GMA. The composites were prepared in accordance with the manufacturers' instructions by mixing equal amounts of the two components at room temperature. The degree of conversion of double bonds of resin matrix during curing was determined in thin film of composites using FTIR transmission spectroscopy. The degree of conversion of Concise and Aflacomp was found to be correspondingly (73.63 ± 4.33)% and (47.75 ± 1.80)% after a day‐polymerization. Sorption, solubility, and volumetric change were determined after storage of composites in water or ethanol/water solution 75 vol % at 37°C (a good food/oral simulating fluid) for 30 days. These properties for both composites were higher in ethanol/water solution than in water. Also these properties for Concise were lower than those for Alfacomp in both liquids. Thermal stability of composites was studied by thermogravimetric analysis which performed in air atmosphere from 50 to 800°C. This analysis of composites showed the degradation of their resin matrix in three steps. The organic resin content of Concise was found to be 18.0% w/w and that of Alfacomp 20.1% w/w. Concise showed generally better properties than Alfacomp. This behavior must due to the differences in the chemical structure of the organic resin matrix and the type of inorganic filler. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Kinetics modeling of carbon‐fiber‐reinforced bismaleimide composites under microwave and thermal curing

This article focuses on the analysis of the curing kinetics of carbon‐fiber‐reinforced bismaleimide (BMI) composites during microwave (MW) curing. A nonisothermal differential scanning calorimetry (DSC) method was used to obtain an accurate kinetic model. The degree of curing, chemical characterization, and glass‐transition temperature of the resin and composites cured by thermal and MW heating were analyzed with DSC, Fourier transform infrared spectroscopy, and dynamic mechanical analysis. The experimental results indicate that MW accelerated the crosslinking reaction of the BMI resin and had different effects on the reaction processes, especially for the glass‐transition temperature and chemical bonds. However, the curing reaction rate of the BMI resin decreased when the carbon fibers were added to the BMI resin during thermal and MW curing. According to the experimental results, the curing kinetic model of the BMI composite was used to provide a theoretical foundation for MW curing analysis. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43770.     

A study of localized curing of glass‐filled composites using microhardness measurements

Extent of cure of hybrid composite systems is examined by conducting hardness measurements at different stages of the photopolymerization reaction and obtaining kinetic parameters that matched the experimental data. The materials are commercial dental composites based on bis[4‐(2‐hydroxy‐3‐methacryloyloxypropoxy)phenyl]propane resins with different photoinitiator concentrations as well as filler particle sizes and combinations. Samples (five per group) were made using nylon molds (2.5 × 5 mm) of the tested composites. The samples were light cured with a constant‐power light source for durations up to 20 s. After curing, all samples underwent Vicker's hardness testing of top and bottom surfaces. While there are significant differences in the polymerization behavior between the top and bottom locations for the tested composites, the corresponding growth exponent n, a kinetic parameter in the kinetic theory, is very close in all cases. For the tested materials the coefficient factor k is much lower for the bottom surfaces compared with the top surfaces. This reduction in the value of k is more severe for the material with a higher concentration of the photoinitiator as well as a higher percentage of glass filler particles in the wavelength range affecting the photopolymerization. It is argued that a relationship between k and the irradiation intensity can be used to quantify the decay of irradiated light with its penetration into the composites. The comparisons can be used to draw preliminary conclusions on the parameters controlling the effective depth of cure in a hybrid composite. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 97: 426–431, 2005     

UV‐curing and mechanical properties of polyester–acrylate nanocomposites films with silane‐modified antimony doped tin oxide nanoparticles

Antimony doped tin oxide (ATO) nanoparticles were used as nanofillers to improve mechanical properties of UV‐cured polyester–acrylate films. To improve the dispersion of ATO nanoparticles in the polyester–acrylate resin matrix and to strengthen interfacial interactions between ATO nanoparticles and the resin matrix ATO nanoparticles were first organically modified with 3‐methacryloxypropyltrimethoxysilane (MPS). The modification of ATO nanoparticles with MPS was confirmed by FTIR spectroscopy and thermogravimetric analysis (TGA). UV‐curing behaviors of the nanocomposites films were investigated by FTIR spectroscopy. Compared with the film with neat ATO nanoparticles, the film with the same amount of MPS‐modified ATO nanoparticles showed slightly higher UV‐curing rate and final conversion. The mechanical properties of the nanocomposites films were measured by universal testing machine. The MPS‐modified ATO nanoparticles could improve considerably the mechanical properties of the UV‐cured polyester–acrylate nanocomposites films. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Irradiation dose control for polymer‐matrix composites fabricated by in situ curing with low‐energy electron beam

The electron beam (EB) with emitting energies lower than 150 keV is applicable in in situ curing of polymer‐matrix composites; however, being poor in penetration ability, it leads to significant attenuation of irradiation dose along the prepreg thickness. In this study, polymer‐matrix composites were fabricated by low‐energy EB irradiation curing, and the effect of dose control of double‐sided irradiation was systematically investigated. Experimental results showed that laminates fabricated by single‐sided irradiated prepregs were low in interlaminar shear strength (ILSS) owing to incomplete curing after being post cured at 180 °C for 30 min. A double‐sided irradiation method which included irradiation of equal dose and different doses on both sides of the prepreg was proposed to overcome this difficulty. Analysis showed that under a total dose of 70 and 100 kGy, the ILSS results were high owing to the low curing degree of two adhesive surfaces; under a total dose of 130 and 160 kGy, laminates fabricated with different EB irradiation doses on both sides exhibited enhanced ILSS compared to those with equal dose on both sides, owing to physical adhesion and chemical crosslinking between layers. The ILSS results exhibited the largest increase of 18.9 and 60.5%, respectively, by tuning the dose differences between both sides of the prepregs. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44944.     

Polymerization behavior of an organophosphorus monomer for use in dental restorative materials

Vibrational overtone activated polymerization of acrylonitrile (AN) has been demonstrated using two initiators, benzoyl peroxide (BP), and 2,2′‐(azobis)isobutyronitrile (AIBN). Excitation of the fifth vibrational overtone of the CH stretch of AIBN at 627 nm and BP at 604 nm initiates the reaction. Monomer conversions were monitored by a gravimetric method. In both cases, the wavelength selectivity was investigated by irradiating the monomer/initiator mixtures at the absorption maximum of the initiator, the absorption maximum of the monomer, and at a wavelength (580 nm for AN/AIBN and 625 nm for AN/BP) where neither the initiator nor the monomer absorbs light. For the AN/AIBN mixture, after 48 h the monomer conversion for the irradiation on the peak absorption of AIBN (627 nm) is about twice as large as the irradiation at 580 nm. For the AN/BP mixture, after 48 h the monomer conversion for the irradiation on the peak absorption of BP (604 nm) is about a factor of 2.2 larger than for the irradiation at 625 nm. The overall quantum yields of both polymerizations were estimated. After 48 h the overall quantum yield for the AN/AIBN mixture irradiated at the initiator absorption (Φ₆₂₇ = 21083) is about 10 times larger than for the sample irradiated at the pure monomer absorption (Φ₅₉₅ = 1942). For the AN/BP mixture, the 604 nm quantum yield (Φ₆₀₄ = 1096) is about 2.4 times larger than the 595 nm quantum yield (Φ₅₉₅ = 448). The influence of the initiator concentration is also presented. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 565–571, 2003     

A comparison of efficiency of two photoinitiators for polymerization of light‐cure dental composite resins

The purpose of the study was to compare the effect of two photoinitiators, (?)camphorquinone (CQ) and 1‐phenyl‐1,2‐propanedione (PPD) on curing performance of light‐cure dental composite resins. Bisphenol A‐glycidyl methacrylate (BisGMA)/triethylene glycol dimethacrylate (TEGDMA) monomer mixture was used as the resin matrix. The resin matrix was mixed with CQ and/or PPD along with 0.25% of 4‐(dimethyl amino) phenethyl alcohol (DMAPEA) catalyst. The effect of photoinitiator on curing performance was evaluated and compared in terms of properties such as depth of cure, diametral tensile strength (DTS), flexural strength (FS), flexural modulus (FM), vickers hardness number (VHN), water sorption (WS), and solubility of cured composite. Statistical evaluation using Analysis of Variance (single factor) showed that the photosensitization efficiency of CQ and PPD are comparable. However, their combination showed synergistic effect for properties such as DTS and solubility. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Ultraviolet‐curing behavior of an epoxy acrylate resin system

Ultraviolet (UV)‐curing behavior of an epoxy acrylate resin system comprising an epoxy acrylate oligomer, a reactive diluent, and a photoinitiator was investigated by Fourier transform infrared (FTIR) spectroscopy. The conversion changes of the resin system containing 20 phr of 1,6‐hexanediol diacrylate as a reactive diluent and 2‐hydroxy‐2‐methyl‐1‐phenyl‐propan‐1‐one as a photoinitiator were measured under different UV‐curing conditions. The fractional conversion was calculated from the area of the absorption peak for the vinyl group vibration occurring at 810 cm^?1. The effects of photoinitiator concentration, total UV dosage, one‐step or stepwise UV irradiation, UV intensity, atmosphere, and temperature on the curing behavior of the resin system were investigated. The conversion of the resin system increased rapidly at the initial stage of the UV‐curing process but increased very slowly after that. The final conversion of the resin system was mainly affected by total UV dosage. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 1180–1185, 2005     

Evaluation of polymerization shrinkage in dental restorative experimental composites based: BisGMA/TEGDMA,filled with MMT

This work concerns to the investigation of the polymerization shrinkage and mechanical properties in dental restoratives experimental composites filled with nano clay Montmorilonite (MMT) Cloisite^® 10A nanoparticles, in glycidyl methacrylate resin, using experimental composites filled with silanized Aerosil OX‐50 Silica as a control group. Six formulations with BisGMA/TEGDMA based polymeric matrix (three added with MMT and three added with silanized silica as filler) containing 50, 60, and 70 wt % were investigated. Characterization of the experimental composites was established with the following analyses: Scanning Electron Microscope, (SEM); Thermo‐Mechanical Analysis, (TMA) for Shrinkage Polymerization; Differential Scanning Calorimetry Analysis (DSC); Knoop Micro Hardness analysis; X‐ray Diffraction (XRD); Degree of Conversion (DC); Elastic Modulus and Flexural Strength; Transmission Electron Microscopy (TEM). Statistical Analyses were realized using two‐way ANOVA (type and amount of filler) and Tukey's test. TMA results showed that composites filled with MMT nanoparticle present statistically lower polymerization shrinkage values and statistically high degree of conversion in all formulations tested, when compared to composites filled with silanized silica. XRD and TEM analyses showed evidences of the intercalation phenomenon in the MMT nanoparticles in relation to BisGMA/TEGDMA polymeric matrix. However, for Flexural Strength, groups filled with MMT nanoparticle showed statistically lower values in all concentration tested. At high filler concentration it was observed the appearance of tactoids and functionalization of MMT nanoparticle did not promote a strong interface adhesion between polymeric matrix and filler. In order to adjust the mechanical properties, it would be convenient to promote the concentration optimization of MMT nanoparticles. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43543.     

Development of low‐shrinkage composites based on novel crosslinking vinylcyclopropanes

Polymerization shrinkage of methacrylate‐based dental composites remains a major concern in restorative dentistry. Cyclic monomers that undergo ring‐opening polymerization are known to exhibit reduced polymerization shrinkage compared to methacrylates. In this article, the synthesis of four crosslinking 1,1‐disubstituted 2‐vinylcyclopropanes bearing rigid spacers is described. These monomers were synthesized by esterification of 1‐ethoxycarbonyl‐2‐vinylcyclopropane‐1‐carboxylic acid with the corresponding diols. The photopolymerization kinetics of these monomers was investigated by photo‐differential scanning calorimeter using bis(4‐methoxybenzoyl)diethylgermane as the photoinitiator. The synthesized vinylcyclopropanes (VCPs) were shown to be more reactive than the frequently used reactive diluent triethylene glycol dimethacrylate. Composites based on these VCPs showed good mechanical properties and exhibited a significantly reduced volumetric shrinkage and shrinkage stress compared to a corresponding dimethacrylate‐based restorative material. This work highlights the excellent potential of VCPs as alternatives to methacrylates in the development of low‐shrinkage dental composites. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45577.     

The mechanical properties of β‐Si3N4 whiskers‐reinforced dental resin composites

The surface‐modified β‐Si₃N₄ whiskers were used as inorganic fillers to reinforce dental resin (Bis‐GMA/TEGDMA) matrix with filler level ranging from 0 to 60 wt %. The experimental results indicated that the fracture strength of the composites increased from 79.85 to 139.8 MPa with increasing the whiskers loading. The compressive strength, elastic modulus, and rockwell hardness all increased monotonously with increasing filler level. Furthermore, thermal cycling did not decrease the fracture strength of the composites. Moreover, the composites showed good biocompatibility to support MG63 cells adhesion and proliferation. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40692.     

Tetraacylgermanes as highly efficient photoinitiators for visible light cured dimethacrylate resins and dental composites

Tetrabenzoylgermane 1 and various substituted tetrabenzoylgermanes 2 – 7 were investigated as visible light (VL) photoinitiators (PIs) for dental dimethacrylate resins and dimethacrylate‐based composites. The tetrabenzoylgermanes 1 – 7 show a very strong VL absorption between 400 and 450 nm. Substituents on the benzoyl chromophore strongly influence their properties such as melting point, solubility, absorption behavior, or PI reactivity. A good photobleaching behavior and a very high reactivity as VL PI was found in photo‐differential scanning calorimeter experiments for selected tetrabenzoylgermanes. Composite pastes containing only ～0.1 wt % of Ge‐PI exhibited a sufficient photocuring due to the high PI‐reactivity of the tetraacylgermanes. Among the investigated germane PIs, tetrakis(2‐methylbenzoyl)germane 2 shows the best performance as VL PI for restorative composites and enables the composites to be photocured using an LED with an emission maximum of 500 nm. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46115.     

Influences of different gravity environments on the curing process and cured products of carbon‐nanotube‐reinforced epoxy composites

The influences of different gravity environments on the curing process and the cured products of carbon‐nanotube‐reinforced epoxy composites were investigated in this study. Different gravity environments were simulated with a superconducting magnet on the basis of which resin matrix composites with different amino‐functionalized multiwalled carbon nanotube (NH₂‐MWCNT) concentrations of 0.1, 0.3, 0.5, and 1 wt % were tested. Fourier transform infrared spectroscopy, differential scanning calorimetry, dynamic mechanical analysis, thermomechanical analysis (TMA), thermogravimetric analysis, scanning electron microscopy, transmission electron microscopy, and three‐point bending tests were used to analyze the characteristics of different curing processes and cured products. From the results, we observed that the curing rate of the epoxy composites was influenced by different gravity values, and there was anisotropy in the NH₂‐MWCNT‐reinforced epoxy composites cured in the simulated microgravity environment. More effects of gravity on the curing process and cured products could be obtained through detailed experiments and discussion; this is important and fundamental for improving and enhancing the properties of composite materials used in different gravity environments. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41413.     

The effect of curing lights and modes on dentin bond strength of bulk-fill composites applied in different thickness

To investigate shear bond strength (SBS) to dentin of a conventional and three bulk-fill composites applied in different increment thickness and cured by mono- and multi-wave LED LCUs. Two hundred and fifty-two extracted sound human molars were prepared for SBS test. The teeth were divided into four groups according to the resin composites used. Conventional composite: Tetric N-Ceram (control); high-viscosity bulk-fills: Tetric N-Ceram Bulk Fill, X-tra Fil, and SonicFill. Each group was subdivided (n?=?7) according to increment thickness (2, 4, and 6?mm) and cured by standard mode of a mono-wave LED or two different modes (standard and xtra power) of a multi-wave LED. The failure mode was stereomicroscopically determined at 40× magnification. Data were analyzed using Three-way ANOVA and further comparisons were assessed by Bonferroni’s multiple comparison test. There were no significant differences within X-tra fil and Tetric N-Ceram Bulk Fill groups for any of the variables (p?>?0.05). A significant decrease in SBS values with increase of layer thickness was observed for SonicFill and control groups. Also, curing mode had a significant effect on both composites at 6?mm thickness and standard mode of multi-wave LED caused the highest SBS value (p???0.05). Adhesive failure was the most common fracture pattern especially at 6?mm thickness applications. Based on the results of this study, the bulk-fill composites can be safely applied in one-step with 4?mm increments, although the examined composites performed better at 2?mm thickness. The performance of the composites at 6?mm increment may show differences related to the curing lights and modes.     

A study on composites from phenol‐formaldehyde‐casein resin

A modified phenol‐formaldehyde (PF) resin was synthesized under alkaline condition in varying proportion of casein up to 20% (w/w) of phenol. All the prepared resins were characterized by free phenol content, free formaldehyde content, viscosity measurements, number average molecular weight determination by conductometry and Infrared Spectroscopy (IR). Their curing kinetics was studied isothermally and by differential scanning calorimetry (DSC) on dynamic runs. The resin samples were cured using concentrated hydrochloric acid and hexamine individually. Cured resins were characterized by IR and Thermogravimetry (TGA). Glass fabric reinforced composites (GFRC) were fabricated by maintaining 40 : 60 proportion of resin to reinforcement material. The laminates thus formed were characterized for their mechanical properties and chemical resistance. Enhancements in thermal stability of the resin as well as toughness of composite with increase in casein content were observed for the resins studied. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Intrinsic flame-retardant epoxy resin composites with benzoxazine: Effect of a catalyst and a low curing temperature

Three kinds of inherent flame-retardant epoxy resin (EP) composites with 20 wt % benzoxazine (BOZ) were prepared with different curing processes with 2-methyl-1H-imidazole (MI) as a catalyst or/and changes in the curing temperature. The effects of the curing process on the flame retardancy, thermal stability, mechanical properties, and curing behaviors were investigated. The composite with added MI cured at low temperature (EBM–LT) had the best properties. It possessed a 35.3% limiting oxygen index and achieved a UL 94 V-0 rating. Thermogravimetric analysis indicated that EBM–LT had the best thermal stability among the three kinds of EP composites with BOZ. The EP composites with BOZ mainly displayed a condensed-phase flame-retardant mechanism. The mechanical properties improvement was attributed to the formation of a heterogeneous network. Differential scanning calorimetry indicated that MI reacted with EP and catalyzed the homopolymerization of BOZ, and EP reacted with BOZ. Fourier transform infrared spectroscopy analysis indicated that curing at lower temperature caused the formation of more homopolymers of BOZ. The relationship of the curing process, network structure, and properties of EP composites with BOZ was established; this could help with the design of high-performance EP composites with BOZ. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47847.     

复合材料缠绕成型用电子束固化环氧树脂体系研究

为了研究适合于缠绕成型的低粘度可电子束固化复合材料的耐热环氧树脂基体,研究了不同组成的电子束固化树脂体系的粘度与温度的关系、耐热性与辐射剂量的关系及浇注体的力学性能。研究表明,树脂EB-4在60℃时粘度为389 mPa.s,树脂辐射固化的最佳剂量为150 kGy,而且在150 kGy辐射固化的EB-1、EB-4的玻璃化转变温度Tg分别为212.96℃、214.77℃,EB-4树脂浇注体的拉伸强度可以达到52.7 MPa,拉伸弹性模量2.79 GPa,断裂延伸率为2.18%,是1种适用于室温或低温下缠绕成型的耐热电子束固化环氧树脂基复合材料树脂体系。     

Fabrication and properties of surface‐modified β‐Si3N4 whiskers reinforced dental resin composites

In this article, three kinds of surface‐modified methods were used to treat β‐Si₃N₄ whiskers before being incorporated into Bis‐GMA/TEGDMA dental resin matrix in order to improve the whiskers' reinforcing effect. The experimental results showed that composites with directly heat‐treated and then silanized β‐Si₃N₄ whiskers had the best reinforcing effect. They had flexural strength of 160 ± 7.0 MPa (mean ± SD; n = 6), compressive strength of 371 ± 1.4 MPa (mean ± SD; n = 5) and HRA of 48.4 ± 0.5(mean ± SD; n = 5), respectively. In addition, water sorption and solubility test demonstrated that the composites were reliable to use as the dental restoration materials. Therefore, the directly heat‐treated and then silanized β‐Si₃N₄ whiskers (better than β‐Si₃N₄ whiskers mixed with SiO₂ nanoparticles or SiO₂ sols) were most suitable fillers to reinforce dental resin composites. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013