Evaluation of two Bis-GMA analogues as potential monomer diluents to improve the mechanical properties of light-cured composite resins.

OBJECTIVES: The aim of this study was to investigate the influence of new diluent agents, diluent ratio and filler content, on relevant mechanical properties of several novel composite resins containing Bis-GMA as resin matrices, and to compare these with the properties of composites based on TEGDMA, a conventionally used diluent. METHODS: Two Bis-GMA analogues were synthesized and 20 experimental composite resins were prepared combining three monomer mixtures (Bis-GMA/TEGDMA, Bis-GMA/CH3 Bis-GMA and Bis-GMA/CF3 Bis-GMA), at three dilution rates (85/15, 10/90, 0/100) and three levels of hybrid filler content (barium aluminosilicate glass): 0, 10 and 35%. Flexural strength (FS), modulus of elasticity (ME) and microhardness (VHN) of the composites were evaluated. Five specimens of each material were prepared for each mechanical test, light-cured over 120 s and stored in water at 37 degrees C for 1 week. Three-point bending test was used for FS measurement and VHN was quantified by using a Vickers microindentor. Data were analyzed by ANOVA and Student-Newman-Keuls tests (P<0.05). RESULTS: Materials with CH3 Bis-GMA showed an enhanced VHN. Mean FS was higher for matrices containing TEGDMA. Overall, dilution favored FS and VHN but not ME. Filler loading specially improved ME and VHN. SIGNIFICANCE: Results correlate with an increase in the extent of polymerization due to the higher flexibility of the less viscous comonomer starting system and the hydrophobic character of the Bis-GMA analogues.     

The application of fluorinated aromatic dimethacrylates and diacrylates to light-cured composite resins. 1. Improvement of transmittance of composite

To improve the transmittance of light-cured composite resins, the matching of the refractive indices of the matrix monomer and filler were examined. Eight fluorinated aromatic dimethacrylates and diacrylates with a low refractive index were synthesized. Three of these monomers had a poor solubility to TEGDMA. The depths of cure and the other physical properties of eight experimental composites prepared from one of five fluorinated monomers, TEGDMA and UDMA were determined compared with those of the control composites prepared from Bis-GMA or Bis-MEPP/ and TEGDMA in the same ratio. These composites contained 70 wt% of silanized silica filler. The depths of cure of the experimental composites except for one were significantly greater than those of the control composites. The mechanical properties of the experimental composites were comparable to those of the control composites with a few exceptions, but the difference in the mechanical properties between these exceptional composites and the control was small. The water sorption of the experimental composites was markedly lower than that of the composite containing Bis-GMA and comparable to that of the composite containing Bis-MEPP. These five fluorinated monomers are considered useful as the matrix monomer of light-cured composite resins.     

Water sorption of CH3- and CF3-Bis-GMA based resins with additives

Objectives

To evaluate the effect of additives on the water sorption characteristics of Bis-GMA based copolymers and composites containing TEGDMA, CH₃Bis-GMA or CF₃Bis-GMA.

Material and methods

Fifteen experimental copolymers and corresponding composites were prepared combining Bis-GMA and TEGDMA, CH₃Bis-GMA or CF₃Bis-GMA, with aldehyde or diketone (24 and 32 mol%) totaling 30 groups. For composites, barium aluminosilicate glass and pyrogenic silica was added to comonomer mixtures. Photopolymerization was effected by 0.2 wt% each of camphorquinone and N,N-dimethyl-p-toluidine. Specimen densities in dry and water saturated conditions were obtained by Archimedes'' method. Water sorption and desorption were evaluated in a desorption-sorption-desorption cycle. Water uptake (%WU), water desorption (%WD), equilibrium solubility (ES; µg/mm³), swelling (f) and volume increase (%V) were calculated using appropriate equations.

Results

All resins with additives had increased %WU and ES. TEGDMA-containing systems presented higher %WU, %WD, ES, f and %V values, followed by resins based on CH₃Bis-GMA and CF₃Bis-GMA.

Conclusions

Aldehyde and diketone led to increases in the water sorption characteristics of experimental resins.     

Influence of additives on the properties of Bis-GMA/Bis-GMA analog comonomers and corresponding copolymers.

OBJECTIVES: The purpose of this study was to evaluate the effect of two additives: propionaldehyde (aldehyde) and 2,3-butanedione (diketone) on the properties of Bis-GMA diluted with TEGDMA and the synthesized Bis-GMA analogs, propoxylated Bis-GMA (CH(3)Bis-GMA) and propoxylated fluorinated Bis-GMA (CF(3)Bis-GMA). METHODS: Nine experimental comonomers were prepared combining Bis-GMA and TEGDMA, CH(3)Bis-GMA, CF(3)Bis-GMA, with aldehyde (32mol%) and diketone (32mol%). Photopolymerization was effected by using Camphorquinone (0.2wt%) and N,N-dimethyl-p-toluidine (0.2wt%). Experimental comonomer viscosity (Brookfield viscometer), polymerization shrinkage (gravimetrically), degree of conversion (FT-IR) and contact angles (contact angle goniometer) were determined. Comonomer and copolymer T(g)s (DSC and Fox equation) were also evaluated. Data were analyzed by one-way ANOVA and Tukey test (alpha=0.05). RESULTS: Bis-GMA/CH(3)Bis-GMA and Bis-GMA/CF(3)Bis-GMA with additives exhibited lower viscosities (p<0.01). Inclusion of additives into the comonomer systems did not produce significant increase in polymerization shrinkage (p>0.05). A significant increase in degree of conversion was shown for Bis-GMA/TEGDMA and Bis-GMA/CH(3)Bis-GMA with additives (p<0.01). Additives reduced contact angle and comonomer T(g) values, whereas the corresponding copolymers with additives showed an increase in T(g). SIGNIFICANCE: Use of novel comonomer systems with the addition of aldehyde and diketone functional groups would improve dental resin composite properties.     

In vitro wear, surface roughness and hardness of propanal-containing and diacetyl-containing novel composites and copolymers based on bis-GMA analogs.

OBJECTIVE: To evaluate the effect of two additives, aldehyde or diketone, on the wear, roughness and hardness of bis-GMA-based composites/copolymers containing TEGDMA, propoxylated bis-GMA (CH(3)bis-GMA) or propoxylated fluorinated bis-GMA (CF(3)bis-GMA). METHODS: Fifteen experimental composites and 15 corresponding copolymers were prepared combining bis-GMA and TEGDMA, CH(3)bis-GMA or CF(3)bis-GMA, with aldehyde (24 mol% and 32 mol%) or diketone (24 mol% and 32 mol%) totaling 30 groups. For composites, hybrid treated filler (barium aluminosilicate glass/pyrogenic silica; 60 wt%) was added to monomer mixtures. Photopolymerization was affected by 0.2 wt% each of camphorquinone and N,N-dimethyl-p-toluidine. Wear (W) test was conducted in a toothbrushing abrasion machine (n=6) and quantified using a profilometer. Surface roughness (R) changes, before and after abrasion test, were determined using a rugosimeter. Microhardness (H) measurements were performed for dry and wet samples using a Knoop microindenter (n=6). Data were analyzed by one-way ANOVA and Tukey's test (alpha=0.05). RESULTS: Incorporation of additives led to improved W and H values for bis-GMA/TEGDMA and bis-GMA/CH(3)bis-GMA systems. Additives had no significant effect on the W and H changes of bis-GMA/CF(3)bis-GMA. With regard to R changes, additives produced decreased values for bis-GMA/CH(3)bis-GMA and bis-GMA/CF(3)bis-GMA composites. Bis-GMA/TEGDMA and bis-GMA/CH(3)bis-GMA copolymers with additives became smoother after abrasion test. SIGNIFICANCE: The findings correlate with additives ability to improve degree of conversion of some composites/copolymers thereby enhancing mechanical properties.     

Physicochemical properties of dental resins formulated with amine-free photoinitiation systems

ObjectiveTo assess the mechanical properties of two different dimethacrylate resin blends containing the photosensitizer camphorquinone (CQ) alone or in combination with one or more synergists including an amine and/or an iodonium.MethodsTwo co-monomer resin blends were formulated using Bis-GMA/TEGDMA and UDMA/TEGDMA, both at 1:1 mass ratio. Each resin blend was divided into four groups, comprising the following four photoinitiation systems: (1) CQ + 2-(dimethylamino)ethyl methacrylate (DMAEMA); (2) CQ + DMAEMA + bis(4-methyl phenyl)iodonium hexafluorophosphate (BPI); (3) CQ; and (4) CQ + BPI. Materials were evaluated for polymerisation kinetics, water sorption, solubility, flexural strength and modulus.ResultsBisGMA/TEGDMA with CQ showed minimal and insignificant degree of conversion and was not tested for water sorption/solubility and mechanical properties. The ternary system (i.e., CQ + DMAEMA + BPI), promoted the highest degree of conversion for each monomer blend. The resins containing amine had higher mechanical properties than the amine free. However, the UDMA amine free resins exhibited greater flexural strength and modulus than the corresponding amine free BisGMA resins. BisGMA/TEGDMA containing CQ + DMAEMA or CQ + BPI had significantly higher water sorption and solubility than the other groups.SignificanceResins containing amine presented better properties than the amine-free systems. The addition of iodonium salt (BPI) improved the degree of conversion of the resins, even without an amine co-initiator. The amine-free initiator system (CQ + BPI) was more effective when used with UDMA versus BisGMA based-resins respectively.     

Fabrication and evaluation of Bis-GMA/TEGDMA dental resins/composites containing nano fibrillar silicate.

OBJECTIVE: To investigate the reinforcement of Bis-GMA/TEGDMA dental resins (without conventional glass filler) and composites (with conventional glass filler) with various mass fractions of nano fibrillar silicate (FS). METHODS: Three dispersion methods were studied to separate the silanized FS as nano-scaled single crystals and uniformly distribute them into dental matrices. The photo-curing behaviors of the Bis-GMA/TEGDMA/FS resins were monitored in situ by RT-NIR to study the photopolymerization rate and the vinyl double bond conversion. Mechanical properties (flexural strength, elastic modulus and work-of-fracture) of the nano FS reinforced resins/composites were tested, and analysis of variance (ANOVA) was used for the statistical analysis of the acquired data. The morphology of nano FS and the representative fracture surfaces of its reinforced resins/composites were examined by SEM/TEM. RESULTS: Impregnation of small mass fractions (1% and 2.5%) of nano FS into Bis-GMA/TEGDMA (50/50 mass ratio) dental resins/composites improved the mechanical properties substantially. Larger mass fraction of impregnation (7.5%), however, did not further improve the mechanical properties (one way ANOVA, P>0.05) and may even reduce the mechanical properties. The high degree of separation and uniform distribution of nano FS into dental resins/composites was a challenge. Impregnation of nano FS into dental resins/composites could result in two opposite effects: a reinforcing effect due to the highly separated and uniformly distributed nano FS single crystals, or a weakening effect due to the formation of FS agglomerates/particles. SIGNIFICANCE: Uniform distribution of highly separated nano FS single crystals into dental resins/composites could significantly improve the mechanical properties of the resins/composites.     

Hydrolytic stability of experimental hydroxyapatite-filled dental composite materials.

OBJECTIVES: The purpose of this study was to analyze the behavior in water, related to mechanical properties, of experimental composites for dental restoration. METHODS: The studied materials were composed of a visible-light-curing monomer mixture (Bis-GMA and TEGDMA or HEMA) and micrometric, nanometric or a mixture of both sizes hydroxyapatite particles as a reinforcing filler. Filler particles were modified with a coupling agent (citric, hydrosuccinic, acrylic or methacrylic acid or silane). The hydrolytic stability of the evaluated materials was studied through total elution and water-uptake tests. Percent net-mass variation was daily monitored and analyzed as a function of time. Mechanical performance was examined through flexural properties and Vickers hardness. Morphological surface changes were observed with scanning electron microscopy. ANOVA statistical analysis was performed (P<0.05). RESULTS: In general, the use of HEMA instead of TEGDMA did not substantially worsen the composite quality. Dental composites containing only nanometric particles of hydroxyapatite as a filler are unsuitable for clinical performance. Midway-filled composite resins loaded with micro-HAP particles, coated with citric, acrylic or methacrylic acid displayed low percent elution and water-uptake values. Mechanical properties were similar or even superior to those measured for silane treated particles. SIGNIFICANCE: More research is needed to further improve the interaction of nano-HAP particles with the polymeric matrix, either as a single filler or, preferentially, mixed with micro-HAP, that will allow to increase the total loading of reinforcing filler and, hence, to improve the mechanical properties.     

Synthesis and evaluation of ethylene glycol 3-diethylamino-propionate methacrylate as a polymerizable amine coinitiator for dental application.

OBJECTIVE: The primary objective of this study was to synthesize and characterize ethylene glycol 3-diethylamino-propionate methacrylate (EGDPM) as a polymerizable coinitiator to replace the commercial amine coinitiator. The 2,2-bis[4-(2-hydroxy-3-methacryloxypropoxy)phenyl]-propane (Bis-GMA) and triethylene glycol dimethylacrylate (TEGDMA) resin mixture was polymerized by camphorquinone/EGDPM initiator system under visible light irradiation. The mechanical properties, water sorption and solubility of cured samples were also evaluated. METHODS: EGDPM was synthesized via Michael-Addition reaction and characterized using FTIR and 1H NMR spectroscopy. Photopolymerization kinetics of the dental resin mixtures were monitored by real-time IR (RTIR). The mechanical properties of cured samples were recorded by dynamic mechanical analyzer (DMA). And the water sorption and solubility of cured samples were detected according to ISO 4049. RESULTS: Both the double bond conversion and the rate of polymerization of the resin mixtures increased as increasing the concentration of EGDPM but were lower than that of ethyl-4-dimethylaminobenzoate (EDMAB) and 2-(dimethylamine)ethyl methacrylate (DMEM) as a coinitiator at some concentration. When it served as diluent, the final double bond conversion was comparable to that of EDMAB, and the rate of polymerization was higher than that of DMEM. The modulus and T(g) of the cured samples were very close. Water sorption and solubility of the samples were almost the same except that of EGDPM as diluent. CONCLUSIONS: EGDPM was synthesized by Michael-Addition reaction. It could be used as a potential coinitiator but not suitable as diluent for dental composite.     

High performance dental resin composites with hydrolytically stable monomers

Objective

The objectives of this project were to: 1) develop strong and durable dental resin composites by employing new monomers that are hydrolytically stable, and 2) demonstrate that resin composites based on these monomers perform superiorly to the traditional bisphenol A glycidyl dimethacrylate/triethylene glycol dimethacrylate (Bis-GMA/TEGDMA) composites under testing conditions relevant to clinical applications.

Preparation of a fluorinated dental resin system and its anti-adhesive properties against S. mutans

ObjectivesThe purpose of this study was to characterize physicochemical properties and investigate anti-bacterial adhesion effect of dental resins containing fluorinated monomers.MethodFluorinated dimethacrylate FDMA was mixed with commonly used reactive diluent triethylene- glycol dimethacrylate (TEGDMA) and fluorinated diluent 1 H,1 H-heptafluorobutyl methacrylate (FBMA) separately at a mass ratio of 60 wt./40 wt. to prepare fluorinated resin systems. Double bond conversion (DC), flexural strength (FS) and modulus (FM), water sorption (WS) and solubility (SL), contact angle and surface free energy, surface element concentration, and anti-adhesion effect against Streptococcus mutans (S. mutans) were investigated according to standard or referenced methods. 2,2-bis[4-(2-hydroxy-3-methacryloy-loxypropyl)-phenyl]propane (Bis-GMA)/TEGDMA (60/40, wt./wt.) was used as control.ResultsBoth fluorinated resin systems had higher DC than Bis-GMA based resin (p < 0.05); compared with Bis-GMA based resin (FS, FDMA/TEGDMA resin system had higher FS (p < 0.05) and comparable FM (p > 0.05), while FDMA/FBMA resins system had lower FS and FM (p < 0.05). Both fluorinated resin systems had lower WS and SL than Bis-GMA based resin (p < 0.05), and FDMA/TEGDMA resin system had the lowest WS (p < 0.05) in all experimental resin systems. Only FDMA/FBMA resin system showed lower surface free energy than Bis-GMA based resin (p < 0.05). When the surface was smooth, FDMA/FBMA resin system had lower amount of adherent S. mutans than Bis-GMA based resin (p < 0.05), while after the surface became roughness, FDMA/FBMA resin system had comparable amount of adherent S. mutans as Bis-GMA based resin (p > 0.05).SignificanceResin system prepared exclusively with fluorinated methacrylate monomers reduced the S. mutans adhesion due to their increased hydrophobicity and decreased surface energy., while flexural properties of it should be improved.     

Synthesis of organic-inorganic hybrid compounds based on Bis-GMA and its sol-gel behavior analysis using Taguchi method.

OBJECTIVES: The aim of this study was the synthesis of organic-inorganic hybrid compounds based on Bis-GMA and incorporation of them into conventional Bis-GMA/TEGDMA dental resins. This was achieved by the synthesis of Bis-GMA bearing two -Si(OEt)3 reactive groups (a bridged monomer) and subsequent hydrolysis-condensation reactions with TEOS, in TEGDMA media. METHODS: The structure of the bridged monomer was characterized by using FTIR technique. The sol-gel behavior of the aforementioned hydrolysis-condensation reactions was investigated by using an experimental design based on the Taguchi method. Therefore, amounts of the bridged monomer, TEOS and TEGDMA in the gelation process were optimized in order to achieve the maximum gel content without complete gelation of the mixture. RESULTS: It was found that the amount of the bridged monomer has the major effect with the amount of TEGDMA having a minor effect. The cross-over effect between the constituents of the mixture was also investigated to be negligible. SIGNIFICANCE: The organic-inorganic hybrids developed based on Bis-GMA can be combined with commonly used methacrylate light-curable dental resins.     

螺环原酸酯对牙科基体树脂的改性研究

目的：用螺环原酸酯膨胀单体对牙科BisS-GMA基体树脂进行改性的研究。方法：分别以BisS-GMA和Bis-GMA作树脂基质,TEGDMA为稀释单体,加入和不加入螺环原酸酯膨胀单体,配制四种基体树脂。以CQ/DMAEMA为光引发体系,光固化后测定并比较其体积收缩率、聚合转化率、粘接拉伸强度和固化时间。结果：含膨胀单体的BisS-GMA基体树脂的体积收缩率较低,聚合转化率和粘接拉伸强度较高,且固化时间合适。结论：螺环原酸酯膨胀单体的开环聚合反应能使BisS-GMA基体树脂的体积收缩率显著降低,并能提高其聚合转化率和粘接拉伸强度。     

Mechanical properties of visible light-cured resins reinforced with hydroxyapatite for dental restoration.

OBJECTIVES: The purpose of this study was to measure and analyze the mechanical properties of several composite materials designed for dental restoration. METHODS: The materials were composed of a visible light-curing monomer mixture (either Bis-GMA+TEGDMA or Bis-GMA+HEMA) as a matrix and hydroxyapatite (either microscopic or nanoscopic particles) as a reinforcing filler. The surface of the hydroxyapatite particles was modified by using a coupling agent (citric, malic, acrylic or methacrylic acid). Five specimens of 14 different composites were prepared for each mechanical test: flexural strength, Young's modulus and Vickers hardness. Mean values and standard deviations were calculated, and ANOVA and Student Newman Keuls multiple comparison tests were applied (P < 0.05). RESULTS: The addition of 50-60 wt% of hydroxyapatite particles to the unfilled monomer mixtures led to the increase of both Young's modulus and surface hardness of the material, while the flexural strength decreased. In general, when microscopic instead of nanoscopic hydroxyapatite was used as a reinforcing filler, mechanical properties were favored. The mechanical properties were also improved by adding citric, acrylic or methacrylic acid as a coupling agent. CONCLUSIONS: An adequate surface modification of the hydroxyapatite particles conferred enhanced mechanical properties to the final dental composite. Microscopic-hydroxyapatite particles are preferred to nanoscopic ones.     

Bis-GMA/TEGDMA树脂水解产物分析

目的检测Bis-GMA/TEGDMA树脂片经去离子水浸泡后的水解产物。方法 Bis-GMA/TEGDMA单体加入CQ/DMAEMA后光照聚合制备树脂片,将树脂片经37℃恒温去离子水浸泡24 h,其中在1h、3 h、6 h和24 h四个时间点各取1 mL浸泡液,用乙酸乙酯萃取、旋蒸,通过高效液相色谱质谱法(HPLC/MS)检测分析,确定树脂水解产物。结果树脂片的水解产物为双酚A-二甘油醚(Bis-GMA-2MA)、双酚A-二氧代丙基醚(Bis-GMA-2MA-2H2O)、单甲基丙烯酸二缩三乙二醇酯(TEGDMA-MA)和二缩三乙二醇(TEGDMA-2MA)。结论 Bis-GMA/TEGDMA树脂片经去离子水浸泡后树脂可发生水解,水解产物及残余Bis-GMA/TEGDMA树脂单体可析出并释放到去离子水中。     

The effect of comonomer composition, silane heating, and filler type on aqueous TEGDMA leachability in model resin composites

Experimental composites using either bisGMA/TEGDMA or UEDMA/ TEGDMA matrices, quartz or barium glass fillers, and 2 different filler silanization methods were evaluated regarding monomer leachability in distilled water. The leached amount was detected and quantified using gas chromatography. The results showed that twice as much TEGDMA is leached from a bisGMA/TEGDMA based composite than from an UEDMA/ TEGDMA based composite, when both contain 50 wt% TEGDMA. The hypothesis suggested that the higher degree of cure of UEDMA/TEGDMA based composites would be reflected in a lower monomer leaching value, and this hypothesis was supported by the findings. Whether such a correlation exists within groups of UEDMA/TEGDMA based matrices having different degrees of cure was not determined and needs to be investigated in future studies. Variables such as filler composition and silane treatment did not affect the leaching values of TEGDMA in water. That finding suggests that future studies should target differences in matrices, and that the need for considering effects of filler composition and silane treatment methods should not receive the same priority.     

Network structure of Bis-GMA- and UDMA-based resin systems

OBJECTIVES: The commonly used dental base monomers 2,2-bis[p-(2'-hydroxy-3'-methacryloxypropoxy)phenylene]propane (Bis-GMA) and 1,6-bis(methacryloxy-2-ethoxycarbonylamino)-2,4,4-trimethylhexane (UDMA) require the use of a diluent monomer, such as triethylene glycol dimethacrylate (TEGDMA). The aim of this study was to measure double bond conversion of UDMA/TEGDMA and Bis-GMA/TEGDMA polymeric systems, determine the leachable portion, and analyze network formation by evaluating crosslinking and pendant double bonds. METHODS: UDMA or Bis-GMA was combined with TEGDMA in systematic increments and irradiated to form light cured polymers. Fourier transform infrared spectroscopy in the near-infrared region was used to measure double bond conversion. The leachable sol fraction was analyzed by 1H NMR. Resin composites were formulated. Flexural strength was measured by three-point bending and volumetric shrinkage was determined with a mercury dilatometer. RESULTS: The amount of base monomer greatly influenced double bond conversion, sol fraction, and crosslinking. Increasing base monomer concentration decreased double bond conversion, increased the leachable fraction, and decreased crosslinking and network formation. At mole fractions higher than 0.125, the UDMA polymers had significantly higher conversion than the Bis-GMA polymers. Bis-GMA polymers had higher leachable amounts of unreacted monomer, while UDMA mixtures had more crosslinking than the Bis-GMA mixtures. In regards to the physical properties of resin composites, increasing the base monomer improved flexural strength and decreased volumetric shrinkage. SIGNIFICANCE: This systematic study for the evaluation of conversion, leachability, crosslinking, and network structure along with physical properties, like volumetric shrinkage and flexural strength, are required for the optimization of competing desirable properties for the development of durable materials.     

Evaluation of highly reactive mono-methacrylates as reactive diluents for BisGMA-based dental composites

ObjectivesThis study evaluates the performance of highly reactive novel monomethacrylates characterized by various secondary moieties as reactive diluent alternatives to TEGDMA in BisGMA filled dental resins. We hypothesize that these monomers improve material properties and kinetics over TEGDMA because of their unique polymerization behavior.MethodsThe cure rates and final double bond conversion of the resins were measured using real-time FTIR spectroscopy. The glass transition temperature and storage modulus of the formed polymers were measured using dynamic mechanical analysis. Flexural modulus and flexural strength values were obtained using a three-point bending flexural test.ResultsPolymerization kinetics and polymer mechanical properties were evaluated for the novel resin composites. It was observed that upon the use of novel monomethacrylates as reactive diluents, polymerization kinetics increased by up to 3-fold accompanied by increases in the extent of cure from 5% to 13% as compared to the BisGMA/TEGDMA control. Polymer composites formed from resins of BisGMA/novel monomethacrylates exhibited comparable T_g values to the control, along with 27–37% reductions in the glass transition half widths indicating the formation of more homogeneous polymeric networks. The BisGMA/monomethacrylate formulations exhibited equivalent flexural modulus and flexural strength values relative to BisGMA/TEGDMA.SignificanceFormulations containing novel monovinyl methacrylates exhibit dramatically increased curing rates while also exhibiting superior or at least comparable composite polymer mechanical properties. Thus, these types of materials are attractive for use as reactive diluent alternatives to TEGDMA in dental formulations.     

Rheological properties of experimental Bis-GMA/TEGDMA flowable resin composites with various macrofiller/microfiller ratio

ObjectivesThe purpose of this study was to investigate the rheological behavior of resin composites and to evaluate the influence of each component, organic as well as inorganic, on their viscoelastic properties by testing model experimental formulations.MethodsSeveral unfilled mixtures of 2,2-bis-[4-(methacryloxy-2-hydroxy-propoxy)-phenyl]-propane (Bis-GMA) and triethylene glycol dimethacrylate (TEGDMA) were prepared as well as experimental flowable resin composites using a Bis-GMA/TEGDMA 50/50 wt% mixture as organic fraction filled at 60% in weight with varying ratios of silanated barium glass (1 μm) and partially hydrophobic fumed silica (0.1 μm). Their rheological properties were investigated using dynamic oscillatory rheometers. Transmission electron microscopy (TEM) was also performed to investigate the spatial organization of the filler particles.ResultsUnfilled Bis-GMA/TEGDMA mixtures all showed a Newtonian behavior. The experimental flowable resin composites were non-Newtonian, shear-thinning fluids. As the quantity of microfiller increased, the viscosity increased and the shear-thinning behavior increased as well. In addition, the experimental composites showed thixotropy, i.e. their viscosity is a function of time after deformation. All these properties were not specifically linked to the creation and destruction of a visible network between inorganic particles, as no difference could be seen between particles’ spatial organization at the equilibrium rest state or immediately after deformation.SignificanceThe complex viscoelastic properties of resin composites are due to interactions between microfiller and monomer molecules. Modifying the chemical and physical properties of the particles’ surface could possibly improve their flow properties and thus their clinical handling performances.     

Water sorption and solubility of dental composites and identification of monomers released in an aqueous environment

Water sorption and solubility of six proprietary composite resin materials were assessed, and monomers eluted from the organic matrix during water storage identified. Water sorption and solubility tests were carried out with the following storage times: 4 h, 24 h and 7, 60 and 180 days. After storage, water sorption and solubility were determined. Eluted monomers were analysed by high performance liquid chromatography (HPLC). Correlation between the retention time of the registered peak and the reference peak was observed, and UV-spectra confirmed the identity. The results showed an increase in water sorption until equilibrium for all materials with one exception. The solubility behaviour of the composite resin materials tested revealed variations, with both mass decrease and increase. The resin composition influences the water sorption and solubility behaviour of composite resin materials. The HPLC analysis of eluted components revealed that triethyleneglycol dimethacrylate (TEGDMA) was the main monomer released. Maximal monomer concentration in the eluate was observed after 7 days. During the test period, quantifiable quantities of urethanedimethacrylate (UEDMA) monomer were observed, whereas 2,2-bis[4-(2-hydroxy-3-methacryloyloxypropoxy)-phenyl]propane (Bis-GMA) was only found in detectable quantities. No detectable quantities of bisphenol-A were observed during the test period.