Organic overlayer model of a dental composite analyzed by laser desorption postionization mass spectrometry and photoemission

Some dental composites consist of a polymerizable resin matrix bound to glass filler particles by silane coupling agents. The resin in these composites includes bisphenol A diglycidyl methacrylate (Bis-GMA) as well as other organic components. Silane coupling agents such as 3-(trimethoxysilyl) propyl methacrylate (MPS) have been used to improve the mechanical properties of the dental composites by forming a covalent bond between the glass filler particles and the resin. These resin-glass composites undergo material property changes during exposure to the oral environment, but degradation studies of the commercial composites are severely limited by their chemical complexity. A simplified model of the dental composite has been developed, which captures the essential chemical characteristics of the filler particle-silane-resin interface. This model system consists of the resin matrix compound Bis-GMA covalently bound via a methacryloyl overlayer to amorphous silicon oxide (SiO2) surface via a siloxane bond. Scanning electron microscopy shows the porous characteristic and elemental composition of the SiO2 film, which approximately mimics that of the glass filler particles used in dental composites. LDPI MS and XPS verify the chemistry and morphology of the Bis-GMA-methacryloyl overlayer. Preliminary results demonstrate that LDPI MS will be able to follow the chemical processes resulting from aging Bis-GMA-methacryloyl overlayers aged in water, artificial saliva, or other aging solutions.     

Systematic variation of interfacial phase reactivity in dental nanocomposites

This study was designed to determine the effect of varying the chemistry of the interfacial phase on critical composite properties in dental nanocomposite materials. Silica nanoparticles were silanized with varying ratios of 3-methacryloxypropyltrimethoxysilane (MPTMS) and octyltrimethoxysilane (OTMS) while keeping the total amount of silane constant at 10% by mass fraction relative to the mass of filler. The silanized nanoparticles were mixed into a dimethacrylate resin (60% filler by mass fraction). The mechanical properties of the uncured pastes were assessed by compression testing between parallel plates. The composites were photo-cured and tested by biaxial flexure and three-point bend flexure testing. Fracture surfaces were analyzed by field-emission scanning electron microscopy (FE-SEM). At maximized filler mass fractions, the workabilities of the uncured pastes were better maintained as the fraction of OTMS in the interphase increased relative to MPTMS. The flexure strengths and moduli of the MPTMS silanized and dual silanized composites were similar but decreased as OTMS mass fractions in the silane mixture increased to 7.5% and 10%. FE-SEM images revealed evidence for phase separation in the composites containing silica silanized with high fractions of OTMS. Among the potential practical benefits of dual silanized nanoparticles are the improved workability of composite pastes with higher filler loadings that should lead to higher modulus composites with lower polymerization shrinkage.     

The bond strength of light-curing composite resin to finally polymerized and aged glass fiber-reinforced composite substrate

OBJECTIVE: This study examines the shear bond strength of visible light-curing composite resin (VCR) to aged glass fiber-reinforced composite (FRC) substrate with multi-phase polymer matrix. METHODS: Linear polymethyl methacrylate and dimethacrylate monomer preimpregnated unidirectional glass fiber reinforcement was used as an adhesion substrate for low-viscosity diacrylate veneering composite resin and restorative composite resin. A total of 60 test specimens were divided into three groups according to the brand and the use of an intermediate monomer resin (IMR). The used IMRs were either BisGMA-HEMA-resin, BisGMA-TEGDMA resin or the controls were left without the IMR treatment. Dry- and water-stored FRC-substrates were used for adhering the VCR with or without the IMR. The shear bond strength of the VCR to the substrate was measured for dry and thermocycled specimens and the results were analyzed with multi-variate ANOVA. RESULTS: The highest mean shear bond strength (23.9 +/- 4.8 MPa) was achieved with FRC/BisGMA-HEMA/VCR combination when the FRC substrate was water stored and the test specimen was thermocycled. FRC/BisGMA-TEGDMA/VCR combination resulted in 15.7 +/- 6.0 MPa with the water-stored FRC substrate and after thermocycling of the test specimens. The lowest shear bond strength (1.0 +/- 0.5 MPa) was obtained with FRC/VCR combination with water-stored substrate and after thermocycling of the test specimens. Significant differences were found between the mean values of three groups according to the use of IMR (p<0.001). The storage conditions of the FRC substrate were related to brand of the IMR or the composite (p<0.001). High mean values of the shear bond strength after thermocycling fatigue were related to the type of IMR (p<0.001). SIGNIFICANCE: The results suggest that the IMRs used in this study greatly influence the mean shear bond strength values when the test specimens are thermocycled.     

Assessment of decontamination methods as pretreatment of silanization of composite glass fillers

In terms of mechanical properties and durability, the surface of glass fillers should be decontaminated in order to optimize the silanization process for the production of resin composites. The objective of this study was to evaluate the decontamination efficiency of 18 cleaning methods on glass fillers as pretreatment of silane coupling. X-ray photoelectron spectroscopy revealed that SiO(2) boiled with a 5% sodium peroxodisulfate aqueous solution for 15 min, followed by ultrasonic rinsing with acetone for 30 min was most effective among all the decontamination methods investigated. In addition, nano-indentation measurements on SiO(2) treated by the above-mentioned method revealed that the surface was not significantly weakened as compared to untreated SiO(2). The results of this study should lead to an improved filler-matrix coupling and thus contribute to the development of better wear and fatigue-resistant composites. Therefore, sodium peroxodisulfate is proposed as a presilanization filler decontamination step in the production process of resin composites.     

Mechanical properties of BIS-GMA resin short glass fiber composites

The use of short glass fibers as a filler for dental restorations or cement resins have not been examined extensively. The mechanical properties and untreated glass fibers (5 microns dia x 25 microns) in Bis-phenol A glycidyl methacrylate (BIS-GMA) diluted with triethylene-glycol dimethacrylate (TEGDMA) resin were investigated for possible use as a restorative dental composite or bone cement. Compression, uniaxial tension and fracture toughness tests were conducted for each filler composite mixtures of 40, 50, 60 and 70%. Set time and maximum temperature of polymerization were determined. The results show that the elastic modulus, tensile strength and compressive strength are dependent on the percent of filler content. Elastic modulus and compressive yield (0.2%) strength of silane treated glass fibers filled composite increased from 2.26 to 4.59 GPa and 43.3 to 66.6 MPa, respectively, wtih increasing the filler content while the tensile strength decreased from 26.7 to 18.6 MPa. The elastic modulus of the untreated composite was less than that of the silane treated fiber composite. The tensile strength and compressive strengths were 20 to 50% lower than those of silane treated composites. The fracture toughness of the silane treated glass fiber additions were not significantly different from the untreated additions. The highest fracture toughness was obtained at 50% filler content with 1.65 MPa m.5. Set time increased from 3.5 to 7.7 minutes with increased filler content and peak temperature dropped from 68.3 to 34 degrees C. The results of this study indicate that the addition of silane coated glass fiber to BIS-GMA resin increased the elastic modulus, tensile and compressive strengths compared with non-treated fibers. The addition of either treated or non-treated fibers increased the set time of the material and decreased the maximum temperature.     

Laser-induced acoustic emissions in experimental dental composites

A laser thermoacoustic technique was innovated to evaluate laser-induced acoustic emissions (AEs) in experimental dental composites aged with 75% ethanol solution. Experimental composite systems of 75/25 BisGMA/TEGDMA resin filled with 0, 12.6, 30.0, and 56.5 vol% of 8-microm silanized and unsilanized BaSiO6 were analyzed. The sample size was 4.65 mm (diameter) x 0.5 mm (thick). Aging effects of immersing in 75% ethanol for up to 14 h on AEs were then evaluated. A continuous-wave CO2 laser was used to heat the samples. Acoustic emissions were collected as a function of filler fraction, laser power, silanization, and immersion time. Onset of burst-pattern acoustic signals characteristic of fracturing occurred at different laser powers for different tested groups. Acoustic emissions generally increased with laser power, in which lower laser powers produced low-amplitude (45-50 dB) signals; the amplitude distribution (50-85 dB) became more extensive as laser powers increased. After immersion, the lower laser powers could produce the same phenomenon. The higher the filler fraction, the fewer AEs generated. A large percentage AE reduction due to silanization was noted as a function of filler fraction. Unsilanized specimens showed more thermal damages than did silanized ones.     

Evaluation of the fatigue behavior of the resin-dentin bond with the use of different methods

The clinical performance of directly bonded resin composites is fundamentally dependent on durable adhesion to prevent gap formation over time. The goal of this investigation was to evaluate the effectiveness of various dentin adhesives by means of quasistatic and dynamic dentin bond strengths, and also to determine marginal and internal gap formation after loading in an artificial oral environment. Three hundred thirty human third molars were used within four weeks of extraction. Adhesives used were A.R.T. Bond, OptiBond FL, Scotchbond Multi-Purpose Plus, Single Bond, Prime & Bond NT, and One Up Bond F for bonding of one resin composite (Z 250). Buccal and lingual aspects of 90 teeth were ground flat to expose dentin, then resin composite cylinders were bonded. Initial bond strengths (n = 10) and adhesive fatigue limits (n = 20) were determined with the use of a shear test apparatus. One hundred eighty conical cavities were prepared into dentin discs and filled with the same materials. After 21 days of storage, initial push-out bond strengths (n = 10) and adhesive fatigue limits (n = 20) were measured. Sixty molars with MO cavities (n = 10) with margins below the cement-enamel junction were filled. Before and after thermomechanical loading (100000 x 50 N and 2500 x thermocycling between + 5 and + 55 degrees C), marginal gap formation and internal adaptation (only after loading) were analyzed under a SEM (x 200). The one-bottle systems showed higher shear bond strengths when evaluated statically and dynamically. However, cyclic fatigue push-out bond strengths resulted in higher values for older multistep systems. Marginal and internal gap analysis confirmed the results, in favor of older adhesive systems (p <.05; Mann-Whitney U test).     

Volumetric contraction and methacrylate conversion in photo-polymerized amorphous calcium phosphate/methacrylate composites

Because of its relatively high solubility in aqueous media and its rapid transformation to hydroxyapatite, amorphous calcium phosphate (ACP) has been utilized as the filler phase of resin-based bioactive composites that have remineralization potential. The objectives of this study were to determine how various methacrylate resins and various types of ACP fillers affect acrylic vinyl conversion and polymerization shrinkage (PS). Several types of photo-crosslinkable resin systems were prepared and admixed with a mass fraction of 40% of either unhybridized, silica- or zirconia-hybridized ACP. After visible light-activated photo-polymerization ACP composites were assessed by near infrared spectroscopy for degree of vinyl conversion and by mercury dilatometry for PS. It was found for these composites that vinyl conversion was independent of filler type but strongly dependent on the type and composition of the resin phase. PS, on the other hand, showed more complex dependence both on the resin type and composition and, in some cases, on the type of ACP. In order to obtain ACP/methacrylate-based composites with maximal vinyl conversion, resin type and composition are of primary importance. However, in order to minimize volume contraction on polymerization it appears necessary to consider both the resin and filler type of these bioactive composites.     

Whisker-reinforced bioactive composites containing calcium phosphate cement fillers: effects of filler ratio and surface treatments on mechanical properties

Calcium phosphate cement (CPC) sets to form microporous solid hydroxyapatite with excellent osteoconductivity, but its brittleness and low strength prohibit use in stress-bearing locations. The aim of this study was to incorporate prehardened CPC particles and ceramic whiskers in a resin matrix to improve the strength and fracture resistance, and to investigate the effects of key microstructural variables on composite mechanical properties. Two types of whiskers were used: silicon nitride, and silicon carbide. The whiskers were surface-treated by fusing with silica and by silanization. The CPC particle fillers were either silanized or not silanized. Seven mass ratios of whisker-silica/CPC were mixed: 0:1 (no whisker-silica), 1:5, 1:2, 1:1, 2:1, 5:1, and 1:0 (no CPC). Each powder was blended with a bisphenol-a-glycidyl methacrylate-based resin to harden in 2 x 2 x 25 mm molds by two-part chemical curing. The specimens were tested in three-point flexure to measure strength, work-of-fracture (toughness), and elastic modulus. Two-way analysis of variance was used to analyze the data, and scanning electron microscopy was used to examine specimen fracture surfaces. The whisker-silica/CPC ratio had significant effects on composite properties (p < 0.001). When this ratio was increased from 0:1 to 1:0, the strength was increased by about three times, work-of-fracture by five times, and modulus by two times. Whisker surface treatments and CPC filler silanization also had significant effects (p < 0.001) on composite properties. Scanning electron microscopy revealed rough fracture surfaces for the whisker composites with steps and whisker pullout. Resin remnants were observed on the surfaces of the pulled-out whiskers, indicating strong whisker-matrix bonding. In conclusion, incorporating highly osteoconductive CPC fillers and ceramic whiskers yielded composites with substantially improved mechanical properties compared with composites filled with CPC particles without whiskers. The composite properties were determined by whisker-to-CPC ratio and filler surface treatments.     

Finite element analysis of thermo-debonding mechanism in dental composites

Finite element method (FEM) has been extensively used for evaluating interfacial status inside biomaterials. This study using FEM was designed to evaluate the thermal stress behavior of a filler-matrix interface. The results were then compared to those of a previous study obtained by a laser thermoacoustic technique (LTAT). The experimental systems (75/25 Bis-GMA/TEGDMA resin reinforced with 0, 25, 50, and 75 wt% 8-microm silanized/unsilanized BaSiO6) as used in the previous study were modeled in this study. The established finite element models were based on coefficient of thermal expansion (CTE) Mismatch Phenomenon. The mechanical properties of the silane coupling agent, such as elastic modulus and thermal expansion coefficient used in the silanized model, were assumed to have optimal heat flux transfer. A third (imaginary) material was proposed to block the transfer of thermal stress between the filler and matrix in the unsilanized model. The thermal load simulation was based on steady-state thermal analysis. The results showed that: (1) The strain energy and interfacial shearing stress calculated from FEM validate the results from the previous LTAT study. (2) Comparing the stress distribution of silanized and unsilanized FEM models, the acoustic signals in LTAT study are mainly derived from debonding of the filler-matrix interface of silanized specimens, and from the matrix area of unsilanized specimens. Based on results to date, we conclude that the finite element method may be a powerful tool for exploring thermoacoustic mechanisms of dental composites.     

The effects of three different desensitizing agents on the shear bond strength of composite resin bonding agents

The aim of this study was to evaluate the effects of three desensitizing agents on the shear bond strengths of four different bonding agents used to bond composite resin to dentin.A total of 160 extracted human molars were sectioned parallel to the occlusal plane under water cooling, polished and randomly divided into 4 groups of 40. Each group was treated with a different desensitizing agent (Tooth Mousse, Ultra-EZ, Cervitec Plus), except for an untreated control group. Each group was then randomly subdivided into 4 groups of 10, and a different dentin bonding agent (XP Bond, AdheSE, Adper Prompt L-pop, GBond) was applied to each group in order to bond the specimens to a resin composite (Gradia Direct) built up using a plastic apparatus. A Universal Testing Machine was used to measure the shear bond strength of each specimen. Statistical analysis was performed using one-way ANOVA and Tukey’s tests.With the exception of the Control/AdheSE and Ultra-EZ/XP Bond groups, no statistically significant differences were found in the shear bond strength values of the groups tested. These findings suggest that the use of different desensitizing agents does not affect the shear bond strength of various adhesive systems used to bond resin composite to dentin.     

Characterization and inhibitory effect of antibacterial dental resin composites incorporating silver-supported materials.

Resin composites with antibacterial activity may be useful for preventing the secondary caries frequently seen around restorations. The purposes of this study were to investigate antibacterial light-activated dental resin composites incorporating each of two silver-supported antibacterial materials and evaluate their long-lasting inhibitory effect against Streptococcus mutans. Two types of silver-supported antibacterial materials, Novaron (N) and Amenitop (AM) were used. These antibacterial materials were incorporated into TEGDMA-UDMA-based light-activated resin composites, and the antibacterial activities and mechanical properties of these composites, and also the release of silver ions, were examined. Two silver-supported antibacterial materials inhibited the growth of the major oral pathogen S. mutans. The minimum inhibitory concentration in suspensions of N and AM against S. mutans was 40 microg/mL and 30 microg/mL, respectively. Composites incorporating 5 wt % (N-5) or more of Novaron and 7 wt % (AM-7) or more of Amenitop inhibited the growth of S. mutans after immersion in water for 6 months. There was no or extremely little release of silver ions from the N-5 and AM-7 composites after 1 day or after 6 months of immersion in water. No significant difference in either compressive or flexural strength was observed between the control and the N-5 composites after 1 day or after 6 months of storage in water. However, for the AM-5 composite, there was a significant difference in both strength parameters between the two immersion periods. These results indicate that a light-activated dental resin composite incorporating silver-supported antibacterial material such as Novaron may be useful clinically because of its long-lasting inhibitory effect against S. mutans and its favorable mechanical properties.     

Effect of cyclic loading and environmental aging on the fracture toughness of dental resin composite

OBJECTIVE: The main purpose of this study was (1) to investigate the effects of cyclic loading and environmental aging on three dental resin composites with different filler compositions: a fiber filler, a hybrid filler, and a microfill; and (2) to predict fracture in dental resin composite under mixed-mode loading conditions. METHODS: Diametral disk specimens 25 mm in diameter and 2 mm in thickness were used in this study. Two methods were used for generating initial cracks in the specimen. The first method involved machining a 3-mm notch in the center of the disk specimens, and then the notch tips were sharpened with a 0.2-mm-diameter jeweler's saw blade. In the second method for obtaining sharper crack tips, a three-way wedge was forced into a 3.175-mm hole drilled in the center of the specimen, resulting in sharp cracks emanating from the notch tips. CYCLIC TESTS: The specimens were aged for 4 months in air, water, artificial saliva, and a 50/50 (by volume) mixture of ethanol and water at room temperature in sealed polyethylene containers. Both unaged and aged specimens (5 specimens for each variable) were subjected to cyclic loading at a frequency of 5 Hz with sinusoidal loads cycling for 1, 1000, and 100,000 cycles at a load level approximately 60% of the fracture load for noncycled specimens. Following load cycling, the specimens were tested in compression in a displacement-controlled loading mode at a loading rate of 1.27 mm/min. RESULTS: Test results show that aging in a 50/50 alcohol-water mixture lowered the fracture toughness of dental resin composite, which was further reduced by cyclic loading. MIXED-MODE TESTS: The maximum tensile stress (MTS) criterion was used to predict fracture in dental resin composite under mixed-mode loading conditions. The loads at failure were used as input into a finite element model. After obtaining the stress field in the specimens by the finite element method, the mixed-mode stress intensity factors were calculated using an interaction energy integral method. RESULTS: Good agreement was obtained between the fracture envelope predicted by the MTS criterion and the experimental fracture toughness data. Hence, it can be concluded that it is only necessary to characterize the mode I fracture toughness to fully characterize the mixed-mode behavior of the dental resin composites that were considered in the present study.     

Correlation of cytotoxicity, filler loading and curing time of dental composites.

Previous studies have shown that dental resin composites tested in cell culture produce cytotoxic effects on human gingival tissues. In this study, the cytotoxic potential of resin composites on primary human gingival fibroblast cultures was evaluated, based on inhibition of cellular protein synthesis measured by [35S] methionine incorporation. Both resin content and percentage of monomer conversion were considered as potential causes of cytotoxicity. Three resin composites were selected to provide a range of filler content from 45 to 86 wt%. Duplicate sample discs (1 mm thick x 10 mm diameter) of each composite were polymerized for 15, 30 and 60 s, followed by heat (110 degrees C, 10 min), and the degree of monomer conversion for each sample group was measured using Fourier transform infrared spectrophotometry. Identically fabricated discs were placed into 35 mm culture dishes with gingival fibroblasts and incubated for 24 h at 37 degrees C. The cell monolayers then were labelled at 24 h with [35S] methionine, washed and solubilized; then incorporated radioactivity was quantitated by liquid scintillation spectrometry. For each composite, as the percentage of monomer conversion increased, cellular toxicity decreased. In comparing different composites having similar monomer conversions, it was found that the filler/resin ratio was not the only factor determining the composite's relative toxicity.     

Changes in color and translucency of porcelain-repairing resin composites after thermocycling

The objective of this study was to determine the changes in color and translucency of dental porcelain-repairing resin composites compared to dental porcelain after thermocycling. Color and spectral reflectance of three shades (A2, A3, and A3.5) of one brand of dental porcelain and three basic shades (A2, A3, and A3.5) and three combinations (A2/A3, A3/3.5, and A2/A3.5) of three brands of porcelain-repairing resin composites (ABT, FSP, and TCR) were measured, before and after thermocycling for 3000 cycles, relative to the illuminant D65. The specimen was 2 mm in thickness, and 1 mm of each shade was layered to make combined shades. Changes in color (DeltaE*ab) and translucency parameter (DeltaTP) were calculated. A general linear model by the material (porcelain or resin composite) and shade was used to compare differences (alpha = 0.05). The range of color changes was 0.68-1.67 in porcelain, 0.56-1.30 in ABT, 2.28-3.10 in FSP, and 0.36-1.15 in TCR. The range of DeltaTP was 0.45-0.96 in porcelain, -0.48 to 0.94 in ABT, -1.31 to 0.82 in FSP, and -0.51 to 1.91 in TCR. After thermocycling, changes in color and TP were correlated with the shade of the material, but not with the material. The discrepancy in the changes of color and translucency after thermocycling between porcelain and porcelain-repairing resin composites should be considered when selecting repairing materials.     

Silica coatings formed on noble dental casting alloy by the sol-gel dipping process.

The sol-gel dipping process, in which liquid silicon alkoxide is transformed into the solid silicon-oxygen network, can produce a thin film coating of silica (SiO2). The features of this method are high homogeneity and purity of the thin SiO2 film and a low sinter temperature, which are important in preparation of coating films that can protect from metallic ion release from the metal substrate and prevent attachment of dental plaque. We evaluated the surface characteristics of the dental casting silver-palladium-copper-gold (Ag-Pd-Cu-Au) alloy coated with a thin SiO2 film by the sol-gel dipping process. The SiO2 film bonded strongly (over 40 MPa) to Ti-implanted Ag-Pd-Cu-Au alloy substrate as demonstrated by a pull test. Hydrophobilization of Ti-implanted/SiO2-coated surfaces resulted in a significant increase of the contact angle of water (80.5 degrees) compared with that of the noncoated alloy specimens (59.3 degrees). Ti-implanted/SiO2-coated specimens showed the release of many fewer metallic ions (192 ppb/cm2) from the substrate than did noncoated specimens (2,089 ppb/cm2). The formation of a thin SiO2 film by the sol-gel dipping process on the surface of Ti-implanted Ag-Pd-Cu-Au alloy after casting clinically may be useful for minimizing the possibilities of the accumulation of dental plaque and metal allergies caused by intraoral metal restorations.     

Evaluation of a new fiber-reinforced resin composite

Efficacy of the usage of an experimental fiber-reinforced composite (FRC) on mechanical properties of an indirect composite was investigated by means of three-point bending and Charpy impact tests. Bond strength between the FRC and the indirect composite was also evaluated by tensile testing. The FRC consisted of a matrix resin with 25% silanized milled glass fiber (11-microm diameter, 150-microm length) and 5% colloidal silica. The values of strain of proportional limit, total strain, and fracture energy of the FRC during the bending test (1.2%, 10.4%, and 41.6 x 10(-3) J) were significantly higher than those of the indirect composite (0.1%, 2.5%, and 11.9 x 10(-3) J). The impact strengths of the 1-mm specimens with FRC ranged from 15.2 to 15.9 kJ/m(2), and were significantly higher than that of the control (3.1 kJ/m(2)). The 2-mm specimens showed significant difference from the control when the FRC thickness was equal or greater than 0.5 mm. The bond strength after the thermocycling was 15.2 MPa, and all of the specimens exhibited cohesive fracture inside the indirect composite. Based upon the results, it was concluded that the FRC tested in this study improved toughness and impact resistance of the indirect composite. The interfacial bonding between the FRC and the indirect composite was strong enough to prevent delamination.     

Dental resin composites containing silica-fused whiskers--effects of whisker-to-silica ratio on fracture toughness and indentation properties.

Dental resin composites need to be strengthened in order to improve their performance in large stress-bearing applications such as crowns and multiple-unit restorations. Recently, silica-fused ceramic whiskers were used to reinforce dental composites, and the whisker-to-silica ratio was found to be a key microstructural parameter that determined the composite strength. The aim of this study was to further investigate the effects of whisker-to-silica ratio on the fracture toughness, elastic modulus, hardness and brittleness of the composite. Silica particles and silicon carbide whiskers were mixed at whisker:silica mass ratios of 0:1, 1:5. 1:2, 1:1, 2:1, 5:1, and 1:0. Each mixture was thermally fused, silanized and combined with a dental resin at a filler mass percentage of 60%. Fracture toughness was measured with a single-edge notched beam method. Elastic modulus and hardness were measured with a nano-indentation system. Whisker:silica ratio had significant effects on composite properties. The composite toughness (mean+/-SD; n = 9) at whisker:silica = 2:1 was (2.47+/-0.28) MPa m(1/2), significantly higher than (1.02+/-0.23) at whisker:silica = 0:1, (1.13+/-0.19) of a prosthetic composite control, and (0.95+/-0.11) of an inlay/onlay composite control (Tukey's at family confidence coefficient = 0.95). Elastic modulus increased monotonically and hardness plateaued with increasing the whisker:silica ratio. Increasing the whisker:silica ratio also decreased the composite brittleness, which became about 1/3 of that of the inlay:onlay control. Electron microscopy revealed relatively flat fracture surfaces for the controls, but much rougher ones for the whisker composites, with fracture steps and whisker pullout contributing to toughness. The whiskers appeared to be well-bonded with the matrix, probably due to the fused silica producing rough whisker surfaces. Reinforcement with silica-fused whiskers resulted in novel dental composites that possessed fracture toughness two times higher than, and brittleness less than half of current dental composites.     

Whisker-reinforced dental core buildup composites: effect of filler level on mechanical properties

The strength and toughness of dental core buildup composites in large stress-bearing restorations need to be improved to reduce the incidence of fracture due to stresses from chewing and clenching. The aims of the present study were to develop novel core buildup composites reinforced with ceramic whiskers, to examine the effect of filler level, and to investigate the reinforcement mechanisms. Silica particles were fused onto the whiskers to facilitate silanization and to roughen the whisker surface for improved retention in the matrix. Filler level was varied from 0 to 70%. Flexural strength, compressive strength, and fracture toughness of the composites were measured. A nano-indentation system was used to measure elastic modulus and hardness. Scanning electron microscopy (SEM) was used to examine the fracture surfaces of specimens. Whisker filler level had significant effects on composite properties. The flexural strength in MPa (mean +/- SD; n = 6) increased from (95+/-15) for the unfilled resin to (193+/- 8) for the composite with 50% filler level, then slightly decreased to (176+/-12) at 70% filler level. The compressive strength increased from (149+/-33) for the unfilled resin to (282+/-48) at 10% filler level, and remained equivalent from 10 to 70% filler level. Both the modulus and hardness increased monotonically with filler level. In conclusion, silica particle-fused ceramic single-crystalline whiskers significantly reinforced dental core buildup composites. The reinforcement mechanisms appeared to be crack deflection and bridging by the whiskers. Whisker filler level had significant effects on the flexural strength, compressive strength, elastic modulus, and hardness of composites.     

Effect of surface treatment on the shear bond strength of three resin cements to a machinable feldspatic ceramic

The aim of this study was to evaluate the shear bond strength of three resin cements to Vita Mark II ceramics under different pretreatments of the ceramic surface and to examine whether simplified pretreatment procedures would result in satisfying results compared to the state of the art. RelyX Unicem (RXU), Calibra (CAL), and Variolink II (VAR) were used as resin cements and bonded to machine milled feldspatic disks, pretreated in five different ways. (1) no pretreatment of the ceramic surface; (2) surface etched with hydrofluoric acid (HF); (3) ceramic surface silanized; (4) ceramic surface etched (HF) and silanized, (5) ceramic surface etched (HF), silanized, and covered with Heliobond. The shear bond strengths were measured initially, after 5000 and 10,000 thermocycles (TC). After 10,000 TC for CAL only procedure 5 resulted in a reliable adhesion median value of 10.7 MPa. VAR showed median values of 24.6, 17.2, and 18.1 MPa for pretreatments 5, 3, and 4, respectively. RXU performed 25.9, 22.0, and 11.0 MPa for procedures 5, 4, and 3, respectively. For procedure 2, RXU revealed the significantly highest value with 15.4 MPa (U-test, p = 0.05). Only RXU-luted specimens of procedure 1 survived the 10,000 thermocycles. The results revealed that a simplification of the ceramic pretreatment for VAR and RXU might be possible.