Influence of radiant exposure on contraction stress, degree of conversion and mechanical properties of resin composites.

OBJECTIVE: To verify the influence of radiant exposure (H) on contraction stress (CS), degree of conversion (DC) and mechanical properties of two restorative composites. METHODS: Filtek Z250 (3M ESPE) and Heliomolar (Ivoclar) were photoactivated with 6, 12, 24, or 36 J/cm2 at continuous irradiance of 600 mW/cm2. CS at 10 min was determined in a low compliance testing system. DC, flexural strength (FS), flexural modulus (FM) and Knoop microhardness (KHN) were measured after 24 h storage at 37 degrees C. KHN and DC measurements were conducted on the irradiated surface of 1mm thick disk-shaped specimens. Bar-shaped specimens were submitted to three-point bending to determine FS and FM. Data were analyzed by one-way ANOVA/Tukey's test (alpha = 0.05) separately for each composite. RESULTS: For Filtek Z250, no significant increase in CS was observed above 12 J/cm2. DC and FM were similar at all H values, while FS increased significantly between 6 and 24 J/cm2. KHN was significantly different among all H levels, except between 12 and 24 J/cm2. For Heliomolar, CS and KHN increased significantly with H, except between 24 and 36 J/cm2. DC, FM and FS did not vary, regardless of the radiant exposure. SIGNIFICANCE: Variables tested behaved differently. CS and KHN were more sensitive to increasing radiant exposures than the other properties evaluated. FS varied only for Filtek Z250, while, for both composites, DC and FM were not affected by different H values.     

Irradiance effects on the mechanical properties of universal hybrid and flowable hybrid resin composites.

OBJECTIVES: A potential problem with high-intensity lights might be failure of polymer chains to grow and cross-link in a desired fashion, thereby affecting the structure and properties of the polymers formed. The purpose of this study was to evaluate mechanical properties of resin composites polymerized using four different light-curing units. METHODS: A conventional quartz-tungsten-halogen (QTH) light, a soft-start light, an argon-ion laser, and a plasma-arc curing light were used to polymerize disk-shaped (9.0mm diameter x 1.0 mm high) and cylinder-shaped (4mm diameter x 8 mm high) specimens of a universal hybrid and a flowable hybrid composite. Biaxial flexure strength, fracture toughness, hardness, compressive strength, and diametral tensile strength were determined for each composite. RESULTS: The use of the plasma-arc curing light, a high-intensity light, resulted in significantly lower hardness for the universal hybrid composite compared with the hardness obtained using the conventional QTH and the soft-start units. Hardness was the only mechanical property that was adversely affected by the use of a high-intensity light. SIGNIFICANCE: High-intensity lights might affect some resin composite mechanical properties, but this effect cannot be generalized to all resin composites and all properties.     

Reduced polymerization stress of MAPO-containing resin composites with increased curing speed,degree of conversion and mechanical properties

Objectives

The degree and rate of photopolymerization in resin-based dental composites will significantly affect polymer network formation and resultant material properties that may determine their clinical success. This study investigates the mechanical properties, the generation of stress from polymerization, tooth cusp deflection and marginal integrity of experimental resin composites that contain different photoinitiators.

Methods

Experimental light-activated resin composites (60 vol% particulate filled in 50/50 mass% bis-GMA/TEGDMA) were formulated using a monoacylphosphine oxide (MAPO) photoinitiator and compared with a conventional camphoroquinone (CQ)-based system. Similar radiant exposure was used (18 J cm⁻²) for polymerization of each material although the curing protocol was varied (400 mW cm⁻² for 45 s, 1500 mW cm⁻² for 12 s and 3000 mW cm⁻² for 6 s). Degree and rate of polymerization was calculated in real-time by near infrared spectroscopy and the generation of stress throughout polymerization measured using a cantilever beam method. Flexural strength and modulus were acquired by three-point bend tests. Standardized cavities in extract pre-molar teeth were restored with each material, the total cuspal deflection measured and post-placement marginal integrity between the tooth and restoration recorded.

Results

Generally, MAPO- exhibited a significantly higher degree of conversion (72 ± 0.8 to 82 ± 0.5%) compared with CQ-based materials (39 ± 0.7 to 65 ± 1.6%) regardless of curing protocol (p < 0.05) and MAPO-based materials exhibited less difference in conversion between curing protocols. CQ-based materials exhibited between ∼85 and 95% of the maximum rate of polymerization at <15% conversion, whereas MAPO-based RBCs did not approach the maximum rate until >50% conversion. Higher irradiance polymerization had a significant deleterious effect on the mechanical properties of CQ-based materials (p < 0.05) whereas MAPO-based materials exhibited increased strength and modulus and were less affected by the curing method. Total cuspal deflection in restored extracted teeth was higher for CQ- compared with MAPO-based materials cured at the lowest irradiance curing protocol (12.9 ± 4.0 and 8.3 ± 1.5 μm) and similar at 3000 mW cm⁻¹ for 6 s (10.1 ± 3.5 and 9.0 ± 1.5 μm). A significant decrease in marginal integrity was observed for CQ-based RBCs cured at high irradiance for short exposure time compared with that of the MAPO-based RBC cured using a similar protocol (p = 0.037).

Significance

Polymer network formation dictates the final properties of the set composite and the use MAPO photoinitiators may provide an effective restorative material that exhibits higher curing speeds, increased degree of conversion, strength and modulus without compromise in terms of polymerization stress and marginal integrity between tooth and restoration.     

Correlation between degree of conversion, filler concentration and mechanical properties of posterior composite resins

The degree of conversion, filler concentration and mechanical properties of seven proprietary light-cured posterior composite resins were investigated. The degree of conversion of composites ranged from 43.5-73.8%. The weight fraction of filler that was obtained was in the range 66.4-85.2%. The volume fraction varied from 58.2-74.2%. The mean values of the observed compressive and diametral tensile strengths ranged from 242.3-324.7 MPa and from 39.8-62.6 MPa, respectively. The Knoop hardness numbers ranged from 41.8-81.9. Significant correlations were observed between the volume fraction of filler and the diametral tensile strength (r = 0.89), and between the volume fraction of filler and the Knoop hardness number (r = 0.89). No correlation was found between the degree of conversion and any of the mechanical properties of the composite resins tested. Because of the positive correlations between the volume fraction of filler and the diametral tensile strength, and between the volume fraction of filler and the Knoop hardness numbers, it is concluded that the filler concentration plays a prominent role in determining the properties of contemporary posterior composite resins.     

Influence of curing modes on the degree of conversion and mechanical parameters of dual-cured luting agents

PurposeTo investigate the effects of different curing modes, including tack cure, on the degree of conversion (DC) and mechanical parameters of dual-cured luting agents for all-ceramic restorations.MethodsImmediate light curing, intermittent light curing (2-s tack cure and a 1-min interval before the main cure), delayed light cuing (2-min delay) and chemical or no light curing were used to cure two dual-cured luting agents, RelyX Unicem and PermaCem 2.0, through a 1.5-mm thick lithium disilicate ceramic slide. DC (n = 3), micro-hardness (n = 5), shrinkage strain (n = 4) and shrinkage stress (n = 3) were measured under the aforementioned curing modes. The data were analyzed using two-way ANOVA and post-hoc Tukey HSD test, with the level of significance set at α = 0.05.ResultsFor both luting agents, all the light-curing modes produced similar final DC, but using chemical cure only could significantly reduce the DC. The mechanical parameters followed a similar pattern. There were positive but nonlinear correlations between DC and the other mechanical parameters, with the increase in these parameters with DC being slower initially.ConclusionsProvided adequate light curing is applied to a dual-cured luting agent, delaying the light curing or using a tack cure first to facilitate seating of a restoration may not have a significant impact on the luting agent’s final degree of conversion. However, using chemical cure only may result in inadequate cure of the luting agent and is recommended only for highly opaque restorations.     

Influence of ketones on selected mechanical properties of resin composites.

The present study investigated a concept for additional cross-linking of dental polymers, by which resistance to wear of resin composites might be increased. Bifunctional ketones were added to monomer mixtures, which were then made light-curing and loaded with filler. The monomer mixtures were varied with respect to type and ratio of monomer and ketone. For measurement of possible effects of the cross-linking agents added, four mechanical properties of the experimental resin composites were determined. Addition of the bifunctional ketone diacetyl resulted in the following increases in mechanical properties: diametral tensile strength, 11%; flexural strength, 29%; modulus of elasticity, 19%; and modulus of resilience, 50%.     

Influence of aldehydes on selected mechanical properties of resin composites.

The present study investigated whether propanol, a monofunctional aldehyde, was able to improve the mechanical properties of dental polymers. The underlying hypothesis was that a cross-linking reaction is possible between various functional groups of different polymers. Propanol was added to monomer mixtures, which were then made light-curing and loaded with filler. The monomer mixtures were varied with respect to monomer composition and content of aldehyde. Four mechanical properties of the experimental resin composites were determined. Addition of propanol gave rise to significant improvements in mechanical properties, which may be indicative of a cross-linking ability of monofunctional aldehydes. With the exception of modulus of elasticity, the mechanical properties of resin composites based on UEDMA/HEMA were superior to those of BISGMA/TEGDMA-based materials, even though the improvements in flexural strength and modulus of resilience were most pronounced for the BISGMA/TEGDMA-based resin composites.     

Effect of chemical and mechanical degradation on surface roughness of three glass ionomers and a nanofilled resin composite

SUMMARY Nanofillers have been incorporated into glass ionomer (GI) restorative materials to improve their mechanical and surface properties. The aim of this present laboratory study was to compare the superficial roughness (Ra) of nanofilled GI (Ketac N100) with that of conventional GI (Fuji IX GP), resin-modified GI (Vitremer), and a nanofilled resin composite (Filtek Supreme) after pH cycling and toothbrush abrasion. Ten specimens of each material were made using Teflon molds, which were polished using aluminum-oxide abrasive disks. Three measurements of Ra were made of each specimen to serve as baseline values. The specimens were submitted to pH cycling for 10 days in a demineralization solution for six hours (pH 4.3) and were then stored in remineralization solution for 18 hours (pH 7.0). Ra measurements were recorded after the pH cycling. Specimens were then submitted to toothbrush abrasion in a brushing machine with a 200g load for 30,000 cycles at 250 cycles/min. The Ra values were then recorded. The surface morphology of specimens from each group was analyzed using a scanning electron microscope. Data were analyzed by analysis of variance, Tukey, and t-tests. After toothbrushing, only Fuji IX GP (1.10 ± 0.80) showed Ra values that were statistically different from those of the other materials evaluated. Ketac N100 (0.68 ± 0.16) showed intermediate Ra values, but it did not differ statistically from the results associated with Vitremer (1.04 ± 0.46) and Filtek (0.30 ± 0.15). Ketac N100 showed intermediate values of superficial roughness among the conventional glass ionomer cement, resin-modified glass ionomer cements, and the nanofilled resin after chemical and mechanical degradation.     

Effect of time and polymerization cycle on the degree of conversion of a resin composite

The aim of this investigation was to verify the influence of 3 light curing units on the degree of conversion, using different irradiation conditions: 1) manufacturers' recommended times of photo-activation, 2) standardizing total energy density among the units and 3) standardizing energy density at the 450-490 nm wavelength range among the units and the effect of these irradiation conditions on the post-cure. Three light curing units were used: halogen, light emitting diodes (LED) and xenon plasma. Seven groups were tested (n=6). Twenty-four hours after the photo-activation procedures, half of the composite specimens were submitted to Fourier Transformed Infrared Spectroscopy analysis. The other half was analyzed after 1 month. The results were submitted to 2-way ANOVA and Tukey's test (5%). Twenty-four hour analysis revealed that the second set of irradiation conditions produced a similar degree of conversion among the LCUs. After 1 month, the conversion values were statistically higher for 20 seconds of halogen exposure (increased from 46.78 to 49.66%), 20 seconds of LED exposure (from 46.20 to 51.15%), 30 seconds of LED exposure (from 48.29% to 50.68%) and 3 seconds of PAC exposure (from 42.57 to 51.39%). The initial degree of conversion and post-cure depended on the photo-activation condition applied.     

Heat curing of UTMA-based hybrid resin: effects on the degree of conversion and cytotoxicity

This study was designed to determine the effects of the heat curing time on a urethane tetramethacrylate (UTMA)-based hybrid resin and specifically on the degree of conversion (DC) and cytotoxicity. The materials used in this study were Estenia, a new-generation hybrid resin, and an experimental fiber reinforcement, Br-100. The DC values of the hybrid resin samples were measured using a Fourier transform infrared (FTIR) spectrophotometer after 180s of light curing followed by heat curing (0, 15, 30, and 60min). A method comparing intensities of C = C and N—H vibrations of the sample was used to calculate the final DC values. FTIR spectra were measured both inside and on the surface of the sample. The calculated DC values increased by increasing the heat curing times. After light curing only and after 15-min heat curing, the DC values inside the samples were smaller than the corresponding DC values at the surfaces of the samples. After 60min of heat curing, the samples achieved homogeneous polymerization (DC% = 65). The cytotoxicity of the material was studied from the glass fiber-reinforced hybrid resin samples, which were first light cured and then heat cured (15, 30, and 60min). Cytotoxicity was tested using both direct contact and extract methods. For the extract tests, the test specimens were incubated in a cell culture media at 37°, 54°, or 72°C for 24h. The heat curing times used had no effect on cytotoxicity. The incubation temperature, however, did have a significant effect. The extract obtained from 72°C incubation showed a cytotoxic effect whereas the others did not. The direct contact test did not show cytotoxicity.     

A Fourier transform Raman spectroscopy analysis of the degree of conversion of a universal hybrid resin composite cured with light-emitting diode curing units

The degree of conversion (DC), of a universal hybrid resin composite cured with LED curing units with low and high power densities and a 510 mW/cm2 quartz tungsten halogen unit, was investigated with Fourier Transform Raman spectroscopy. Three curing depths (0, 2, 4mm) and 0 and 7 mm light guide tip - resin composite (LT - RC) distances were tested. The DC of the LED units varied between 52.3% - 59.8% at the top surface and 46.4% - 57.0% at 4 mm depth. The DC of specimen cured with a 0 mm LT- RC distance at 4 mm depth varied between 50.8% - 57.0% and with 7 mm distance between 46.4% - 55.4%. The low power density LED unit showed a significantly lower DC for both distances at all depth levels compared to the other curing units (p < 0.05). Significant differences between the other curing units were only found at the 4 mm depth level cured from 7 mm distance (p < 0.05). The reduction in DC by increasing LT- RC distance was less than 10% for all curing units. It can be concluded that the improved LED curing units could cure the studied resin composite to the same DC as the control unit.     

Effect of different polymerization devices on the degree of conversion and the physical properties of an indirect resin composite

Polymerization of indirect resin composites (IRC) is carried out in the 'laboratories using special photo-polymerization devices to achieve a higher degree of conversion (DC). Such devices present variation in chambers and light output which may have consequences on the chemical and physical properties of IRCs. This study evaluated the effect of different polymerization devices on the flexural strength, Vickers microhardness and DC of an IRC. Specimens were prepared from an IRC material, Sinfony (3M ESPE), using special molds for flexural strength test (N=30) (25 x 2 x 2 mm, ISO 4049), Vickers microhardness test (N=30) (5 x 4 mm) and for DC (N=30) utilizing Micro-raman Spectroscopy. All specimens were submitted to initial polymerization with a Visio Alpha unit (3M ESPE) and then randomly divided into three groups (n=10/ group). Specimens in Group 1 (control) received additional polymerizations using a Visio Beta Vario device (3M ESPE), and those in Group 2 and Group 3 using Powerlux (EDG) and Strobolux (EDG) devices, respectively. DC and mechanical tests were then conducted. For the mechanical tests, the data were analyzed using ANOVA and Tukey's tests (p < 0.05) and for DC, one-way ANOVA was used. Polymerization in Strobolux (Group 3) resulted in significantly lower flexural strength (MPa) values (134 +/- 27) compared to Visio Beta Vario (165 +/- 20) (Group 1) (p < 0.05). The lowest microhardness values (Kg/mm2) were obtained in Group 3 (30 +/- 1) (p < 0.05). DC was similar in all groups (75 +/- 1, 91 +/- 5, 85 +/- 7% for Visio Beta Vario, Powerlux and Strobolux, respectively) (p = 0.1205). The type of polymerization device may affect the flexural strength and Vickers hardness of the IRC tested. DC also seems to be affected by the type of polymerization device but the results were not significant.     

The mechanical properties of nanofilled resin-based composites: Characterizing discrete filler particles and agglomerates using a micromanipulation technique

ObjectiveTo assess the mechanical properties of discrete filler particles representative of several inorganic fillers in modern dental resin-based composites (RBCs) and to assess the validity of a novel micromanipulation technique.MethodRBCs with microhybrid (Filtek? Z250), ‘nanohybrid’ (Grandio) and ‘nanofilled’ (Filtek? Supreme), filler particle morphologies were investigated. Filler particles were provided by the manufacturer or separated from the unpolymerized resin using a dissolution technique. Filler particles (n = 30) were subjected to compression using a micromanipulation technique between a descending glass probe and a glass slide. The number of distinct fractures particles underwent was determined from force/displacement and stress/deformation curves and the force at fracture and pseudo-modulus of stress was calculated.ResultsAgglomerated fillers (‘nanoclusters’) exhibited up to four distinct fractures, while spheroidal and irregular particles underwent either a single fracture or did not fracture following micromanipulation. Z-tests highlighted failure of nanoclusters to be significant compared with spheroidal and irregular particles (P < 0.05). The mean force at first fracture of the nanoclusters was greater (1702 ± 909 μN) than spheroidal and irregular particles (1389 ± 1342 and 1356 ± 1093 μN, respectively). Likewise, the initial pseudo-modulus of stress of nanoclusters (797 ± 555 MPa) was also greater than spheroidal (587 ± 439 MPa) or irregular (552 ± 275 MPa) fillers.SignificanceThe validity of employing the micromanipulation technique to determine the mechanical properties of filler particulates was established. The ‘nanoclusters’ exhibited a greater tendency to multiple fractures compared with conventional fillers and possessed a comparatively higher variability of pseudo-modulus and load prior to and at fracture, which may modify the damage tolerance of the overall RBC system.     

Influence of carboxylic anhydrides on selected mechanical properties of heat-cured resin composites.

Resin composites are still in need of improved abrasion resistance for them to be ideal restorative materials for use in large occlusal cavities. The present study proposes a concept for additional cross-linking of dental monomers, by which mechanical properties and possibly the resistance to abrasion of the resin composites are increased. Cyclic acid anhydrides were added as cross-linking agents to different monomer mixtures, which were then loaded with filler. The monomer mixtures were varied with respect to type and ratio of monomer and anhydride. For measurement of diametral tensile strength, flexural strength, modulus of elasticity, and modulus of resilience, specimens were initially cured by light and then post-cured for one h at 150 degrees C. Resin composites based on UEDMA and HEMA were found to be superior to BISGMA- and TEGDMA-based composites. Increases in mechanical properties were highest when unsaturated anhydrides were used. An optimal effect of anhydride addition was found in resin composites also containing methacrylamide. Such materials resulted in a 20% increase in the mechanical properties investigated.