Six-month evaluation of a resin/dentin interface created by methacrylate and silorane-based materials

Objectives: This study aimed to compare the micro-tensile bond strength of methacrylate resin systems to a silorane-based restorative system on dentin after 24 hours and six months water storage. Material and Methods: The restorative systems Adper Single Bond 2/Filtek Z350 (ASB), Clearfil SE Bond/Z350 (CF), Adper SE Plus/Z350 (ASEP) and P90 Adhesive System/Filtek P90 (P90) were applied on flat dentin surfaces of 20 third molars (n=5). The restored teeth were sectioned perpendicularly to the bonding interface to obtain sticks (0.8 mm2) to be tested after 24 hours (24 h) and 6 months (6 m) of water storage, in a universal testing machine at 0.5 mm/min. The data was analyzed via two-way Analysis of Variance/Bonferroni post hoc tests at 5% global significance. Results: Overall outcomes did not indicate a statistical difference for the resin systems (p=0.26) nor time (p=0.62). No interaction between material × time was detected (p=0.28). Mean standard-deviation in MPa at 24 h and 6 m were: ASB 31.38 (4.53) and 30.06 (1.95), CF 34.26 (3.47) and 32.75 (4.18), ASEP 29.54 (4.14) and 33.47 (2.47), P90 30.27 (2.03) and 31.34 (2.19). Conclusions: The silorane-based system showed a similar performance to methacrylate-based materials on dentin. All systems were stable in terms of bond strength up to 6 month of water storage.

Color stability of silorane-based composites submitted to accelerated artificial ageing-An in situ study

Objectives: To assess the in situ color stability, surface and the tooth/restoration interface degradation of a silorane-based composite (P90, 3M ESPE) after accelerated artificial ageing (AAA), in comparison with other dimethacrylate monomer-based composites (Z250/Z350, 3M ESPE and Esthet-X, Dentsply). Methods: Class V cavities (25 mm(2) x 2 mmdeep) were prepared in 48 bovine incisors, which were randomly allocated into 4 groups of 12 specimens each, according to the type of restorative material used. After polishing, 10 specimens were submitted to initial color readings (Easyshade, Vita) and 2 to analysis by scanning electronic microscopy (SEM). Afterwards, the teeth were submitted to AAA for 384 h, which corresponds to 1 year of clinical use, after which new color readings and microscopic images were obtained. The values obtained for the color analysis were submitted to statistical analysis (1-way ANOVA, Tukey, p < 0.05). Results: With regard to color stability, it was verified that all the composites showed color alteration above the clinically acceptable levels (Delta E >= 3.3), and that the silorane-based composite showed higher Delta E (18.6), with a statistically significant difference in comparison with the other composites (p < 0.05). The SEM images showed small alterations for the dimethacrylate-based composites after AAA and extensive degradation for the silorane-based composite with a rupture at the interface between the matrix/particle. Conclusion: It may be concluded that the silorane-based composite underwent greater alteration with regard to color stability and greater surface and tooth/restoration interface degradation after AAA. (C) 2011 Elsevier Ltd. All rights reserved.

Light-curing Time and Aging Effects on the Nanomechanical Properties of Methacrylate- and Silorane-based Restorations

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Microtensile Bond Strength Of Methacrylate And Silorane Resins To Enamel And Dentin.

The aim of this study was to evaluate the microtensile bond strength (µTBS) of two substrates (enamel and dentin) considering two study factors: type of composite resin [methacrylate-based (Filtek Supreme) or silorane-based (Filtek LS)] and aging time (24 h or 3 months). Twenty human molars were selected and divided into 2 groups (n=10) considering two dental substrates, enamel or dentin. The enamel and dentin of each tooth was divided into two halves separated by a glass plate. Each tooth was restored using both tested composite resins following the manufacturer's instructions. The samples were sectioned, producing 4 sticks for each composite resin. Half of them were tested after 24 h and half after 3 months. µTBS testing was carried out at 0.05 mm/s. Data were analyzed by three-way ANOVA and Tukey's HSD tests at α=0.05. Significant differences between composite resins and substrates were found (p<0.05), but no statistically significant difference was found for aging time and interactions among study factors. The methacrylate-based resin showed higher µTBS than the silorane-based resin. The µTBS for enamel was significantly higher than for dentin, irrespective of the composite resin and storage time. Three months of storage was not sufficient time to cause degradation of the bonding interaction of either of the composite resins to enamel and dentin.

Effect Of 4-(n,n-dimethylamino)phenethyl Alcohol On Degree Of Conversion And Cytotoxicity Of Photo-polymerized Cq-based Resin Composites.

The aim of this study was to evaluate the degree of conversion (DC) and the cytotoxicity of photo-cured experimental resin composites containing 4-(N,N-dimethylamino)phenethyl alcohol (DMPOH) combined to the camphorquinone (CQ) compared with ethylamine benzoate (EDAB). The resin composites were mechanically blended using 35 wt% of an organic matrix and 65 wt% of filler loading. To this matrix was added 0.2 wt% of CQ and 0.2 wt% of one of the reducing agents tested. 5x1 mm samples (n=5) were previously submitted to DC measurement and then pre-immersed in complete culture medium without 10% (v/v) bovine serum for 1 h or 24 h at 37 °C in a humidifier incubator with 5% CO2 and 95% humidity to evaluate the cytotoxic effects of experimental resin composites using the MTT assay on immortalized human keratinocytes cells. As a result of absence of normal distribution, the statistical analysis was performed using the nonparametric Kruskal-Wallis to evaluate the cytotoxicity and one-way analysis of variance to evaluate the DC. For multiple comparisons, cytotoxicity statistical analyses were submitted to Student-Newman-Keuls and DC analysis to Tukey's HSD post-hoc test (=0.05). No significant differences were found between the DC of DMPOH (49.9%) and EDAB (50.7%). 1 h outcomes showed no significant difference of the cell viability between EDAB (99.26%), DMPOH (94.85%) and the control group (100%). After 24 h no significant difference were found between EDAB (48.44%) and DMPOH (38.06%), but significant difference was found compared with the control group (p>0.05). DMPOH presented similar DC and cytotoxicity compared with EDAB when associated with CQ.

FiltekTM Silorane and FiltekTM Supreme XT resins: tissue reaction after subcutaneous implantation in isogenic mice

The aim of this study was to evaluate the tissue compatibility of a silorane-based resin system (FiltekTM Silorane) and a methacrylate-based nanoparticle resin (FiltekTM Supreme XT) after implantation in the subcutaneous connective tissue of isogenic mice. One hundred and thirty five male isogenic BALB/c mice were randomly assigned to 12 experimental and 3 control groups, according to the implanted material and the experimental period of 7, 21 and 63 days. At the end of each period, the animals were killed and the tubes with the surrounding tissues were removed and processed for microscopic analysis. Samples were subjected to a descriptive and a semi-quantitative analyses using a 4-point scoring system (0-3) to evaluate the collagen fiber formation and inflammatory infiltrate. Data were statistically analyzed using the Kruskal Wallis test (?=0.05). The results showed that there was no significant difference between the experimental and control groups considering the three evaluation periods (p>0.05). The silorane-based and the methacrylate-based nanoparticle resins presented similar tissue response to that of the empty tube (control group) after subcutaneous implantation in isogenic mice.

FiltekTM Silorane and FiltekTM Supreme XT resins: tissue reaction after subcutaneous implantation in isogenic mice

The aim of this study was to evaluate the tissue compatibility of a silorane-based resin system (FiltekTM Silorane) and a methacrylatebased nanoparticle resin (FiltekTM Supreme XT) after implantation in the subcutaneous connective tissue of isogenic mice. One hundred and thirty five male isogenic BALB/c mice were randomly assigned to 12 experimental and 3 control groups, according to the implanted material and the experimental period of 7, 21 and 63 days. At the end of each period, the animals were killed and the tubes with the surrounding tissues were removed and processed for microscopic analysis. Samples were subjected to a descriptive and a semi-quantitative analyses using a 4-point scoring system (0-3) to evaluate the collagen fiber formation and inflammatory infiltrate. Data were statistically analyzed using the Kruskal Wallis test (a=0.05). The results showed that there was no significant difference between the experimental and control groups considering the three evaluation periods (p>0.05). The silorane-based and the methacrylate-based nanoparticle resins presented similar tissue response to that of the empty tube (control group) after subcutaneous implantation in isogenic mice.

Effect of thermo-mechanical load cycling on silorane-based composite restorations

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Heat treatment of pre-hydrolyzed silane increases adhesion of phosphate monomer-based resin cement to glass ceramic

This study evaluated the influence of different forms of heat treatment on a pre-hydrolyzed silane to improve the adhesion of phosphate monomer-based (MDP) resin cement to glass ceramic. Resin and feldspathic ceramic blocks (n=48, n=6 for bond test, n=2 for microscopy) were randomly divided into 6 groups and subject to surface treatments: G1: Hydrofluoric acid (HF) 9.6% for 20 s + Silane + MDP resin cement (Panavia F); G2: HF 9.6% for 20 s + Silane + Heat Treatment (oven) + Panavia F; G3: Silane + Heat Treatment (oven) + Panavia F; G4: HF 9.6% for 20 s + Silane + Heat Treatment (hot air) + Panavia F; G5: Silane + Heat Treatment (hot air) + Panavia F; G6: Silane + Panavia F. Microtensile bond strength (MTBS) test was performed using a universal testing machine (1 mm/min). After debonding, the substrate and adherent surfaces were analyzed using stereomicroscope and scanning electron microscope (SEM) to categorize the failure types. Data were analyzed statistically using two-way test ANOVA and Tukey's test (=0.05). Heat treatment of the silane containing MDP, with prior etching with HF (G2: 13.15 ± 0.89a; G4: 12.58 ± 1.03a) presented significantly higher bond strength values than the control group (G1: 9.16 ± 0.64b). The groups without prior etching (G3: 10.47 ± 0.70b; G5: 9.47 ± 0.32b) showed statistically similar bond strength values between them and the control group (G1). The silane application without prior etching and heat treatment resulted in the lowest mean bond strength (G6: 8.05 ± 0.37c). SEM analysis showed predominantly adhesive failures and EDS analysis showed common elements of spectra (Si, Na, Al, K, O, C) characterizing the microstructure of the glass-ceramic studied. Heat treatment of the pre-hydrolyzed silane containing MDP in an oven at 100 °C for 2 min or with hot air application at 50 ± 5 ºC for 1 min, was effective in increasing the bond strength values between the ceramic and resin cement containing MDP.

Effects of surface treatment, hydration and application method on the bond strength of a silorane adhesive and resin system to dentine

Objectives: To evaluate the effects of surface treatment, surface hydration (SH) and application method (AM) on the tensile bond strength of the Silorane Adhesive System (SAS) to dentine. Methods: Ninety bovine teeth were used. For the control group (n = 10), each dentine surface was treated according to the manufacturer's instructions of the SAS. The remaining teeth were randomly distributed into two groups (n = 40), according to the type of dentine surface treatment (ST) - 37% phosphoric acid or Er:YAG Laser prior to the application of the SAS. Each group was further divided into 2 subgroups (n = 20), according to the SH status: dry (D) or wet (W). Each subgroup was further divided into 2 subgroups (n = 10), according to the application method [AM: Active (AC) mode or Passive (PA) mode]. A coat of resin composite (Filtek P90) was applied on the surface. Artificial ageing was performed with a thermo-mechanical cycling machine. The specimens were sectioned into 1 mm × 1 mm × 10 mm sticks and stressed to failure using a universal testing machine. The remaining teeth in each group were used for Scanning Electron Microscopy to examine the fractured area. Data were subjected to a three-way ANOVA, Tukey's test and Dunnet's test (α = 0.05). Results: The ANOVA showed significant differences for SH and AM, but not for ST. For SH, the results of Tukey's test were (in MPa): D-14.9(±3.8)a, W-17.1(±4.3)b; and for AM: PA-14. 9(±4.2)a, AC-17.1(±3.9) b. Conclusions: Acid etching, when combined with a moist dentine surface and the use of primer agitation, improves the bond strength of the SAS to dentine. Clinical Significance: According to the results of the present in vitro study, modification of the application protocols for the silorane-based adhesive system may improve its clinical performance. © 2012 Published by Elsevier Ltd.

Effect of silica coating combined to a MDP-based primer on the resin bond to Y-TZP ceramic

The aim of this study was to evaluate the influence of silica coating and 10-methacryloyloxydecyl dihydrogen phosphate (MDP)-based primer applications upon the bonding durability of a MDP-based resin cement to a yttrium stabilized tetragonal zirconia (Y-TZP) ceramic. Ninety-six Y-TZP tabs were embedded in an acrylic resin (free surface for adhesion: 5 x 5 mm(2)), ground finished and randomly divided into four groups (N = 24) according to the ceramic surface conditioning: (1) cleaning with isopropanol (ALC); (2) ALC + phosphoric acid etching + MDP-based primer application (MDP-primer); (3) silica coating + 3-methacryloyloxypropyl trimethoxysilane (MPS)-based coupling agent application (SiO(2) + MPS-Sil); and (4) SiO(2) + MDP-primer. The MDP-based resin cement was applied on the treated surface using a cylindrical mold (diameter=3 mm). Half of the specimens from each surface conditioning were stored in distilled water (37 C, 24 h) before testing. Another half of the specimens were stored (90 days) and thermo-cycled (12,000x) during this period (90d/TC) before testing. A shear bond strength (SBS) test was performed at a crosshead speed of 0.5 mm/min. Two factors composed the experimental design: ceramic conditioning strategy (in four levels) and storage condition (in two levels), totaling eight groups. After 90d/TC (Tukey; p < 0.05), SiO(2) + MDP-primer (24.40 MPa) promoted the highest SBS. The ALC and MDP-primer groups debonded spontaneously during 90d/TC. Bonding values were higher and more stable in the SiO2 groups. The use of MDP-primer after silica coating increased the bond strength. (C) 2010 Wiley Periodicals, Inc. J Biomed Mater Res Part 8: Appl Biomater 95B: 69-74, 2010.

Environment-friendly soy flour-based resins without formaldehyde

Glyoxalated soy flour adhesives for wood particleboard added with a much smaller proportion of glyoxalated lignin or tannin and without any addition of either formaldehyde or formaldehyde-based resin are shown to yield results satisfying the relevant standard specifications for interior wood boards. Adhesive resin formulations in which the total content of natural material is either 70 or 80% of the total resin solids content gave good results. The resins comprising 70% by weight of natural material can be used in a much lower proportion on wood chips and can afford pressing times fast enough to be significant under industrial panel pressing conditions. The best formulation of all the ones tried was the one based on glyoxalated precooked soy flour (SG), to which a condensed tannin was added in water solution and a polymeric isocyanate (pMDI), where the proportions of the components SG/T/pMDI was 54/16/30 by weight. (C) 2008 Wiley Periodicals, Inc.

Polymerization stress, shrinkage and elastic modulus of current low-shrinkage restorative composites

Objective. To compare currently available low-shrinkage composites with others regarding polymerization stress, volumetric shrinkage (total and post-gel), shrinkage rate and elastic modulus. Methods. Seven BisGMA-based composites (Durafill/DU, Filtek Z250/FZ, Heliomolar/HM, Aelite LS Posterior/AP, Point 4/P4, Filtek Supreme/SU, ELS/EL), a silorane-based (Filtek LS, LS), a urethane-based (Venus Diamond, VD) and one based on a dimethacrylate-derivative of dimer acid (N`Durance, ND) were tested. Polymerization stress was determined in 1-mm high specimens inserted between two PMMA rods attached to a universal testing machine. Total volumetric shrinkage was measured using a mercury dilatometer. Maximum shrinkage rate was used as a parameter of the reaction speed. Post-gel shrinkage was measured using strain-gages. Elastic modulus was obtained by three-point bending. Data were submitted to one-way ANOVA/Tukey test (p = 0.05), except for elastic modulus (Kruskal-Wallis). Results. Composites ranked differently for total and post-gel shrinkage. Among the materials considered as ""low-shrinkage"" by the respective manufacturers, LS, EL and VD presented low post-gel shrinkage, while AP and ND presented relatively high values. Polymerization stress showed a strong correlation with post-gel shrinkage except for LS, which presented high stress. Elastic modulus and shrinkage rate showed weak relationships with polymerization stress. Significance. Not all low-shrinkage composites demonstrated reduced polymerization shrinkage. Also, in order to effectively reduce polymerization stress, a low post-gel shrinkage must be associated to a relatively low elastic modulus. (C) 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of surface conditioning methods on the microtensile bond strength of resin composite to composite after aging conditions

Objectives. This study evaluated the effect of two different surface conditioning methods on the repair bond strength of a bis-GMA-adduct/bis-EMA/TEGDMA based resin composite after three aging conditions.Methods. Thirty-six composite resin blocks (Esthet X, Dentsply) were prepared (5 mm x 6 mm x 6 mm) and randomly assigned into three groups for aging process: (a) immersion in citric acid (pH 3.0 at 37 degrees C, 1 week) (CA); (b) boiling in water for 8h (BW) and (c) thermocycling (x5000, 5-55 degrees C, dwell time: 30s) (TC). After aging, the blocks were assigned to one of the following surface conditioning methods: (1) silica coating (30 mu m SiOx) (CoJet, 3M ESPE) + silane (ESPE-Sil) (CJ), (2) phosphoric acid + adhesive resin (Single Bond, 3M ESPE) (PA). Resin composite (Esthet.X (R)) was bonded to the conditioned substrates incrementally and light polymerized. The experimental groups formed were as follows: Gr1:CA + PA; Gr2:CA + CJ Gr3:BW + PA; Gr4: BW + CJ; Gr5:TC + PA; Gr6: TC + CJ. The specimens were sectioned in two axes (x and y) with a diamond disc under coolant irrigation in order to obtain non-trimmed bar specimens (sticks, 10 mm x 1 mm x 1 mm) with 1 mm(2) of bonding area. The microtensile test was accomplished in a universal testing machine (crosshead speed: 0.5 mm min(-1)).Results. The means and standard deviations of bond strength (MPa +/- S.D.) per group were as follows: Gr1: 25.5 +/- 10.3; Gr2: 46.3 +/- 10.1; Gr3: 21.7 +/- 7.1; Gr4: 52.3 +/- 15.1; GrS: 16.1 +/- 5.1; Gr6, 49.6 +/- 13.5. The silica coated groups showed significantly higher mean bond values after all three aging conditions (p < 0.0001) (two-way ANOVA and Tukey tests, alpha = 0.05). The interaction effect revealed significant influence of TC aging on both silica coated and acid etched groups compared to the other aging methods (p < 0.032). Citric acid was the least aggressive aging medium.Significance. Chairside silica coating and silanization provided higher resin-resin bond strength values compared to acid etching with phosphoric acid followed by adhesive resin applications. Thermocycling the composite substrates resulted in the lowest repair bond strength compared to citric acid challenge or boiling in water. (C) 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Ceramic Primer Heat-Treatment Effect on Resin Cement/Y-TZP Bond Strength

The purpose of this study was to evaluate the effect of different heat-treatment strategies for a ceramic primer on the shear bond strength of a 10-methacryloyloxydecyl-dihydrogen-phosphate (MDP)-based resin cement to a yttrium-stabilized tetragonal zirconia polycrystal (Y-TZP) ceramic. Specimens measuring 4.5 x 3.5 x 4.5 mm(3) were produced from Y-TZP presintered cubes and embedded in polymethyl methacrylate (PMMA). Following finishing, the specimens were cleaned using an ultrasound device and distilled water and randomly divided into 10 experimental groups (n=14) according to the heat treatment of the ceramic primer and aging condition. The strategies used for the experimental groups were: GC (control), without primer; G20, primer application at ambient temperature (20 degrees C); G45, primer application + heat treatment at 45 degrees C; G79, primer application + heat treatment at 79 degrees C; and G100, primer application + heat treatment at 100 degrees C. The specimens from the aging groups were submitted to thermal cycling (6000 cycles, 5 degrees C/55 degrees C, 30 seconds per bath) after 24 hours. A cylinder of MDP-based resin cement (2.4 mm in diameter) was constructed on the ceramic surface of the specimens of each experimental group and stored for 24 hours at 37 degrees C. The specimens were submitted to a shear bond strength test (n=14). Thermal gravimetric analysis was performed on the ceramic primer. The data obtained were statistically analyzed by two-way analysis of variance and the Tukey test (alpha=0.05). The experimental group G79 without aging (7.23 +/- 2.87 MPa) presented a significantly higher mean than the other experimental groups without aging (GC: 2.81 +/- 1.5 MPa; G20: 3.38 +/- 2.21 MPa; G100: 3.96 +/- 1.57 MPa), showing no difference from G45 only (G45: 6 +/- 3.63 MPa). All specimens of the aging groups debonded during thermocycling and were considered to present zero bond strength for the statistical analyses. In conclusion, heat treatment of the metal/zirconia primer improved bond strength under the initial condition but did not promote stable bonding under the aging condition.