Eduardo José Souza-Junior

Degree of Conversion of Simplified Contemporary Adhesive Systems as Influenced by Extended Air-Activated or Passive Solvent Volatilization Modes

This study evaluated the effect of five methods of solvent volatilization on the degree of conversion (DC) of nine one-bottle adhesive systems using Fourier transform infrared/attenuated total reflectance (FTIR/ATR) analysis. Nine adhesives were tested: Adper Single Bond 2 (SB), Adper Easy One (EO), One Up Bond F Plus (OUP), One Coat Bond SL (OC), XP Bond (XP), Ambar (AM), Natural Bond (NB), GO, and Stae. The adhesive systems were applied to a zinc-selenide pellet and 1) cured without solvent volatilization, 2) left undisturbed for 10 seconds before curing, 3) left undisturbed for 60 seconds before curing, 4) air-dried with an air stream for 10 seconds before curing, and 5) air-dried with an air stream for 60 seconds before curing. FTIR/ATR spectra were obtained, and the DC was calculated by comparing the aliphatic bonds/reference peaks before and after light activation for 10 seconds (FlashLite 1401). The DC means of each material were analyzed by one-way analysis of variance and post hoc Tukey test (p<0.05). The DC of GO and Stae adhesive systems was not affected by the five evaporation conditions. Air-drying for 60 seconds before curing yielded the highest DC for SB, EO, and OC. Extended solvent volatilization time (60 seconds) either with or without air-drying before curing provided the highest DC for AM, NB, XP, and OUP. Thus, the monomer conversion of adhesive systems was material dependent. In general, the 60-second passive or active air-drying modes to volatilize solvents before curing enhanced the degree of conversion for the one-bottle simplified adhesive systems.

Influence of extended light exposure time on the degree of conversion and plasticization of materials used as pit and fissure sealants

AIM To evaluate the conversion and plasticization of fissure sealer materials, as influenced by extended curing time. METHODS Twenty specimens (n=5) of a pit and fissure sealant and a flowable composite at two curing times (20 and 60 sec) were photocured with the Bluephase 16i light-emitting diode. The conversion was determined by Fourier transform infrared/attenuated total reflection spectroscopy 24 h after polymerization. Hardness was measured, and samples were stored in absolute ethanol for 24 h. A second hardness measurement was executed after storage to assess plasticization by the percentage of hardness decrease. Data were analyzed by analysis of variance and Pearsons correlation (α=0.05). RESULTS The pit and fissure sealant showed lower degree of conversion than the flowable composite. The 60-sec curing time increased the conversion only for the flowable composite. Plasticization was lower for the flowable composite than for the pit and fissure sealant. The 60-sec light exposure time showed a similar percentage of hardness decrease of 20 sec. A low correlation between the conversion and plasticization was found. CONCLUSION Extended curing time improved the conversion only for the flowable composite. The pit and fissure sealant presented lower conversion and higher plasticization than the flowable composite.

Influence of the curing mode on the degree of conversion of a dual-cured self-adhesive resin luting cement beneath ceramic

Abstract Objective. To evaluate the effect of the delayed photoactivation and ceramic barrier on the degree of conversion (DC) of self-adhesive resin cement. Materials and methods. Circular specimens (5 mm in diameter × 1 mm in thickness) of the RelyX U-100 resin cement were made using the following curing protocols (n = 10): (G1) 40 s beneath a IPS Empress II ceramic; (G2) 40 s of direct photocuring; (G3) 80 s beneath the ceramic; (G4) 80 s of direct photocuring; (G5) self-curing; (G6) 5 min in the absence of light (self-curing) followed by transceramic photocuring for 40 s; (G7) 5 min in the absence of light (self-curing) followed by transceramic photocuring for 80 s. All the specimens were photoactivated by LED (800 mW/cm2). After 24 h of dry storage, the DC was measured by FTIR, on the top surface of the specimens. Data were submitted to one-way ANOVA and Tukey test (p ≤ 0.05). Results. Direct photocuring with no ceramic interposition, regardless of the curing time (40 s and 80 s) promoted the highest conversion mean (56.79 ± 1.19 and 59.98 ± 2.93, respectively) and the 5 min delay time for the transceramic photocuring presented a similar mean compared to the immediate transceramic photocuring. The DC was influenced by the ceramic barrier, decreasing the conversion values (49.72 ± 1.91 for 40 s and 52.36 ± 2.50 for 80 s), with no statistical difference from the groups with the previous 5 min of photoactivation delay. The self-cure only showed the worst DC values. Conclusion. Direct photocuring provided a higher degree of conversion for the self-adhesive resin cement. The delayed light activation did not influence the degree of conversion for the resin cement tested.

Dynamic mechanical thermal analysis of composite resins with CQ and PPD as photo-initiators photoactivated by QTH and LED units

OBJECTIVES The aim of this study was to evaluate the thermal and mechanical properties of the composite resins containing the photo-initiators camphorquinone (CQ) and/or phenyl-propanodione (PPD) when photoactivated with halogen lamp (XL2500/3M-ESPE), monowave (UltraBlueIS/DMC) and polywave (UltraLume5/Ultradent) LED units. MATERIALS AND METHODS A blend of BisGMA, UDMA, BisEMA and TEGDMA was prepared with the same wt% of photo-initiators CQ and/or PPD and 65wt% of silaneted filler particles. Compression strength (CS), diametral tensile strength (DTS) and diametral modulus (DM) were tested. Thermogravimetric analysis (TGA) was made and the lost residual monomer were verified. Dynamic mechanical thermal analysis (DMTA) was used for to analyze the glass transition temperature (Tg) and the storage modulus in 37°C. Degree of conversion (DC) was accomplished in the same samples of DMA using middle-infrared spectroscopy (mid-IR). RESULTS CQ, CQ/PPD and PPD obtained the same results for all mechanical properties (CS, DTS and DM), lost residual monomer and storage modulus in 37°C, regardless LCU used. The results of Tg showed that the combination PPD-UltraLume5 produced the highest values. DC showed that the combination CQ-UltraLume5 resulted in the highest values and PPD-XL2500 in the lowest DC values. CONCLUSION The study shows that PPD is not only effective photosensitizers, but also photocrosslinking agents for dental composite resins with a similar efficiency to CQ.

Color Stability and Polymerization Behavior of Direct Esthetic Restorations

OBJECTIVES The current study evaluated the effect of accelerated artificial aging (AAA) on the color stability (CS) and degree of conversion (DC) of nanofilled and nanohybrid resin composites associated to different adhesive systems in direct esthetic restorations. MATERIAL AND METHODS Eighty bovine incisors were used to obtained dentin blocks (4 × 4 × 1 mm). The restorative systems were bonded to the blocks and photoactivated according to the manufacturers instructions. Three adhesive systems were used: Adper Scotchbond Multi-Purpose (conventional of three steps), Tetric N-Bond (conventional of two steps) and ClearFill SE Bond (self-etching). Also, two composites were used: Filtek Z350 XT (nanofilled) and IPS Empress Direct (nanohybrid). The restorations were made using a silicone mold placed on top of the prepared dentin blocks (N = 10). CS was measured after 300 hours of AAA by means of ultraviolet light using a spectrophotometer and CIE L*a*b* parameters on the top surface of the composite and at the bonded interface. The DC was performed using Fourier transform infrared spectroscopy (N = 10). Data were analyzed using two-way analysis of variance and Tukeys test (α = 0.05). RESULTS The adhesive systems had no significant influence on the color stability (ΔE) of either the restoration surface (α = 0.90) or the bonded interface (α = 0.78). However, composite influenced the color as measured by ΔE and isolated coordinates (α < 0.001). The nanohybrid composite showed increased DC values (67%) compared with the nanofilled (61%) with statistically significant differences (α < 0.001). CONCLUSIONS The adhesive system did not affect the final color of direct esthetic restorations. The nanohybrid composite demonstrated a higher DC and increased color stability after AAA compared to the nanofilled composite. CLINICAL SIGNIFICANCE The long-term color stability of composite restorations is a critical aspect of esthetic restorative procedures. Optimal Polymerization behavior of resin composite as indicated by the degree of conversion also influence on the color stability after artificial aging of composite restorations.

Photoinitiator concentration and modulated photoactivation: influence on polymerization characteristics of experimental composites

This study determined the influence of photoinitiator concentration on polymerization characteristics of experimental composites photoactivated by different methods. Composites based on BisGMA/TEGDMA and 65% of filler were prepared with the concentration of camphorquinone/amine C1-0.5%, C2-1%, C3-1.5%, and photocured using 4 methods: High-intensity (HI), Low-intensity (LI), Soft-start (SS) and Pulse-delay (PD). Were determined the degree of conversion (DC), depth of cure (DCure) and crosslink density (CLD). Data were submitted to ANOVA and Tukey’s test (p < 0.05). DC and DCure revealed that there were no differences among the photoactivation methods. C3 and C2 showed higher DC than C1. The CLD evaluation revealed considerable differences among the photoactivation methods. Photoinitiator concentration is a determinant factor in the polymerization characteristics of composites. Composite with low photoinitiator concentration show decreased DC and DCure, when compared with the composites with higher concentrations. Photoactivation methods had no effect on the DC and DCure. However, photoactivation methods showed differences when CLD was tested for composites with higher concentration of photoinitiators.

Influence of etching time and bonding strategies on the microshear bond strength of self- and light-cured pit-and-fissure sealants

This study evaluated the impact of extended etching and bonding strategies on the microshear bond strength of three sealant materials. Two pit-and-fissure sealants [FluroShield, Dentsply (light-cured) and AlphaSeal, DFL (self-cured)] and one light-cured flowable composite resin (Permaflo, Ultradent) were evaluated according to different enamel etching times (15 s or 30 s) and bonding procedures (no adhesive application, application of primer/hydrophobic resin or hydrophobic resin only). Intact enamel blocks were obtained from bovine teeth and sealed via the tested protocols. After 24 h, the microshear bond strength test was performed in a universal testing machine at a crosshead speed of 0.5 mm/min. Failure modes were classified by stereomicroscopy. Data were submitted to a three-way ANOVA and to Tukeys test (α=0.05). There was no statistically significant difference (p>0.05) among the materials. Permaflo showed higher bond strength when etched for 30 s alone. Enamel overetching decreased the bond strength of the light-cured sealant. Primer/bond previous treatment improved bond performance for AlphaSeal. In conclusion, from the tested conditions, all sealant materials presented similar bond strength values in relation to bonding protocol and etching time. The flowable composite can be used as a pit-and-fissure sealant. The use of a three-step adhesive system was essential for the self-cured sealant application.

Dual-cured etch-and-rinse adhesive systems increase the bond durability of direct coronal dentin restorations.

This study aimed to evaluate the bond durability of dentin restorations bonded with light- or dual-cured etch-and-rinse adhesive systems. A three-step adhesive system (Scotchbond Multipurpose Plus), an acetone-based two-step adhesive system (Prime & Bond 2.1), and an ethanol-based two-step adhesive system (Excite) were tested. Both the light- and the dual-cured versions were evaluated. High C-factor dentin cavities were prepared on 120 bovine incisors, which were then restored with resin composite (n=10). The samples were stored in water for 24 hours, and half of them were subjected to additional degradation with 10% NaOCl for five hours. The push-out bond strength test was performed in a universal testing machine until failure. Failure modes were evaluated by scanning electron microscopy. Data were analyzed by three-way analysis of variance and Tukey tests (p<0.05). The dual-cured adhesive system presented a higher immediate bond strength and durability than those that were light cured. The three-step adhesive system produced the highest values, whereas the acetone-based adhesive system produced the lowest result. Therefore, the use of dual-cured etch-and-rinse adhesive systems can induce increased bond durability to direct coronal dentin restorations.

Selective Enamel Etching: Effect on Marginal Adaptation of Self-Etch LED-Cured Bond Systems in Aged Class I Composite Restorations

The aim of this study was to evaluate the influence of previous enamel etch and light emitting diode (LED) curing on gap formation of self-etch adhesive systems in Class I composite restorations after thermomechanical aging (TMA). Thus, on 192 human molars, a box-shaped Class I cavity was prepared maintaining enamel margins. Self-etch adhesives (Clearfil SE and Clearfil S3) were used to restore the preparation with a microhybrid composite. Before application of the adhesives, half of the teeth were enamel etched for 15 seconds with 37% phosphoric acid; the other half were not etched. For the photoactivation of the adhesives and composite, three light-curing units (LCUs) were used: one polywave (Ultra-Lume LED 5, UL) and two single-peak (FlashLite 1401, FL and Radii-cal, RD) LEDs. After this, epoxy resin replicas of the occlusal surface were made, and the specimens were submitted to TMA. New replicas were made from the aged specimens for marginal adaptation analysis by scanning electron microscopy. Data were submitted to Kruskal-Wallis and Wilcoxon tests (α=0.05). Before TMA, when enamel was etched before the application of S3, no gap formation was observed; however, there were gaps at the interface for the other tested conditions, with a statistical difference (p≤0.05). After TMA, the selective enamel etching previous to the S3 application, regardless of the LCU, promoted higher marginal adaptation compared to the other tested groups (p≤0.05). Prior to TMA, higher marginal integrity was observed, in comparison with specimens after TMA (p≤0.05). With regard to Clearfil SE and Clearfil Tri-S cured with FL, no differences of gap formation were found between before and after aging (5.3 ± 3.8 and 7.4 ± 7.5, respectively), especially when the Clearfil Tri-S was used in the conventional protocol. When cured with RD or UL and not etched, Clearfil Tri-S presented the higher gap formation. In conclusion, additional enamel etching promoted better marginal integrity for Clearfil Tri-S, showing it to be an efficient technique for Class I composite restorations. The two-step self-etch adhesive was not influenced by selective enamel etching or by the LED-curing unit.

Nanoleakage evaluation of resin luting systems to dental enamel and leucite-reinforced ceramic

Purpose: The aim of this study was to evaluate the nanoleakage patterns between dental enamel and reinforced leucite ceramic, bonded with resin luting systems and a flowable composite resin. Materials and Methods: Twelve crowns of bovine incisors were randomly divided into four groups (n = 3) according to the luting procedure: Excite/Variolink II, Clearfil SE Bond/Panavia F, Scotchbond Multi‐Purpose Plus/RelyX ARC, and Single Bond 2/Filtek Z350 Flow. To evaluate the nanoleakage patterns, IPS Empress Esthetic disks (5 mm Ø and 1.2‐mm thick) were bonded to enamel, and, after 24 h, the specimens were immersed in a 50% (w/v) solution of silver nitrate (24 h), fixed, dehydrated, and processed scanning electron microscopy (SEM). Results: None nanoleakage on interface of the groups that Single Bond 2 followed by the flowable composite were used. The highest percentage of nanoleakage was shown by the Excite/Variolink II protocol. Also, in all conditions tested, none silver nitrate uptake was observed between the leucite‐reinforced ceramic and the resin luting cement. Conclusions: The use of a two‐step etch‐and‐rinse adhesive with flowable composite was able to promote an adequate seal of the bond interface at the enamel. Moreover, the conventional dual‐cured resin cements associated with simplified and dual‐cured adhesives tested are also indicated to bond thin ceramics to enamel, since all presented low silver nitrate uptake. Microsc. Res. Tech., 2012.