Effect of curing protocol on the polymerization of dual-cured resin cements

Objectives. The purpose of this study was to evaluate how curing protocol affects the extent of polymerization of dual-cured resin cements. Methods. Four commercial resin cements were used (DuoLink, Panavia F 2.0, Variolink II and Enforce). The extent of polymerization of the resin cements cured under different conditions was measured using a (1)H Stray-Field MRI method, which also enabled to probe molecular mobility in the kHz frequency range. Results. Resin cements show well distinct behaviours concerning chemical cure. Immediate photo-activation appears to be the best choice for higher filler loaded resin cements (Panavia F 2.0 and Variolink). A photo-activation delay (5 min) did not induce any significant difference in the extent of polymerization of all cements. Significance. The extent of polymerization of dual-cured resin cements considerably changed among products under various curing protocols. Clinicians should optimize the materials choice taking into account the curing characteristics of the cements. (C) 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Hardening of a dual-cure resin cement using QTH and LED curing units

Objective: This study evaluated the surface hardness of a resin cement (RelyX ARC) photoactivated through indirect composite resin (Cristobal) disks of different thicknesses using either a light- emitting diode (LED) or quartz tungsten halogen (QTH) light source. Material and Methods: Eighteen resin cement specimens were prepared and divided into 6 groups according to the type of curing unit and the thickness of resin disks interposed between the cement surface and light source. Three indentations (50 g for 15 s) were performed on the top and bottom surface of each specimen and a mean Vickers hardness number (VHN) was calculated for each specimen. The data were analyzed using two-way ANOVA and Tukey-Kramer test was used for post-hoc pairwise comparisons. Results: Increased indirect resin disk thickness resulted in decreased mean VHN values. Mean VHN values for the top surfaces of the resin cement specimens ranged from 23.2 to 46.1 (QTH) and 32.3 to 41.7 (LED). The LED curing light source produced higher hardness values compared to the QTH light source for 2- and 3-mm-thick indirect resin disks. The differences were clinically, but not statistically significant. Increased indirect resin disk thickness also resulted in decreased mean VHN values for the bottom surfaces of the resin cement: 5.8 to 19.1 (QTH) and 7.5 to 32.0 (LED). For the bottom surfaces, a statistically significant interaction was also found between the type of curing light source and the indirect resin disk thickness. Conclusions: Mean surface hardness values of resin cement specimens decreased with the increase of indirect resin disk thickness. The LED curing light source generally produced higher surface hardness values.

Effect of ceramic shade on the degree of conversion of a dual-cure resin cement analyzed by FTIR

Objectives: The aim of this research was to evaluate the degree of monomer conversion of different resin cement shades when photocured under different feldspathic ceramic shades. The photocuring time was also evaluated as well as the translucency of each ceramic shade. Methods: Three VITA VM7 ceramic shades (Base Dentin 0M1, Base Dentin 2M2 and Base Dentin 5M3) were used to determine the translucency percentage. A spectrophotometer MiniScan was used to measure the opacity percentage of each specimen (2-mm-thick) and then the translucency was calculated. To measure the degree of conversion (DC), the resin cement (Variolink II; A3 Yellow and transparent) specimens (thickness: 100 μm) were photocured under a ceramic block (2-mm-thick) for 20 or 40 s. Specimens photocured without the ceramic block were used as control. Sixteen groups (n = 3) were evaluated. Micro-ATR/FTIR spectrometry was used to evaluate the extent of polymerization of all specimens after 24 h. The %DC was calculated of experimentally polymerized versus maximally polymerized composite. Results: The translucency percentages of 0M1, 2M2 and 5M3 ceramics were 12.41 (1.02)%, 5.75 (1.91)% and 1.07 (0.03)%, respectively. The %DC of both resin cement shades cured under ceramic 5M3 was significantly lower than the other groups (p < 0.05). The %DC of 0M1 groups exhibited no significant difference from 2M2 groups (p > 0.05), with the exception of the transparent cement photocured for 40 s. Conclusion: Photocuring under 2 mm ceramic showed that the increase in chroma saturation significantly decreased Variolink II resin cement %DC (100-μm-thick). © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of Temperature on the Degree of Conversion and Working Time of Dual-Cured Resin Cements Exposed to Different Curing Conditions

Objectives: This study evaluated the degree of conversion (DC) and working time (WT) of two commercial, dual-cured resin cements polymerized at varying temperatures and under different curing-light accessible conditions, using Fourier transformed infrared analysis (FTIR). Materials and Methods: Calibra (Cal; Dentsply Caulk) and Variolink II (Ivoclar Vivadent) were tested at 25 degrees C or preheated to 37 degrees C or 50 degrees C and applied to a similar-temperature surface of a horizontal attenuated-total-reflectance unit (ATR) attached to an infrared spectrometer. The products were polymerized using one of four conditions: direct light exposure only (600 mW/cm(2)) through a glass slide or through a 1.5- or 3.0-mm-thick ceramic disc (A2 shade, IPS e.max, Ivoclar Vivadent) or allowed to self-cure in the absence of light curing. FTIR spectra were recorded for 20 min (1 spectrum/s, 16 scans/spectrum, resolution 4 cm(-1)) immediately after application to the ATR. DC was calculated using standard techniques of observing changes in aliphatic-to-aromatic peak ratios precuring and 20-min postcuring as well as during each 1-second interval. Time-based monomer conversion analysis was used to determine WT at each temperature. DC and WT data (n=6) were analyzed by two-way analysis of variance and Tukey post hoc test (p=0.05). Results: Higher temperatures increased DC regardless of curing mode and product. For Calibra, only the 3-mm-thick ceramic group showed lower DC than the other groups at 25 degrees C (p=0.01830), while no significant difference was observed among groups at 37 degrees C and 50 degrees C. For Variolink, the 3-mm-thick ceramic group showed lower DC than the 1-mm-thick group only at 25 degrees C, while the self-cure group showed lower DC than the others at all temperatures (p=0.00001). WT decreased with increasing temperature: at 37 degrees C near 70% reduction and at 50 degrees C near 90% for both products, with WT reduction reaching clinically inappropriate times in some cases (p=0.00001). Conclusion: Elevated temperature during polymerization of dual-cured cements increased DC. WT was reduced with elevated temperature, but the extent of reduction might not be clinically acceptable.

Microhardness of resin cements in the intraradicular environment: Effects of water storage and softening treament

Objectives. To analyze the microhardness of four dual-cure resin cements used for cementing fiber-reinforced posts under the following conditions: after 7 days of storage in water, after additional 24 h of immersion in 75% ethanol, and after 3 months of storage in water. Hardness measurements were taken at the cervical, middle and apical thirds along the cement line. Methods. Root canals of 40 bovine incisors were prepared for post space. Fibrekor (R) glass fiber-reinforced posts (Jeneric/Pentron) of 1 mm in diameter were cemented using Panavia F 2.0 (Kuraray), Variolink (Ivoclar-Vivadent), Rely X Unicem (3M ESPE) or Duolink (Bisco) (N = 10). After 7 days of water storage at 37 degrees C, half the sample (N = 5) was longitudinally sectioned and the initial microhardness measured along the cement line from cervical to apex. These same samples were further immersed in 75% ethanol for 24 h and reassessed. The remaining half (N = 5) was kept unsectioned in deionized water at 37 degrees C for 3 months, followed by sectioning and measuring. Data were analyzed by a series of two-way ANOVA and Tukey tests at alpha = 5%. Results. Statistically significant differences were identified among the cements, thirds and conditions. Significant interactions were also observed between cements and thirds and between cements and conditions. Panavia F exhibited significantly higher initial microhardness than the other three cements, which showed no statistical difference among themselves. Variolink and Duolink showed significantly higher microhardness values in the cervical third, without significant difference among the thirds for the other cements. Immersion in ethanol significantly reduced the hardness values for all cements, regardless of the thirds. Storage in water for 3 months had no influence on the hardness of most of the cements, with the exception of Unicem that showed a significant increase in the hardness values after this period. Results showed heterogeneity in the microhardness of the cements inside the canal. All cements presented some degree of softening after ethanol treatment, which suggests instability of the polymer. The quality of curing of resin cements in the root canal environment seems unpredictable and highly material dependent. (C) 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Bonding Efficacy of New Self-etching, Self-adhesive Dual-curing Resin Cements to Dental Enamel

Purpose: This study evaluated the efficacy of the union between two new self-etching self-adhesive resin cements and enamel using the microtensile bond strength test.Materials and Methods: Buccal enamel of 80 bovine teeth was submitted to finishing and polishing with metallographic paper to a refinement of #600, in order to obtain a 5-mm(2) flat area. Blocks (2 x 4 x 4 mm) of laboratory composite resin were cemented to enamel according to different protocols: (1) untreated enamel + RelyX Unicem cement (RX group); (2) untreated enamel + Bifix SE cement (BF group); (3) enamel acid etching and application of resin adhesive Single Bond + RelyX Unicem (RXA group); (4) enamel acid etching and application of resin adhesive Solobond M + Bifix SE (BFA group). After 7 days of storage in distillated water at 37 degrees C, the blocks were sectioned for obtaining microbar specimens with an adhesive area of 1 mm(2) (n = 120). Specimens were submitted to the microtensile bond strength test at a crosshead speed of 0.5 mm/min. The results (in MPa) were analyzed statistically by ANOVA and Tu key's test.Results: Enamel pre-treatment with phosphoric acid and resin adhesive (27.9 and 30.3 for RXA and BFA groups) significantly improved (p <= 0.05) the adhesion of both cements to enamel compared to the union achieved with as-polished enamel (9.9 and 6.0 for RX and BF).Conclusion: Enamel pre-treatment with acid etching and the application of resin adhesive significantly improved the bond efficacy of both luting agents compared to the union achieved with as-polished enamel.

The influence of chemical activation on hardness of dual-curing resin cements.

During the cementation of metallic restorations, the polymerization of dual-curing resin cements depends exclusively on chemical activation. This study evaluated the influence of chemical activation compared with dual-curing (chemical and light activation), on the hardness of four dual-curing resin cements. In a darkened environment, equal weight proportions of base and catalyst pastes of the cements Scotchbond Resin Cement, Variolink II, Enforce and Panavia F were mixed and inserted into moulds with cavities of 4 mm in diameter and 2 mm in height. Subsequently, the cements were: 1) not exposed to light (chemical activation = self-cured groups) or 2) photoactivated (dual-curing = dual-cured groups). The Vickers hardness number was measured at 1 hour, 24 hours and 7 days after the start time of cements' spatulation. For all the cements, the hardness values of self-cured groups were lower than those of the respective dual-cured groups at 1 hour and 24 hours. At 7 days, this behavior continued for Variolink II and Panavia F, whilst for Scotchbond Resin Cement and Enforce there was no statistical difference between the two activation modes. All cements showed a significant increase in their hardness values from 1 hour to 7 days for both activation modes. Of the self-cured groups, Scotchbond Resin Cement and Variolink II presented the highest and the lowest hardness values, respectively, for all three times tested. Within the limitations of this study, up to the time of 24 h, chemical activation alone was unable to promote similar hardness as to that obtained with dual-curing.

Influence of activation modes on diametral tensile strength of dual-curing resin cements.

In metallic restorations, the polymerization of dual-curing resin cements depends exclusively on chemical activation. The effect of the lack of photoactivation on the strength of these cements has been rarely studied. This study evaluated the influence of activation modes on the diametral tensile strength (DTS) of dual-curing resin cements. Base and catalyst pastes of Panavia F, Variolink II, Scotchbond Resin Cement, Rely X and Enforce were mixed and inserted into cylindrical metal moulds (4 x 2 mm). Cements were either: 1) not exposed to light (chemical activation = self-cured groups) or 2) photoactivated through mylar strips (chemical and photo-activation = dual-cured groups) (n = 10). After a 24 h storage in 37 masculineC distilled water, specimens were subjected to compressive load in a testing machine. A self-curing resin cement (Cement-It) and a zinc phosphate cement served as controls. Comparative analyses were performed: 1) between the activation modes for each dual-curing resin cement, using Students t test; 2) among the self-cured groups of the dual-curing resin cements and the control groups, using one-way ANOVA and Tukeys test (alpha = 0.05). The dual-cured groups of Scotchbond Resin Cement (53.3 MPa), Variolink II (48.4 MPa) and Rely X (51.6 MPa) showed higher DTS than that of self-cured groups (44.6, 40.4 and 44.5 MPa respectively) (p < 0.05). For Enforce (48.5 and 47.8 MPa) and Panavia F (44.0 and 43.3 MPa), no significant difference was found between the activation modes (p > 0.05). The self-cured groups of all the dual-curing resin cements presented statistically the same DTS as that of Cement-It (44.1 MPa) (p > 0.05), and higher DTS than that of zinc phosphate (4.2 MPa). Scotchbond Resin Cement, Variolink II and Rely X depended on photoactivation to achieve maximum DTS. In the absence of light, all the dual-curing resin cements presented higher DTS than that of zinc phosphate and statistically the same as that of Cement-It (p > 0.05).

Diametral tensile strength of dual-curing resin cements submitted exclusively to autopolymerization.

OBJECTIVES: To evaluate, at different times, the diametral tensile strength (DTS) of dual-curing resin cements that were not photopolymerized. METHOD AND MATERIALS: Equal amounts of base and catalyst pastes of Panavia F (Kuraray), Variolink II (Vivadent), Rely X (3M ESPE), and Enforce (Dentsply) were mixed and inserted into cylindrical molds (4 x 2 mm) (n = 10). Cements were not photopolymerized. DTS test was performed in a testing machine at 30 minutes, 1 hour, 24 hours, and 7 days. The specimens were stored in light-proof containers with distilled water at 37 degrees C until the time of assay. An autopolymerizing resin cement (Cement-It, Jeneric Pentron) and a zinc phosphate cement served as controls. One-way analysis of variance (ANOVA) and Tukey test were performed separately for each cement and for each time (P <.05). RESULTS: All cements showed an increase in DTS when tested at 1 and 24 hours. Tests at 24 hours and 7 days revealed no statistically significant differences. In all groups, the zinc phosphate cement had the lowest DTS mean values (2.1 MPa, 3.6 MPa, 6.5 MPa, and 6.9 MPa), while Cement-It (35.1 MPa, 33.6 MPa, 46.9 MPa, and 46.3 MPa) and Enforce (31.9 MPa, 31.7 MPa, 43.4 MPa, and 47.6 MPa) presented the highest DTS mean values. CONCLUSION: All cements presented maximal strength at 24 hours. The dual-curing resin cements, even when nonphotopolymerized, demonstrated higher DTS than the zinc phosphate cement and similar or lower values than the autopolymerizing resin cement.

Effects of curing protocol and storage time on the micro-hardness of resin cements used to lute fiber-reinforced resin posts

Objectives: To determine the micro-hardness profile of two dual cure resin cements (RelyX - U100 (R), 3M-ESPE and Panavia F 2.0 (R), Kuraray) used for cementing fiber-reinforced resin posts (Fibrekor (R) - Jeneric Pentron) under three different curing protocols and two water storage times. Material and methods: Sixty 16mm long bovine incisor roots were endodontically treated and prepared for cementation of the Fibrekor posts. The cements were mixed as instructed, dispensed in the canal, the posts were seated and the curing performed as follows: a) no light activation; b) light-activation immediately after seating the post, and; c) light-activation delayed 5 minutes after seating the post. The teeth were stored in water and retrieved for analysis after 7 days and 3 months. The roots were longitudinally sectioned and the microhardness was determined at the cervical, middle and apical regions along the cement line. The data was analyzed by the three-way ANOVA test (curing mode, storage time and thirds) for each cement. The Tukey test was used for the post-hoc analysis. Results: Light-activation resulted in a significant increase in the microhardness. This was more evident for the cervical region and for the Panavia cement. Storage in water for 3 months caused a reduction of the micro-hardness for both cements. The U100 cement showed less variation in the micro-hardness regardless of the curing protocol and storage time. Conclusions: The micro-hardness of the cements was affected by the curing and storage variables and were material-dependent.

The effect of polymerization procedure on Vickers hardness of dual-curing resin cements

To investigate the surface hardness (Vickers hardness, HVN) of one light-curing flowable resin composite and five dual-curing resin cements after different polymerization procedures.

Light curing through glass ceramics: effect of curing mode on micromechanical properties of dual-curing resin cements

OBJECTIVES The aim of this study was to investigate micromechanical properties of five dual-curing resin cements after different curing modes including light curing through glass ceramic materials. MATERIALS AND METHODS Vickers hardness (VH) and indentation modulus (Y HU) of Panavia F2.0, RelyX Unicem 2 Automix, SpeedCEM, BisCem, and BeautiCem SA were measured after 1 week of storage (37 °C, 100 % humidity). The resin cements were tested following self-curing or light curing with the second-generation light-emitting diode (LED) curing unit Elipar FreeLight 2 in Standard Mode (1,545 mW/cm(2)) or with the third-generation LED curing unit VALO in High Power Mode (1,869 mW/cm(2)) or in XtraPower Mode (3,505 mW/cm(2)). Light curing was performed directly or through glass ceramic discs of 1.5 or 3 mm thickness of IPS Empress CAD or IPS e.max CAD. VH and Y HU were analysed with Kruskal-Wallis tests followed by pairwise Wilcoxon rank sum tests (α = 0.05). RESULTS RelyX Unicem 2 Automix resulted in the highest VH and Y HU followed by BeautiCem SA, BisCem, SpeedCEM, and finally Panavia F2.0. Self-curing of RelyX Unicem 2 Automix and SpeedCEM lowered VH and Y HU compared to light curing whereas self-curing of Panavia F2.0, BisCem, and BeautiCem SA led to similar or significantly higher VH and Y HU compared to light curing. Generally, direct light curing resulted in similar or lower VH and Y HU compared to light curing through 1.5-mm-thick ceramic discs. Light curing through 3-mm-thick discs of IPS e.max CAD generally reduced VH and Y HU for all resin cements except SpeedCEM, which was the least affected by light curing through ceramic discs. CONCLUSIONS The resin cements responded heterogeneously to changes in curing mode. The applied irradiances and light curing times adequately cured the resin cements even through 1.5-mm-thick ceramic discs. CLINICAL RELEVANCE When light curing resin cements through thick glass ceramic restorations, clinicians should consider to prolong the light curing times even with LED curing units providing high irradiances.

Light curing through glass ceramics with a second- and a third-generation LED curing unit: effect of curing mode on the degree of conversion of dual-curing resin cements

Objectives The aim of this study was to measure the degree of conversion (DC) of five dual-curing resin cements after different curing modes with a second- and a third-generation light-emitting diode (LED) curing unit. Additionally, irradiance of both light curing units was measured at increasing distances and through discs of two glass ceramics for computer-aided design/manufacturing (CAD/CAM). Materials and methods Irradiance and spectra of the Elipar FreeLight 2 (Standard Mode (SM)) and of the VALO light curing unit (High Power Mode (HPM) and Xtra Power Mode (XPM)) were measured with a MARC radiometer. Irradiance was measured at increasing distances (control) and through discs (1.5 to 6 mm thickness) of IPS Empress CAD and IPS e.max CAD. DC of Panavia F2.0, RelyX Unicem 2 Automix, SpeedCEM, BisCem, and BeautiCem SA was measured with an attenuated total reflectance–Fourier transform infrared spectrometer when self-cured (negative control) or light cured in SM for 40 s, HPM for 32 s, or XPM for 18 s. Light curing was performed directly (positive control) or through discs of either 1.5- or 3-mm thickness of IPS Empress CAD or IPS e.max CAD. DC was analysed with Kruskal–Wallis tests followed by pairwise Wilcoxon rank sum tests (α = 0.05). Results Maximum irradiances were 1,545 mW/cm2 (SM), 2,179 mW/cm2 (HPM), and 4,156 mW/cm2 (XPM), and all irradiances decreased by >80 % through discs of 1.5 mm, ≥95 % through 3 mm, and up to >99 % through 6 mm. Generally, self-curing resulted in the lowest DC. For some cements, direct light curing did not result in higher DC compared to when light cured through ceramic discs. For other cements, light curing through ceramic discs of 3 mm generally reduced DC. Conclusions Light curing was favourable for dual-curing cements. Some cements were more susceptible to variations in curing mode than others. Clinical relevance When light curing a given cement, the higher irradiances of the third-generation LED curing unit resulted in similar DC compared to the second-generation one, though at shorter light curing times.

The effects of exposure time on the surface microhardness of three dual-cured dental resin cements

This study evaluated the exposure time of light-curing of the polymers used for cementation on microhardness test in different storage times. The polymers (specifically called resin cements) were RelyX ARC, RelyX U100, and SET. Five specimens of each group were prepared and photo-polymerized with exposure times of 20 s and 180 s, using a LED polymerization unit with wavelength of 440 ~ 480 nm and light output was consistently 1,500 mW/cm2. The Vickers hardness test was performed in a MMT-3 Microhardness Tester. Data were submitted to ANOVA and Tukey's test (α = 0.05). The values of RelyX ARC showed statistically significant difference to groups with light exposure when considering only chemical cure (p < 0.05). The groups with light exposure (20 s and 180 s) showed no significant difference between them (p > 0.05). The RelyX U100 cured only chemically showed statistically significant difference between 48 h and 7 days (p < 0.05). The SET resin cement showed no significant difference to groups without light exposure for all storage times (p > 0.05). The values of hardening of the dual-cured resin cements improved after setting by light and chemical activation demonstrating the importance of light curing. © 2011 by the authors.

BOND STRENGTH DURABILITY of SELF-ETCHING ADHESIVES and RESIN CEMENTS TO DENTIN

Objectives: To evaluate the microtensile bond strength (mu TBS) of one-(Xeno III, Dentsply) and two-step (Tyrian-One Step Plus, Bisco) self-etching adhesive systems bonded to dentin and cemented to chemically cured (C&B Metabond) or light-cured paste of a dual-cure resin cement (Variolink II, Ivoclar) within a short (24 h) and long period of evaluation (90 days). Material and Methods: Forty recently extracted human molars had their roots removed and their occlusal dentin exposed and ground wet with 600-grit SiC paper. After application of one of the adhesives, the resin cement was applied to the bonded surface and a composite resin block was incrementally built up to a height of 5 mm (n = 10). The restored teeth were stored in distilled water at 37 C for 7 days. The teeth were then cut along two axes (x and y), producing beam-shaped specimens with 0.8 mm(2) cross-sectional area, which were subjected to mu TBS testing at a crosshead speed of 0.05 mm/min and stressed to failure after 24 h or 90 days of storage in water. The mu TBS data in MPa were subjected to three-way analysis of variance and Tukey's test (alpha = 0.05). Results: The interaction effect for all three factors was statistically significant (three-way ANOVA, p < 0.001). All eight experimental means (MPa) were compared by the Tukey's test (p < 0.05) and the following results were obtained: Tyrian-One Step Plus /C&B/24 h (22.4 +/- 7.3); Tyrian-One Step Plus /Variolink II/24 h (39.4 +/- 11.6); Xeno III/C&B/24 h (40.3 +/- 12.9); Xeno III/Variolink II/24 h (25.8 +/- 10.5); Tyrian-One Step Plus / C&B/90 d (22.1 +/- 12.8) Tyrian-One Step Plus/VariolinkII/90 d (24.2 +/- 14.2); Xeno III/C&B/90 d (27.0 +/- 13.5); Xeno III/Variolink II/90 d (33.0 +/- 8.9). Conclusions: Xeno III/Variolink II was the luting agent/adhesive combination that provided the most promising bond strength after 90 days of storage in water.