The effect of ionizing radiation on properties of fluoride-releasing restorative materials

Abstract The purpose of this study was to evaluate the effect of ionizing radiation from high energy X-ray on fluoride release, surface roughness, flexural strength, and surface chemical composition of the materials. The study groups comprised five different restorative materials: Beautifil II, GCP Glass Fill, Amalgomer CR, Zirconomer, and Fuji IX GP. Twenty disk-shaped specimens (8x2 mm) for fluoride release and 20 bar-shaped specimens (25 x 2x 2 mm) for flexural strength were prepared from each material. Each material group was divided into two subgroups: irradiated (IR) and non-irradiated (Non-IR). The specimens from IR groups were irradiated with 1.8 Gy/day for 39 days (total IR = 70.2 Gy). The amount of fluoride released into deionized water was measured using a fluoride ion-selective electrode and ion analyzer after 24 hours and on days 2, 3, 7, 15, 21, 28, 35, and 39 (n = 10). The flexural strength was evaluated using the three-point bending test (n = 10). After the period of measurement of fluoride release, seven specimens (n = 7) from each group were randomly selected to evaluate surface roughness using AFM and one specimen was randomly selected for the SEM and EDS analyses. Data were analyzed with two-way ANOVA and Tukey tests (p = 0.05). The irradiation significantly increased fluoride release and surface roughness for Amalgomer CR and Zirconomer groups (p < 0.05). No significant change in flexural strength of the materials was observed after irradiation (p > 0.05). The ionizing radiation altered the amount of fluoride release and surface roughness of only Amalgomer CR and Zirconomer. The effect could be related to the chemical compositions of materials.

Structural and mechanical properties of a giomer-based bulk fill restorative in different curing conditions

ABSTRACT Objective: The main goal of this study was to compare the polymerization degree of bulk-fill giomer resin cured with three different light-curing units (LCUs): a polywave third-generation (Valo); a monowave (DemiUltra: DU); and a second-generation LED (Optima 10: Opt) LCUs by using structural and mechanical properties. Material and methods: Giomer samples of 2 and 4 mm cured with three LCUs were employed in vitro analysis. The degree of curing (DC%) was determined with Fourier-Transform Infrared Spectroscopy (FTIR). Microstructural features were observed with scanning electron microscopy (SEM). Flexural strength (FS), compression strength (CS), elastic modulus and fracturing strain were determined for mechanical properties. Surface microhardness (SMH) values were also measured. Oneway ANOVA, two-way analysis of variance and Tukey multiple comparison tests were used for statistically analyzing the FS and SMH. Results: DC% values were 58.2, 47.6, and 39.7 for the 2 mm samples cured with DU, Opt., and Valo LCUs, respectively. DC% values of the 4 mm samples were 50.4, 44.6, and 38.2 for DU, Opt, and Valo, respectively. SMH values were Valo, Opt<DU at top of the samples; Valo<DU, Opt at 2 mm, and DU, Valo<Opt at 4 mm depth. Giomer samples cured with Opt and DU exhibited higher FS values than Valo. CS values were similar but compressive modulus and fracturing strain (%) varied depending on the curing protocol. Conclusions: Based on the results, it can be concluded that curing device and protocol strongly affect crosslinking reactions and thus DC%, SMH, compressive modulus and strain at break values. Consequently, it can be deduced that curing protocol is possibly the most important parameter for microstructure formation of highly-filled composite restoratives because it may bring some structural defects and physical frailties on restorations due to lower degree of polymerization.

The influence of "C-factor" and light activation technique on polymerization contraction forces of resin composite

OBJECTIVES: This study evaluated the influence of the cavity configuration factor ("C-Factor") and light activation technique on polymerization contraction forces of a Bis-GMA-based composite resin (Charisma, Heraeus Kulzer). MATERIAL AND METHODS: Three different pairs of steel moving bases were connected to a universal testing machine (emic DL 500): groups A and B - 2x2 mm (CF=0.33), groups C and D - 3x2 mm (CF=0.66), groups e and F - 6x2 mm (CF=1.5). After adjustment of the height between the pair of bases so that the resin had a volume of 12 mm³ in all groups, the material was inserted and polymerized by two different methods: pulse delay (100 mW/cm² for 5 s, 40 s interval, 600 mW/cm² for 20 s) and continuous pulse (600 mW/cm² for 20 s). Each configuration was light cured with both techniques. Tensions generated during polymerization were recorded by 120 s. The values were expressed in curves (Force(N) x Time(s)) and averages compared by statistical analysis (ANOVA and Tukey's test, p<0.05). RESULTS: For the 2x2 and 3x2 bases, with a reduced C-Factor, significant differences were found between the light curing methods. For 6x2 base, with high C-Factor, the light curing method did not influence the contraction forces of the composite resin. CONCLUSIONS: Pulse delay technique can determine less stress on tooth/restoration interface of adhesive restorations only when a reduced C-Factor is present.

Effect of reduced exposure times on the cytotoxicity of resin luting cements cured by high-power led

OBJECTIVE: Applications of resin luting agents and high-power light-emitting diodes (LED) light-curing units (LCUs) have increased considerably over the last few years. However, it is not clear whether the effect of reduced exposure time on cytotoxicity of such products have adequate biocompatibility to meet clinical success. This study aimed at assessing the effect of reduced curing time of five resin luting cements (RLCs) polymerized by high-power LED curing unit on the viability of a cell of L-929 fibroblast cells. MATERIAL AND METHODS: Disc-shaped samples were prepared in polytetrafluoroethylene moulds with cylindrical cavities. The samples were irradiated from the top through the ceramic discs and acetate strips using LED LCU for 20 s (50 percent of the manufacturer's recommended exposure time) and 40 s (100 percent exposure time). After curing, the samples were transferred into a culture medium for 24 h. The eluates were obtained and pipetted onto L-929 fibroblast cultures (3x10(4) per well) and incubated for evaluating after 24 h. Measurements were performed by dimethylthiazol diphenyltetrazolium assay. Statistical significance was determined by two-way ANOVA and two independent samples were compared by t-test. RESULTS: Results showed that eluates of most of the materials polymerized for 20 s (except Rely X Unicem and Illusion) reduced to a higher extent cell viability compared to samples of the same materials polymerized for 40 s. Illusion exhibited the least cytotoxicity for 20 s exposure time compared to the control (culture without samples) followed by Rely X Unicem and Rely X ARC (90.81 percent, 88.90 percent, and 83.11 percent, respectively). For Rely X ARC, Duolink and Lute-It 40 s exposure time was better (t=-1.262 p=0,276; t=-9.399 p=0.001; and t=-20.418 p<0.001, respectively). CONCLUSION: The results of this study suggest that reduction of curing time significantly enhances the cytotoxicity of the studied resin cement materials, therefore compromising their clinical performance.

Light-activation through indirect ceramic restorations: does the overexposure compensate for the attenuation in light intensity during resin cement polymerization?

OBJECTIVES: This study evaluated the effects of light exposure through simulated indirect ceramic restorations (SICR) on hardness (KHN) of dual-cured resin cements (RCs), immediately after light-activation and 24 h later. MATERIAL AND METHODS: Three dual-cured RCs were evaluated: Eco-Link (Ivoclar Vivadent), Rely X ARC (3M ESPE), and Panavia F (Kuraray Medical Inc.). The RCs were manipulated in accordance to the manufacturers' instructions and were placed into cylindrical acrylic matrixes (1-mm-thick and 4-mm diameter). The RC light-activation (Optilux 501; Demetron Kerr) was performed through a glass slide for 120 s (control group), or through 2-mm or 4-mm thick SICRs (IPS Empress II; Ivoclar Vivadent). The specimens were submitted to KHN analysis immediately and 24 h after light-activation. The data obtained at the 2 evaluation intervals were submitted to 2-way ANOVA repeated measures and post-hoc Tukey's test (pre-set alpha of 5 percent). RESULTS: Lower KHN was observed when light-activation was performed through SICRs for Eco-Link at all evaluation intervals and for Rely X ARC 24 h later. For Panavia F, no significant difference in KHN was observed between control and experimental groups, regardless of evaluation interval. Most groups exhibited higher KHN after 24 h than immediately after light-activation, with the exception of Rely X ARC light-activated through SICR, as no significant difference in KHN was found between evaluation intervals. CONCLUSIONS: Light overexposure did not compensate for light intensity attenuation due to the presence of SICR when Rely X and Eco-Link were used. Although hardness of such RCs increased over a 24-h interval, the RCs subjected to light overexposure did not reach the hardness values exhibited after direct light exposure.

A critical analysis of the degree of conversion of resin-based luting cements

OBJECTIVE: This study analyzed the degree of conversion (DC percent) of four resin-based cements (All Ceram, Enforce, Rely X ARC and Variolink II) activated by two modes (chemical and dual), and evaluated the decrease of DC percent in the dual mode promoted by the interposition of a 2.0-mm-thick IPS Empress 2 disc. MATERIAL AND METHODS: In the chemical activation, the resin-based cements were prepared by mixing equal amounts of base and catalyst pastes. In the dual activation, after mixing, the cements were light-activated at 650 mW/cm² for 40 s. In a third group, the cements were light-activated through a 2.0-mm-thick IPS Empress 2 disc. The DC percent was evaluated in a FT-IR spectrometer equipped with an attenuated total reflectance crystal (ATR). The data were analyzed by two-way ANOVA and Tukey's HSD test. RESULTS: For all resin-based cements, the DC percent was significantly higher with dual activation, followed by dual activation through IPS Empress 2, and chemical activation (p<0.05). Irrespective of the activation mode, Rely X presented the highest DC percent (p<0.05). Chemically activated Variolink and All Ceram showed the worst results (p<0.05). The DC percent decreased significantly when activation was performed through a 2.0-mm-thick IPS Empress 2 disc (p<0.05). CONCLUSION: The results of the present study suggest that resin-based cements could present low DC percent when the materials are dually activated through 2.0 mm of reinforced ceramic materials with translucency equal to or less than that of IPS-Empress 2.

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. CONCLUSION: 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.

Influence of post-cure treatments on hardness and marginal adaptation of composite resin inlay restorations: an in vitro study

OBJECTIVES: The purpose of this study was to evaluate the Vickers hardness number (VHN) and the in vitro marginal adaptation of inlay restorations of three hybrid composite resins (Filtek Z250, Opallis and Esthet-X) subjected to two post-cure treatments. MATERIAL AND METHODS: For the microhardness test, three different groups were prepared in accordance with the post-cure treatments: control group (only light cure for 40 s), autoclave group (light cure for 40 s + autoclave for 15 min at 130ºC); and microwave group (light cure for 40 s + microwave for 3 min at 450 W). To assess the marginal adaptation, the composite resin was inserted incrementally into a mesial-occlusal-distal cavity brass mold and each increment light-cured for 40 s. A previous reading in micrometers was taken at the cervical wall, using a stereomicroscope magnifying glass equipped with a digital video camera and image-analysis software. Subsequently, the specimens were subjected to the post-cure treatments (autoclave and microwave) and a reading was taken again at the cervical wall. Data were compared using ANOVA for the hardness test, split-plot ANOVA for the adaptation assessment and Tukey's test for multiple comparisons. A significance level of 5 percent was adopted for all analyses. RESULTS: The post-cure treatments increased the hardness of conventional composites (p<0.001) and the gap values of inlay restorations (p<0.01). Filtek Z250 showed higher hardness (p<0.001) and lower gap values than Opallis and Esthet-X (p<0.05). Gap values did not exceed 90 µm for any of the experimental conditions. CONCLUSION: The post-cure treatments increased the VHN and the gap values on the cervical floor of composite resin inlays. Moreover, Filtek Z250 showed the best results, with higher hardness and lower gap values.

Effect of gamma irradiation on fluoride release and antibacterial activity of resin dental materials

This study evaluated the effect of gamma irradiation on fluoride release and antibacterial activity of FluroShield (FS) and Clearfil Protect Bond (CPB). Four groups were formed: G1-FS + gamma; G2-FS without gamma; G3-CPB + gamma; G4-CPB without gamma. For fluoride release analysis, 12 disks of each material were prepared and covered with nail polish, except for one side (50.4 mm² area). G1 and G3 were sterilized with a 14.5 KGy dose at 27ºC for 24 h, while G2 and G4 (controls) were not sterilized and were maintained under the same time and temperature conditions. Fluoride release measurements were made in duplicate (n=6) by an ion specific electrode. The antibacterial activity of the CPB and FS against Streptococcus mutans after gamma sterilization was evaluated by the agar-disc diffusion method. The diameter of the zones of microbial growth inhibition was recorded after 48 h. Data were analyzed statistically by ANOVA and Tukey's test (α=5 percent). Gamma sterilization decreased the fluoride release of FS by approximately 50 percent, while CPB was not affected. There was no statistically significant difference (p>0.05) in the antibacterial effect of CPB between gamma and non-gamma sterilization groups. FS presented no antibacterial activity. Gamma irradiation decreased the fluoride release of FS, but did not affect the antibacterial activity of the studied materials.

Este estudo avaliou o efeito da esterilização com raios-gama na liberação de flúor e atividade antibacteriana de materiais resinosos, Fluroshield (FS) e Clearfil Protect Bond (CPB). Quatro grupos foram formados: G1-FS e gama; G2-FS sem gama; G3-CPB e gama; G4-CPB sem gama. Doze discos de cada material foram preparados para análise de liberação de flúor, os quais foram cobertos com esmalte de unha, exceto em um lado com 50,4 mm² de área. G1 e G3 foram esterilizados com dose de 14,5 KGy por 24 h/27ºC, enquanto G2 e G4 (controles) não foram esterilizados e foram mantidos sob as mesmas condições de tempo e temperatura. As leituras de liberação de flúor foram feitas em duplicata (n=6) por um eletrodo específico. A atividade antibacteriana foi avaliada pelo teste de difusão em agar. Os halos de inibição foram medidos após 48 h. Os dados foram analisados pelos testes ANOVA e Tukey (α=5 por cento). A esterilização gama diminuiu a liberação de flúor de FS em cerca de 50 por cento, enquanto CPB não foi afetado. Não houve diferença estatisticamente significante entre os grupos esterilizados e controle no efeito antibacteriano do CPB. FS não apresentou atividade antibacteriana. A esterilização gama diminuiu a liberação de flúor de FS, mas não afetou a atividade antibacteriana dos materiais estudados.

Degree of conversion of adhesive systems light-cured by LED and halogen light

This study evaluated the effect of blue light emitting diode (LED) and quartz tungsten halogen (QTH) on the degree of conversion (DC) of an etch-and-rinse Single Bond adhesive system (SB) and a mixture composed of primer solution and resin bond from Clearfil SE Bond self-etching adhesive system (CB) using Fourier transform infrared analysis (FTIR). Adhesives were applied to potassium bromide pellet surfaces and FTIR analyses were performed before and after photo-activation for 10 s with either LED (Freelight 1 - 400 mw/cm²) or QTH (XL 3000 - 630 mw/cm²) light-curing units (n=8). Additional FTIR spectra were obtained from photo-activated samples stored in distilled water for 1 week. The DC was calculated by comparing the spectra obtained from adhesive resins before and after photo-activation. The results were analyzed by two-way split-plot ANOVA and Tukey's test (p<0.05). Both adhesive systems exhibited low DC ( percent) immediately after photo-activation (SB/QTH: 18.7 ± 3.9; SB/LED: 13.5 ± 3.3; CF/QTH: 13.6 ± 1.9; CF/LED: 6.1 ± 1.0). The DC of samples light-cured with LED was lower than DC of those light-cured with QTH, immediately after light curing and after 1 week (SB/QTH: 51.3 ± 6.6; SB/LED: 50.3 ± 4.8; CF/QTH: 56.5 ± 2.9; CF/LED: 49.2 ± 4.9). The LED curing unit used to photo-activate the adhesive resins promoted lower DC than the QTH curing unit both immediately after light curing and 1 week after storage in water.

Este estudo avaliou a influência de sistemas de fotoativação no grau de conversão (GC) de sistemas adesivos por meio da análise infravermelha transformada de Fourier (FTIR). Os sistemas adesivos Single Bond (SB) e Clearfil SE Bond (CF) foram aplicados em pastilhas de brometo de potássio e fotoativados com luz halógena (XL 3000 - 630 mw/cm²) (QTH) e LED (Elipar Freelight 1 - 400 mw/cm²) por 10 s (n=8). Foram obtidos espectros de FTIR antes e imediatamente após a fotoativação, e tambem após 1 semana de armazenamento em água destilada. Calculou-se o GC comparando-se a razão entre os picos das bandas dos espectros, antes e após a fotoativação. Os resultados de GC foram submetidos à ANOVA e ao teste de Tukey (p<0,05). Para ambos os sistemas adesivos, o GC ( por cento) obtido imediatamente após a fotoativação com LED foi inferior ao obtido utilizando-se QTH (SB/QTH: 18,7 ± 3,9; SB/LED: 13,5 ± 3,3; CF/QTH: 13,6 ± 1,9; CF/LED: 6,1 ± 1,0). Após uma semana foi observado um aumento significativo no GC de todos os grupos, porém os valores dos grupos fotoativados com LED mantiveram-se inferiores aos obtidos com QTH (SB/QTH: 51,3 ± 6,6; SB/LED: 50,3 ± 4,8; CF/QTH: 56,5 ± 2,9; CF/LED: 49,2 ± 4,9). O GC dos adesivos fotoativados com LED foi inferior ao observado após fotoativação com QTH, imediatamente após fotoativação como após 1 semana de armazenamento em água.