RESUMO
OBJECTIVE: To formulate an experimental methacrylate-based photo-polymerizable resin for 3D printing with ytterbium trifluoride as filler and to evaluate the mechanical, physicochemical, and biological properties. METHODS: Resin matrix was formulated with 60 wt% UDMA, 40 wt% TEGDMA, 1 wt% TPO, and 0.01 wt% BHT. Ytterbium Trifluoride was added in concentrations of 1 (G1 %), 2 (G2 %), 3 (G3 %), 4 (G4 %), and 5 (G5 %) wt%. One group remained without filler addition as control (GC). The samples were designed in 3D builder software and printed using a UV-DLP 3D printer. The samples were ultrasonicated with isopropanol and UV cured for 60 min. The resins were tested for degree of conversion (DC), flexural strength, Knoop microhardness, softening in solvent, radiopacity, colorimetric analysis, and cytotoxicity (MTT and SRB). RESULTS: Post-polymerization increased the degree of conversion of all groups (p < 0.05). G2 % showed the highest DC after post-polymerization. G2 % showed no differences in flexural strength from the G1 % and GC (p > 0.05). All groups showed a hardness reduction after solvent immersion. No statistical difference was found in radiopacity, softening in solvent (ΔKHN%), colorimetric spectrophotometry, and cytotoxicity (MTT) (p > 0.05). G1 % showed reduced cell viability for SRB assay (p < 0.05). SIGNIFICANCE: It was possible to produce an experimental photo-polymerizable 3D printable resin with the addition of 2 % ytterbium trifluoride as filler without compromising the mechanical, physicochemical, and biological properties, comparable to the current provisional materials.
Assuntos
Dureza , Teste de Materiais , Metacrilatos , Impressão Tridimensional , Metacrilatos/química , Resistência à Flexão , Polimerização , Polietilenoglicóis/química , Resinas Compostas/química , Ácidos Polimetacrílicos/química , Poliuretanos/química , Colorimetria , Propriedades de SuperfícieRESUMO
To evaluate the polymerization shrinkage stress and cuspal strain (CS) generated in an artificial (typodont) and in a natural tooth using different resin composites. Twenty artificial and 20 extracted natural molars were selected. Each tooth was prepared with a 4x4 mm MOD cavity. The natural and typodont teeth were divided into four experimental groups (n=10), according to the resin composite used: Filtek Z100 (3M Oral Care) and Beautifil II LS (Shofu Dental). The cavities were filled using two horizontal increments and the CS (µS) was measured by the strain gauge method. Samples were sectioned into stick-shaped specimens and the bond strength (BS) (MPa) was evaluated using a microtensile BS test. Shrinkage stress and CS were analyzed using 3D finite element analysis. No difference was found between the type of teeth for the CS as shown by the pooled averages: Natural tooth: 541.2 A; Typodont model: 591.4 A. Filtek Z100 CS values were higher than those obtained for Beautifil II LS, regardless of the type of teeth. No statistical difference was found for the BS data. Adhesive failures were more prevalent (79.9%). High shrinkage stress values were observed for Filtek Z100 resin, regardless of tooth type. The CS of typodont teeth showed a shrinkage stress effect, generated during restoration, equivalent to that of natural teeth.
Assuntos
Resinas Compostas , Análise do Estresse Dentário , Análise de Elementos Finitos , Teste de Materiais , Polimerização , Estresse Mecânico , Resistência à Tração , Resinas Compostas/química , Humanos , Valores de Referência , Propriedades de Superfície , Reprodutibilidade dos Testes , Colagem Dentária/métodos , Coroa do DenteRESUMO
OBJECTIVE: To evaluate the effect of four different photoactivation protocols (according to "photoactivated faces" - mesial/distal, cervical/incisal or center - and "photoactivation time" - 6-3 s) of a high-power photo activator (Valo Cordless®-Ultradent) on the shear bond strength (SBS) between metal brackets and dental enamel and on the degree of conversion (DC) of an orthodontic resin. MATERIALS AND METHODS: 40 bovine incisor crowns were randomly assigned to 4 groups (n = 10). The brackets were bonded with Transbond XT® resin using 4 protocols according to the "photoactivation protocol" factor (which was subdivided into photoactivated faces and photoactivation time): V3C = 3 s + center; V6C = 6 s + center; V3M3D = 3 s on mesial + 3 s on distal; V3C3I = 3 s on cervical + 3 s on incisal. All the samples were stored for 4 months (water,37ºC) and then subjected to a SBS test (100KgF,1 mm/min). 40 resin discs were made to evaluate the monomer degree of conversion. Data from the SBS and DC were assessed by One-way ANOVA and Tukey's test (5%). Bond failures were analyzed according to the Adhesive Remnant Index (ARI) and evaluated by the Kruskal-Wallis test (5%). RESULTS: There was a statistically significant difference (p = 0.008) in the One-way ANOVA result for SBS values between all groups, but the protocols showed statistically similar results (p ≥ 0.05-Tukey's tests) concerning the photoactivated faces (V6C, V3M3D and V3C3I) and photoactivation time (V3C and V6C) factors individually. There was no statistically significant difference (p ≥ 0.05) in the One-way ANOVA result for DC values. CONCLUSION: The SBS and DC values will vary depending on the protocol applied. CLINICAL RELEVANCE: It is possible to maintain the bracket fixation quality with the use of a high-power LED photo activator associated with a shorter photoactivation time. However, it is assumed that not all types of protocols that might be applied will provide quality bonding, such as V3C, V3M3D and V3C3I, which may - depending on the SBS and DC values - affect the final treatment time, due to brackets debonding, or increase of possibility of damage to dental enamel during bracket removal. Clinical studies are suggested to confirm the hypotheses of this research.
Assuntos
Colagem Dentária , Esmalte Dentário , Análise do Estresse Dentário , Teste de Materiais , Braquetes Ortodônticos , Distribuição Aleatória , Cimentos de Resina , Resistência ao Cisalhamento , Animais , Bovinos , Colagem Dentária/métodos , Cimentos de Resina/química , Esmalte Dentário/química , Propriedades de Superfície , Técnicas In Vitro , Fatores de Tempo , Coroa do Dente , PolimerizaçãoRESUMO
In this study, lignin derived from corncobs was chemically modified by substituting the hydroxyl groups present in its structure with methacrylate groups through a catalytic reaction using methacrylic anhydride, resulting in methacrylated lignin (ML). These MLs were incorporated in polymerization reaction of the monomer 2-[(acryloyloxy)ethyl trimethylammonium] chloride (Cl-AETA) and Cl-AETA, Cl-AETA/ML polymers were obtained, characterized (spectroscopic, thermal and microscopic analysis), and evaluated for removing Cr (VI) and As (V) from aqueous media in function of pH, contact time, initial metal concentrations and adsorbent amount. The Cl-AETA/ML polymers followed the Langmuir adsorption model for the evaluated metal anions and were able to remove up to 91 % of Cr (VI) with a qmax (maximum adsorption capacity) of 201 mg/g, while for As (V), up to 60 % could be removed with a qmax of 58 mg/g. The results demonstrate that simple modifications in lignin enhance its functionalization and properties, making it suitable for removing contaminants from aqueous media, showing promising results for potential future applications.
Assuntos
Cromo , Lignina , Poluentes Químicos da Água , Lignina/química , Cromo/química , Cromo/isolamento & purificação , Adsorção , Poluentes Químicos da Água/química , Poluentes Químicos da Água/isolamento & purificação , Purificação da Água/métodos , Polímeros/química , Polímeros/síntese química , Água/química , Concentração de Íons de Hidrogênio , PolimerizaçãoRESUMO
CONTEXT: Molecularly imprinted polymers (MIPs) have promising applications as synthetic antibodies for protein and peptide recognition. A critical aspect of MIP design is the selection of functional monomers and their adequate proportions to achieve materials with high recognition capacity toward their targets. To contribute to this goal, we calibrated a molecular dynamics protocol to reproduce the experimental trends in peptide recognition of 13 pre-polymerization mixtures reported in the literature for the peptide toxin melittin. METHODS: Three simulation conditions were tested for each mixture by changing the box size and the number of monomers and cross-linkers surrounding the template in a solvent-explicit environment. Fully atomistic MD simulations of 350 ns were conducted with the AMBER20 software, with ff19SB parameters for the peptide, gaff2 parameters for the monomers and cross-linkers, and the OPC water model. Template-monomer interaction energies under the LIE approach showed significant differences between high-affinity and low-affinity mixtures. Simulation systems containing 100 monomers plus cross-linkers in a cubic box of 90 Å3 successfully ranked the mixtures according to their experimental performance. Systems with higher monomer densities resulted in non-specific intermolecular contacts that could not account for the experimental trends in melittin recognition. The mixture with the best recognition capacity showed preferential binding to the 13-26-α-helix, suggesting a relevant role for this segment in melittin imprinting and recognition. Our findings provide insightful information to assist the computational design of molecularly imprinted materials with a validated protocol that can be easily extended to other templates.
Assuntos
Simulação de Dinâmica Molecular , Peptídeos , Peptídeos/química , Meliteno/química , Polimerização , Polímeros Molecularmente Impressos/química , Impressão Molecular/métodosRESUMO
The present study examined different concentrations of the butylated hydroxytoluene (BHT) inhibitor on the kinetics of conversion, polymerization shrinkage stress, and other correlated physicochemical properties of experimental resin composites (ERC). A model composite was formulated with 75 wt% filler containing 0.5 wt% camphorquinone and 1 wt% amine with BHT concentrations of 0.01 wt% (BHT-0.01); 0.1 wt% (BHT-0.1); 0.25 wt% (BHT-0.25); 0.5 wt% (BHT-0.5); 1 wt% (BHT-1), and control (no BHT). They were tested on polymerization shrinkage stress (PSS; n = 5), degree of conversion (DC; n = 3), maximum polymerization rate (RpMAX; n = 5), water sorption (Wsp; n = 0), and solubility (Wsl; n = 10), flexural strength (FS; n = 10), flexural modulus (FM; n = 10), Knoop microhardness (KH; n = 10), and microhardness reduction (HR; n = 10). Data concerning these tests were submitted to one-way ANOVA and Tukey's test (α = 0.05; ß = 0.2). BHT-0.25, BHT-0.5, and BHT-1 showed a gradually significant decrease in PSS (p = 0.037); however, BHT-1 demonstrated a decrease in the physicochemical properties tested. Thus, within the limitations of this study, it was possible to conclude that BHT concentrations between 0.25 and 0.5 wt% are optimal for reducing shrinkage stress without affecting other physicochemical properties of ERCs.
Assuntos
Hidroxitolueno Butilado , Resinas Compostas , Teste de Materiais , Polimerização , Estresse Mecânico , Hidroxitolueno Butilado/química , Resinas Compostas/química , Fenômenos Químicos , Solubilidade , Água/química , DurezaRESUMO
OBJECTIVES: This study evaluated the depth of cure (DoC) of eight resin-based composites (RBCs) photocured using one multipeak light-curing unit (LCU) on the standard output setting for the manufacturer's RBC recommended exposure time and at a higher irradiance for 3 seconds. METHODS: Three conventional RBCs: Tetric EvoCeram (Evo), Tetric N-Ceram (Cer), Tetric Prime (Pri); and five bulk-fill: Tetric N-Ceram Bulk Fill (CerBF), Opus Bulk Fill APS (OpusBF), Opus Bulk Fill Flow APS (OpusF), Tetric PowerFill (PFill) and Tetric PowerFlow (PFlow) were examined. Only PFill and PFlow are formulated to be photocured in 3 seconds. The RBCs were packed into a metal mold and photocured using a Bluephase PowerCure LCU for the RBC manufacturer's recommended exposure time on the standard mode and using the 3-second high irradiance mode. After photocuring, the specimens were immersed in a solvent for 1 hour. The length of the remaining RBC was measured and divided by 2. Data were analyzed using two-way analysis of variance (ANOVA) followed by the Tukey post hoc multiple comparison test (α=0.05). RESULTS: There was no significant difference in the DoC values for PFill and PFlow when photocured using the 3-second high irradiance protocol compared to the lower irradiance standard mode protocol. All other RBCs had significantly lower DoC values (p<0.001) when photocured off-label using the 3-second high irradiance mode. CONCLUSION: Of the eight RBCs tested, only PFill and PFlow achieved the same DoC when the high irradiance 3-second curing method was used compared to when their longer lower irradiance protocol was used.
Assuntos
Resinas Compostas , Lâmpadas de Polimerização Dentária , Teste de Materiais , Resinas Compostas/uso terapêutico , Humanos , Fatores de Tempo , Polimerização , Cura Luminosa de Adesivos Dentários/métodos , Materiais Dentários/uso terapêutico , Materiais Dentários/química , Metacrilatos , Propriedades de SuperfícieRESUMO
OBJECTIVES: The study aimed to assess the impact of diphenyliodonium hexafluorophosphate (DPI) on the physicochemical properties of experimental resin composites (ECRs) featuring reduced concentrations of camphorquinone (CQ)/amine. METHODS: Five concentrations of CQ (0.125, 0.25, 0.5, 0.75, and 1 mol%) with dimethylaminoethyl amine benzoate (EDAB) in a 1:2 mol% ratio (CQ:EDAB) were incorporated into a 50:50 mass% monomer blend of bisphenol glycidyl methacrylate (BisGMA) and triethyleneglycol dimethacrylate (TEGDMA). An additional 5 groups with the same CQ:EDAB concentrations had 0.5 mol% DPI added. Each resin group contained 60 wt% of 0.7 µm barium-alumino-silicate glass. Light transmission (n = 3), real-time degree of polymerization (n = 3), temperature change during polymerization (n = 5), polymerization shrinkage strain (n = 3), flexural strength, and modulus (n = 12), as well as water sorption and solubility (n = 5), were evaluated. Data were analyzed using two-way ANOVA and Tukey's post-hoc test (α = 0.05). RESULTS: Light transmission was reduced in groups containing 0.125 and 0.25 mol% of CQ without DPI. DPI increased temperature, degree and rate of polymerization, despite the reduction in CQ/amine concentration. Additionally, there was an increase in polymerization shrinkage strain, flexural strength and modulus, and a reduction in water sorption and solubility in ECRs with DPI, even with lower concentrations of CQ/EDAB. SIGNIFICANCE: DPI improved the assessed properties of composites across various concentrations of CQ/EDAB, showing the benefit of reducing the quantity of CQ used without compromising the properties and curing of the resin composites.
Assuntos
Resinas Compostas , Teste de Materiais , Polietilenoglicóis , Polimerização , Ácidos Polimetacrílicos , Terpenos , Resinas Compostas/química , Terpenos/química , Polietilenoglicóis/química , Ácidos Polimetacrílicos/química , Bis-Fenol A-Glicidil Metacrilato/química , Propriedades de Superfície , Oniocompostos/química , Poliuretanos/química , Resinas Acrílicas , Compostos de Bifenilo , Cânfora/análogos & derivadosRESUMO
Objective: To evaluate the enamel bonding ability and orthodontic adhesive resin degree of conversion using the experimental bracket design. Material and Methods. Thirteen bovine teeth were used in the study. The experimental bracket was modified with a translucent region in the center of its body. After enamel etching, Orthocem orthodontic adhesive (FGM, Joinville, Brazil) was applied on the bracket base for bonding. The groups were divided as follows (n = 10 per group): (1) control (CB) with standard brackets and (2) spot bracket (SB) with experimental brackets featuring a 0.8 mm translucent region at the center using carbide bur. Shear bond strength (SBS) was evaluated after 24 hours in a universal testing machine and adhesive remnant index (ARI). The degree of conversion (DC) was analyzed using Raman spectroscopy (n = 3 per group). Data were then analyzed using Student's t-test and Mann-Whitney statistical methods. Results: The SB group exhibited a higher mean SBS (10.33 MPa) compared to the CB Group (8.77 MPa). However, there was no statistical difference between the groups (p = 0.376). Both SB and CB groups had a mean ARI score of 1. Raman analysis revealed a higher degree of conversion in the SB group (49.3%) compared to the CB group (25.9%). Conclusions: The experimental support showed a higher degree of adhesive conversion, although there was no significant increase in bond strength.
Assuntos
Resinas Compostas , Colagem Dentária , Esmalte Dentário , Braquetes Ortodônticos , Polimerização , Resistência ao Cisalhamento , Animais , Bovinos , Colagem Dentária/métodos , Esmalte Dentário/química , Resinas Compostas/química , Teste de Materiais , Cimentos Dentários/química , Cimentos de Resina/químicaRESUMO
This study examined the effect of high irradiance and short exposure times on the depth of cure of six resin-based composites (RBCs). Bluephase PowerCure and the Valo X light-curing units (LCUs) were used to photocure bulk-fill RBCs for their recommended exposure times: Admira Fusion x-tra (AFX/20s), Aura Bulk Fill (ABF/20s), Filtek One Bulk Fill (FOB/20s), Opus Bulk Fill APS (OBF/30s), Tetric EvoCeram Bulk Fill (TEC/10s) and Tetric PowerFill (TPF/10s). In addition, all bulk-fill RBCs were tested for depth of cure with one short 3 s exposure time from the Bluephase PowerCure or the Valo X in the Xtra Power mode. The RBCs (n = 10 per RBC) were inserted into a 4 mm diameter metal mold and covered by a polyester strip before being photocured. After 24 h of storage, uncured RBC was scraped away to determine the depth of cure of the RBCs. None of the RBCs achieved a 4 mm depth of cure. The depth of cure of TEC and TPF was unaffected by the exposure times (recommended or short) when using the Valo X. The depth of cure of AFX/20s, AFX/Xtra Power, ABF/Xtra Power, FOB/Xtra Power, and OBF/30s RBCs was greater when using Valo X compared to the Bluephase PowerCure. It was concluded that short exposure times can reduce depth of cure and should only be used for some RBCs.