Desenvolvimento e caracterização de nanocompósito de resina epóxi com nanopartículas de sílica para revestimento de dutos para transporte de petróleo

The use of polymer based coatings is a promising approach to reduce the corrosion problem in carbon steel pipes used for the transport of oil and gas in the oil industry. However, conventional polymer coatings offer limited properties, which often cannot meet design requirements for this type of application, particularly in regard to use temperature and wear resistance. Polymer nanocomposites are known to exhibit superior properties and, therefore, offer great potential for this type of application. Nevertheless, the degree of enhancement of a particular property is greatly dependent upon the matrix/nanoparticle material system used, the matrix/nanoparticle interfacial bonding and also the state of dispersion of the nanoparticle in the polymer matrix. The objective of the present research is to develop and characterize polymer based nanocomposites to be used as coatings in metallic pipelines for the transportation of oil and natural gas. Epoxy/SiO2 nanocomposites with nanoparticle contents of 2, 4, and 8 wt % were processed using a high-energy mill. Modifications of the SiO2 nanoparticles‟ surfaces with two different silane agents were carried out and their effect on the material properties were investigated. The state of dispersion of the materials processed was studied using Scanning and Transmission Electron Microscopy (SEM and TEM) micrographs. Thermogravimetric analysis (TG) were also conducted to determine the thermal stability of the nanocomposites. In addition, the processed nanocomposites were characterized by dynamic mechanical analysis (DMA) to investigate the effect of nanoparticles content and silane treatment on the viscoelastic properties and on the glass transition temperature. Finally, wear tests of the pin-on-disc type were carried out to determine the effects of the nanoparticles and the silane treatments studied. According to the results, the addition of SiO2 nanoparticles treated with silane increased the thermal stability, the storage modulus and Tg of the epoxy resin and decreased wear rate. This confirms that the interaction between the nanoparticles and the polymer chains plays a critical role on the properties of the nanocomposites

Morfologia e propriedades mecânicas da fibra de sisal unidirecional e em sobreposição de compósito com resina epóxi

The composites manufactured with long fibres aligned in a single direction, and overlay has been shown to have better performance than the short fibers randomly distributed. In particular, the lignocellulosic fibers extracted from the sisal leaves, used in conjunction with the epoxy resin has attracted the attention of many researchers because the final properties of the system formed. In this work composites based on epoxy resin reinforced with sisal fibers were manufactured. The sisal fibres were treated with an alkaline solution of 0.06 mol/l NaOH. The treated, and untreated fibres were subjected to tension x extension tests. The composites were manufactured in the "Lossy" mold with the specifications of the samples to be produced (300x20x4 mm). The tension tests were carried out in accordance with the ASTM standards 3039 (for the composite aligned in a single direction) and ASTM D5573 (for composites in overlay), three point bending tests were performed according to ASTM D790. Analyzing the results of the tests of tension and three point bending tests, it was observed that the composites with the configuration of overlapping had the better elastic module in both tests. As to the maximum resistance to tension, the best result was the composites aligned in a single direction. Tests of absorption of water and micrographs are in progress

Análise fractográfica do modo de falha de compósitos carbono/epóxi

A utilização de compósitos poliméricos na fabricação de aeronaves vem sendo cada vez mais intensa. em função disso, a possibilidade de ocorrer falhas em serviço de um componente fabricado em compósito polimérico torna-se cada vez maior. A análise de falhas de materiais compósitos ainda é um tema pouco explorado, principalmente no Brasil, porém vem tornando-se cada vez mais importante em apoio à área de prevenção e investigação de acidentes aeronáuticos. Este trabalho teve como objetivo a caracterização de fraturas em laminados unidirecionais de fibra de carbono de módulo intermediário com sistema de resina epóxi modificada, tipo 8552, em resistência ao cisalhamento interlaminar nas condições ambiente e saturado de umidade em câmara higrotérmica. A análise fractográfica no plano de falha dos laminados foi realizada por microscopias óptica e eletrônica de varredura. A comparação dos resultados mostrou que o condicionamento higrotérmico afetou significativamente a região de interface da resina sem alterar a adesão interfacial fibra/resina. Os aspectos de fratura presentes na região de resina, como cristas de galo e escarpas, e do reforço foram detalhados, podendo-se assim estabelecer a direção de propagação da trinca e caracterizar o modo de falha, por ser do tipo misto (arrancamento e cisalhamento simultaneamente).

Evaluation of the physical and chemical properties of two commercial and three experimental root-end filling materials

Objective. The aim of this study was to evaluate the pH, calcium release, setting time, and solubility of two commercially available mineral trioxide aggregate (MTA) cements (white MTA Angelus and MTA Bio), and of three experimental cements (light-cured MTA, Portland cement with 20% bismuth oxide and 5% calcium sulfate, and an epoxy resin-based cement).Study design. For evaluation of pH and calcium ion release, polyethylene tubes with 1.0 mm internal diameter and 10.0 mm length were filled with the cements and immediately immersed in flasks containing 10 mL deionized water. After 3, 24, 72, and 168 hours, the tubes were removed and the water from the previous container was measured for its pH and calcium content with a pH meter and an atomic absorption spectrophotometer. For analysis of the setting time, Gilmore needles weighing 100 g and 456.5 g were used, in accordance with the American Society for Testing and Materials specification no. C266-03. Solubility of each cement was also tested.Results. All the cements were alkaline and released calcium ions, with a declining trend over time. After 3 hours, Portland cement + bismuth oxide and MTA Bio had the highest pH and light-cured MTA the lowest. After 1 week, MTA Bio had the highest pH and light-cured MTA and epoxy resin-based cement the lowest. Regarding calcium ion release, after 3 hours, Portland cement + bismuth oxide showed the highest release. After 1 week, MTA Bio had the highest. Epoxy resin-based cement and light-cured MTA had the lowest calcium release in all evaluation periods. Regarding setting times, white MTA Angelus and MTA Bio had the shortest, Portland cement + bismuth oxide had an intermediate setting time, and the epoxy resin-based cement had the longest. The materials that showed the lowest solubility values were the epoxy resin-based cement, Portland cement + bismuth oxide, and light-cured MTA. The highest solubility values were presented in white MTA Angelus and MTA Bio.Conclusions. The white MTA Angelus and MTA Bio had the shortest setting times, higher pH and calcium ion release, and the highest solubility. In contrast, the epoxy resin-based cement and light-cured MTA showed lower values of solubility, pH, and calcium ion release. (Oral Surg Oral Med Oral Pathol Oral Radiol Endod 2010; 110: 250-256)

Evaluation of Ultrasonic and ErCr:YSGG Laser Retrograde Cavity Preparation

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

Effects of mechanical cycling on the bonding of zirconia and fiber posts to human root dentin

Purpose: To evaluate the effect of cyclical mechanical loading on the bond strength of a fiber and a zirconia post bonded to root dentin.Materials and Methods: Forty single-rooted human teeth (maxillary incisors and canines) were sectioned, and the root canals were prepared at 12 mm. Twenty randomly seleced specimens received a quartz fiber post (FRC) (D.T. Light-Post) and 20 others received a zirconia post (ZR) (Cosmopost). The posts were resin luted (All Bond 2 + resin cement Duo-link) and each specimen was embedded in epoxy resin inside a PVC cylinder. Ten specimens with FRC post and 10 specimens with ZR post were submitted to fatigue testing (2,000,000 cycles; load: 50 N; angle of 45 degrees; frequency: 8 Hz), while the other 20 specimens were not fatigued. Thus, 4 groups were formed: G1: FRC+O cycles; G2: FRC+2,000,000 cycles; G3: ZR+O cycles; G4: ZR+2,000,000 cycles. Later, the specimens were cut perpendicular to their long axis to form 2-mm-thick disk-shaped samples (4 sections/specimen), which were submitted to the push-out test (1 mm/min). The mean bond strength values (MPa) were calculated for each tooth (n = 10) and data were submitted to statistical analysis (alpha = 0.05).Results: Two-way ANOVA revealed that the bond strength was significantly affected by mechanical cycling (p = 0.0014) and root post (p = 0.0325). The interaction was also statistically significant (p = 0.0010). Tukey's test showed that the mechanical cycling did not affect the bonding of FRC to root dentin, while fatigue impaired the bonding of zirconium to root dentin.Conclusion: (1) the bond strength of the FRC post to root dentin was not reduced after fatigue testing, whereas the bonding of the zirconia post was significantly affected by the fatigue. (2) Cyclical mechanical loading appears to damage the bond strength of the rigid post only.

In vitro evaluation of the effectiveness of irrigants and intracanal medicaments on microorganisms within root canals

Aim To evaluate in vitro the effectiveness of sodium hypochlorite (NaOCl). chlorhexidine (CHX) and live intracanal medicaments on microorganisms within root canals.Methodology Ninety-six human single-rooted extracted teeth were used. After removing the crowns, canal preparation was completed and the external root Surfaces were coated with epoxy resin. Following sterilization. The teeth were contaminated with Candida albicans and enterococcus faecalis. and were incubated at 37 +/- 1 degreesC for 7 days. The teeth were divided according to the irrigant solution or intracanal medicament: group 1. sterile physiologic solution (SPS) and calcium hydroxide (Ca(OH)(2)) paste: group 2. SPS and camphorated paramonochlorophenol (CPMC): group 3.SPS and tricresol formalin: group 4, SPS and CaOH2 + CPMC paste: group 5, SPS and PMC furacin; group 6.2.5%, NaOCl without intracanal medication: group 7, 2.0% CHX without intracanal medication and group 8, SPS Without intracanal medication (control group). Microbiological samples were collected with sterile paper points, and bacterial growth was determined. The data were submitted to the analysis of variance (ANOVA. P = 0.05).Results For C. albicans, groups 3 and S were statistically less effective than groups 1, 2. 4 and 5 (Kruskal-Wallis (K-W) = 65.241; gl = 7; P = 0.001). For E. faecalis, groups 6 and 8 were statistically less effective than groups 1-4 and 7 (K-W = 61.048; gl = 7; P = 0.001).Conclusions Ca(OH)(2) + CPMC paste was the most effective intracanal medicament for the elimination of the two microorganisms; 2.0% CHX solution was more effective than 2.5% NaOCl against E. faecalis.

Effect of mechanical cycling on the push-out bond strength of fiber posts adhesively bonded to human root dentin

This study evaluated the effect of mechanical cycling on the bond strength of fiber posts bonded to root dentin. The hypotheses examined were that bond strength is not changed after fatigue testing and bond strength does not present vast variations according to the type of fiber post. Sixty crownless, single-rooted human teeth were endodontically treated, with the space prepared at 12 mm. Thirty specimens received a quartz fiber post (Q-FRC (DT Light-Post), and the remaining 30 specimens received a glass fiber post (G-FRC) (FRC Postec Plus). All the posts were resin luted (All Bond+Duolink), and each specimen was embedded in a cylinder with epoxy resin. The specimens were divided into six groups: G1-Q-FRC+no cycling, G2- Q-FRC+20,000 cycles (load: 50N, angle of 45 degrees; frequency: 8Hz); G3- Q-FRC+2,000,000 cycles; G4- G-FRC+no cycling; G5- G-FRC+20,000 cycles; G6- GFRC+2,000,000 cycles. The specimens were cut perpendicular to their long axis, forming 2-mm thick disc-samples, which were submitted to the push-out test. ANOVA (alpha=.05) revealed that: (a) QFRC (7.1 +/- 2.2MPa) and G-FRC (6.9 +/- 2.1MPa) were statistically similar (p=0.665); (b) the no cycling groups (7.0 +/- 2.4MPa), 20,000 cycles groups (7.0 +/- 2.1MPa) and 2,000,000 cycles groups (7.0 +/- 2.0MPa) were statistically similar (p=0.996). It concluded that mechanical cycling did not affect the bond strength of two fiber posts bonded to dentin.

BIOSENSORS FOR GLUCOSE NEEDLE-SHAPED FOR IN-VIVO MONITORING

Different procedures for obtaining a needle biosensor for the determination of glucose to be inserted subcutaneously in vivo, have been compared. Platinum wires with a diameter of 75 mum, teflon-coated were inserted in hypodermic needles and fixed with a two-component epoxy resin. Using a dip-coating procedure, several layers were deposited on electrodes. The first coating was cellulose acetate, the second was immobilized glucose oxidase (GOD) mixed with bovine serum albumin (BSA) and glutaraldheyde, the third coating was a polyurethane coating obtained with commercially available products. A large number of electrodes have been tried and statistically evaluated but they seem to be affected by poor reproducibility evidenced by a large spreading in successive calibration curves. Then, the polyurethane coating has been replaced by a thin polycarbonate membrane salinized and fixed on the tip of the needle. Reproducible results were achieved and first results of in vivo measurements on rabbits are reported.

Release of formaldehyde by 4 endodontic sealers

Objective. The purpose of this study was to evaluate the release of formaldehyde by some root canal filling materials. Study design. Two older endodontic sealers, AH 26 and Endomethasone, and 2 recently available sealers, AH Plus and Top Seal, were analyzed. Infrared and electronic spectroscopy were used to determine formaldehyde content after set of the materials. Results. Analysis showed that the AH 26 and Endomethasone sealers released formaldehyde. Although the AH Plus and Top Seal sealers have similar chemical composition, they released formaldehyde in a minimal concentration. Conclusions. The AH 26 and Endomethasone sealers released formaldehyde after setting; however, a minimum release was observed for the AH Plus and Top Seal sealers. Copyright © 1999 by Mosby, Inc.

Evaluation of apical sealing of three endodontic sealers

Aim: The apical sealing ability of three different endodontic sealers was evaluated in extracted teeth using dye penetration. Methodology: The root canals of 99 extracted human maxillary central incisors were prepared sequentially 2 mm beyond the apical foramen with a size 55 Nitiflex file. The teeth were divided into three experimental groups and obturated by lateral condensation of cold gutta-percha and one of the following sealers: group 1, zinc oxide and eugenol sealer (Fill Canal); group 2, glass ionomer sealer (Ketac-Endo) and group 3, epoxy resin sealer (AH Plus). The teeth were covered with nail varnish to within 1 mm of the apical foramen and immersed in 2% methylene blue in a reduced pressure environment for 24h. After this period, the teeth were washed and cut longitudinally for apical leakage analysis. The values were obtained from the maximum depth of leakage as well as the average between the maximum and minimum values observed for each group. Results: Statistical evaluation of the results showed no significant difference in the leakage between Fill Canal and Ketac-Endo (P > 0.05). Leakage with AH Plus was significantly less (P < 0.01) than with the other sealers. Conclusions: All three sealers allowed some leakage to occur. Leakage with AH Plus was significantly different than with Fill Canal or Ketac-Endo.

Radiographic evaluation of periradicular repair after endodontic treatment of dog's teeth with induced periradicular periodontitis

Eighty-four root canals of premolars from six dogs were left open for 7 days, and then sealed and followed for 45 days until periradicular periodontitis developed. The root canals were then treated endodontically using 5.25% sodium hypochlorite as the irrigating solution. After instrumentation, all root canals were filled with a calcium hydroxide-based antibacterial dressing (Calen PMCC or Calasept) that was left in place for 30 days. After this period the root canals were filled with gutta-percha cones and a root canal sealer (Sealapex or AH Plus)-group I: Calen PMCC + Sealapex; group II: Calasept + Sealapex; group III: Calen PMCC + AH Plus; and group IV: Calasept + AH Plus. Periapical radiographs of the teeth were made after root canal filling and after 90, 180, 270, and 360 days. Radiographic images were digitalized by scanning, and the Mocha program was used to measure the periapical lesions. Analysis showed that the lesions of groups I to III were statistically similar reduction in size, whereas group IV had a smaller reduction in lesion size (p < 0.05). Copyright © 2001 by The American Association of Endodontists.

Apical and periapical repair of dogs' teeth with periapical lesions after endodontic treatment with different root canal sealers.

The aim of this study was to evaluate the apical and periapical repair after root canal treatment of dogs' teeth with pulp necrosis and chronic periapical lesion using different root canal sealers. After periapical lesion induction, forty-four root canals of 3 dogs were submitted to biomechanical preparation using 5.25% sodium hypochlorite as an irrigating solution. A calcium hydroxide dressing (Calen PMCC) was applied for 15 days and the root canals were filled using the lateral condensation technique with gutta-percha points and Sealapex, AH Plus or Sealer Plus for sealing. After 180 days, the animals were sacrificed by anesthetic overdose and the obtained histological sections were stained with hematoxylin-eosin for optical microscopic analysis of the apical and periapical repair. The groups filled with Sealapex and AH Plus had better histological repair (p < 0.05) than the group filled with Sealer Plus, that had unsatisfactory results.

Effect of silica coating on flexural strength of fiber posts

Purpose: Fiber-reinforced composite (FRC) posts can be air-abraded to obtain good attachment to the resin cement. This study tested the effect of silica coating on the flexural strength of carbon, opaque, and translucent quartz FRC posts. Materials and Methods: Six experimental groups of FRC posts (n = 10 per group) were tested, either as received from the manufacturer or after chairside silica coating (30-μm CoJet-Sand). Results: There was no significant difference in the flexural strength of nonconditioned (504 to 525 MPa) and silica-coated (514 to 565 MPa) specimens (P > .05) (analysis of variance). The type of post did have a significant effect on flexural strength (P < .05). Conclusion: Chairside silica coating did not affect the flexural strength of both carbon and quartz FRC posts.

Relationships between the curing conditions and some mechanical properties of hybrid thermosetting materials

The relationship between the heat of polymerization (ΔH) and activation energy (Ea) parameters, obtained by differential scanning calorimetry (DSC) and the ratio of epoxy resin to hardener of the thermosetting materials based on an organic-inorganic hybrid epoxy resin (OG) was investigated. Activation energy (Ea) and heat of polymerization (ΔH) increased with an increasing OG content, up to 70 wt%. Further increase in OG content to 80wt% reduced Ea and ΔH. Dynamic mechanical analysis indicates that the maximum cross-link density is obtained at 83 wt% OG, whereas fracture toughness and tensile modulus mechanical properties are maximized at 70 wt% OG. ©2006 Sociedade Brasileira de Química.