Dielectric thermal analysis as a tool for quantitative-evaluation of the viscosity and the kinetics of epoxy resin cure

Dielectric thermal analysis has been proved as a valuable tool for monitoring the epoxy curing process and the related rheological properties in the fabrication of polymer-matrix composite materials. This technique also has the potential to be applied in the monitoring of magnet impregnation processes as well as in quality control. In this work we present the quantitative evaluation of the viscosity changing and the curing kinetics for a commercial Stycast epoxy resin system at different temperatures through the impedance analysis. The results showed correlation between the real component of the complex impedance and the isothermal reaction extent. Comparing the dielectric analysis result with the viscosity measured by rotational rheometer we observed a similar behavior reported for dynamic mechanic analysis. The results comparison have shown that the kinetics parameters obtained from DSC and DETA analysis showed different sensitivities related to the characteristics of curing stages. We concluded that the dielectric thermal analysis should be applied in quantitative evaluation of cure kinetics.

Epoxy Composite with Milimetric Carbon Nanotubes

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

Characterization of cure of carbon/epoxy prepreg used in aerospace field

Carbon/epoxy 8552 prepreg is a thermoplastic toughened high-performance epoxy being used in the manufacture of advanced army material. Understanding the cure behavior of a thermosetting system is essential in the development and optimization of composite fabrication processes. The cure kinetics and rheological behavior were evaluated using a differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA) and a rheometer. Values of the kinetic parameters were obtained from dynamic DSC scans using an nth order reaction model. Rheological measurements as a function of temperature and time were made for the prepreg system. The manufacturer's recommended cure cycle was evaluated and considered adequate to consolidated the studied system.

Leaf-cutting ants toxicity of limonexic acid and degraded limonoids from Raulinoa echinata. X-ray structure of epoxy-fraxinellone

Phytochemical survey of roots extracts of the South Brazilian endemic plant Raulinoa echinata Cowan, Rutaceae led to the isolation of known degraded limonoids: fraxinellone, fraxinellonone and epoxy-fraxinellone. The latter was previously isolated also from the stems, but the relative configuration could not be solved by NMR experiments. This paper deals with the X-ray diffraction analysis of epoxy-fraxinellone and its toxicity to leaf-cutting ants, describes the isolation of fraxinellonone and fraxinellone for the first time in Raulinoa. Epoxy-fraxinellone showed no toxicity to the leaf-cutting ants (Atta sexdens rubropilosa). The limonoid limonexic acid, isolated from stems, presented high toxicity to the leaf-cutting ants, diminishing considerably their longevity. ©2005 Sociedade Brasileira de Química.

Relationship between the dielectric and mechanical properties and the ratio of epoxy resin to hardener of the hybrid thermosetting polymers

The relationship between the dielectric properties (dielectric constant, ε′, and loss factor, ε; activation energy, E a) and the ratio of epoxy resin (OG) to hardener of the epoxy resin thermosetting polymers was investigated. The amplitude of the ε″ peak decreases with increasing OG content until about 73 wt.% and slightly increases at higher OG content. The temperature of the position of the ε″ peak increases with the increasing of OG content, reaching maximum values for compositions in the range of 67 and 73 wt.%, and then it decreases sharply at higher OG content. The activation energy obtained from dielectric relaxation increased with increasing wt.% OG up to around 70 wt.%. Further increase in concentration of OG up to 83 wt.% reduced E a. The curves of tensile modulus and fracture toughness mechanical properties as a function of OG content presented a similar behavior. ©2006 Sociedade Brasileira de Química.

A review on the development and properties of continuous fiber/epoxy/aluminum hybrid composites for aircraft structures

Weight reduction and improved damage tolerance characteristics were the prime drivers to develop new family of materials for the aerospace/ aeronautical industry. Aiming this objective, a new lightweight Fiber/ Metal Laminate (FML) has been developed. The combination of metal and polymer composite laminates can create a synergistic effect on many properties. The mechanical properties of FML shows improvements over the properties of both aluminum alloys and composite materials individually. Due to their excellent properties, FML are being used as fuselage skin structures of the next generation commercial aircrafts. One of the advantages of FML when compared with conventional carbon fiber/epoxy composites is the low moisture absorption. The moisture absorption in FML composites is slower when compared with polymer composites, even under the relatively harsh conditions, due to the barrier of the aluminum outer layers. Due to this favorable atmosphere, recently big companies such as EMBRAER, Aerospatiale, Boing, Airbus, and so one, starting to work with this kind of materials as an alternative to save money and to guarantee the security of their aircrafts.

Damping behavior of hygrothermally conditioned carbon fiber/epoxy laminates

Carbon fiber reinforced polymer composites have been used in wide variety of applications including, aerospace, marine, sporting equipment as well as in the defense sector due to their outstanding properties at low density. In many of their applications, moisture absorption takes place which may result in a reduction in mechanical properties even at lower temperature service. In this work, the viscoelastic properties, such as storage modulus (E′) and loss modulus (E″), were obtained through vibration damping tests for three carbon fiber/epoxy composite families up to the saturation point (6 weeks). Three carbon fiber/epoxy composites having [0/0] s, [0/90] s, and [±45] s orientations were studied. During vibration tests the storage modulus (E′) and loss modulus (E″) were monitored as a function of moisture uptake, and it was observed that the natural frequencies and E′ values decreased with the increase during hygrothermal conditioning due to the matrix plasticization. © 2007 Wiley Periodicals, Inc.

Fatigue behaviour study on repaired aramid fiber/epoxy composites

Aramid fiber reinforced polymer composites have been used in a wide variety of applications, such as aerospace, marine, sporting equipment and in the defense sector, due to their outstanding properties at low density. The most widely adopted procedure to investigate the repair of composites has been by repairing damages simulated in composite specimens. This work presents the structural repair influence on tensile and fatigue properties of a typical aramid fiber/epoxy composite used in the aerospace industry. According to this work, the aramid/epoxy composites with and without repair present tensile strength values of 618 and 680MPa, respectively, and tensile modulus of 26.5 and 30.1 GPa, respectively. Therefore, the fatigue results show that in loads higher than 170 MPa, both composites present a low life cycle (lower than 200,000 cycles) and the repaired aramid/epoxy composite presented low fatigue resistance in low and high cycle when compared with non-repaired composite. With these results, it is possible to observe a decrease of the measured mechanical properties of the repaired composites.

Persistence of epoxy-based sealer residues in dentin treated with different chemical removal protocols

The presence of residual endodontic sealer in the pulp chamber may cause discoloration of the dental crown and interfere with the adhesion of restorative materials. The aim of this study was to compare the efficacy of different solvents in removing residues of an epoxy resin-based sealer (AH Plus) from the dentin walls of the pulp chamber, by scanning electron microscopy (SEM). Forty-four bovine incisor dental crown fragments were treated with 17% EDTA and 2.5% NaOCl. Specimens received a coating of AH Plus and were left undisturbed for 5 min. Then, specimens were divided in four groups (n = 10) and cleaned with one of the following solutions: isopropyl alcohol, 95% ethanol, acetone solution, or amyl acetate solution. Negative controls (n = 2) did not receive AH Plus, while in positive controls (n = 2) the sealer was not removed. AH Plus removal was evaluated by SEM, and a score system was applied. Data were analyzed by Kruskal-Wallis and Dunn tests. None of the solutions tested was able to completely remove AH Plus from the dentin of the pulp chamber. Amyl acetate performed better than 95% ethanol and isopropyl alcohol (p < 0.05), but not better than acetone (p > 0.05) in removing the sealer from dentin. No significant differences were observed between acetone, 95% ethanol, and isopropyl alcohol (p > 0.05). It was concluded that amyl acetate and acetone may be good options for cleaning the pulp chamber after obturation with AH Plus. SCANNING 35:17-21, 2013. © 2012 Wiley Periodicals, Inc. © Wiley Periodicals, Inc.

Dielectric behavior of epoxy/BaTiO3 composites using nanostructured ceramic fibers obtained by electrospinning

Composite materials made of epoxy resin and barium titanate (BT) electrospun nanostructured fibers were prepared. BT fibers were synthesized from a sol based on barium acetate, titanium isopropoxide, and poly(vinyl pyrrolidone). The fibers were heat-treated at different temperatures and characterized by X-ray diffraction, scanning electron microscopy (SEM), and Raman spectroscopy. Mats of BT fibers heat-treated at 800 C were embedded in epoxy resin into suitable molds. The composites were characterized by SEM, and dielectric measurements were performed by means of dielectric spectroscopy. The dielectric permittivity and dielectric modulus of epoxy resin/BT-fiber composites were measured for two types of samples: with the electrodes parallel and perpendicular to the BT fiber layers. Interestingly, composite samples with electrodes perpendicular to the fiber layers and a BT content as low as 2 vol % led to dielectric permittivities three times higher than that of pure epoxy resin. © 2013 American Chemical Society.

Effect of the root canal final rinse protocols on the debris and smear layer removal and on the push-out strength of an epoxy-based sealer

The aim of the present study was to evaluate the efficacy of QMiX, SmearClear, and 17% EDTA for the debris and smear layer removal from the root canal and its effects on the push-out bond strength of an epoxy-based sealer by scanning electron microscopy (SEM). Forty extracted human canines (n=10) were assigned to the following final rinse protocols: G1-distilled water (control), G2-17% EDTA, G3-SmearClear, and G4-QMiX. The specimens were submitted to a SEM analysis to evaluate the presence of debris and smear layer, respectively, in the apical or cervical segments. In sequence, forty extracted human maxillary canines with the root canals instrumented were divided into four groups (n=10) similar to the SEM analysis study. After the filling with AH Plus, the roots were transversally sectioned to obtain dentinal slices. The specimens were submitted to a push-out bond strength test using an electromechanical testing machine. The statistical analysis for the SEM and push-out bond strength studies were performed using the Kruskal-Wallis and Dunn tests (α=5%). There was no difference among the G2, G3, and G4 efficacy in removing the debris and smear layer (P>0.05). The efficacy of these groups was superior to the control group. The push-out bond strength values of G2, G3, and G4 were superior to the control group. The ability to remove the debris and smear layer by SmearClear and QMiX was as effective as the 17% EDTA. The final rinse with these solutions promoted similar push-out bond strength values. © 2013 Wiley Periodicals, Inc.

Effect of fiber surface on flexural strength in carbon fabric reinforced epoxy composites

The effect of carbon fiber surface characteristics on flexural properties of structural composites is studied in this work. Two types of intermediate modulus carbon fibers were used: T800HB and IM7. Results revealed that higher mechanical properties are linked with higher interfacial adhesion. Morphologies and chemical compositions of commercial carbon fibers (CF) were characterized by Fourier Transformed Infra Red (FTIR) and Scanning Electronic Microscopy (SEM). Comparing the results, the T800HB apparently has more roughness, since the IM7 seems to be recovered for a polymeric film. On other hand, the IM7 one shows higher interactivity with epoxy resin system Cycom 890 RTM. Composites produced with Resin Transfer Molding (RTM) were tested on a flexural trial. Interfacial adhesion difference was showed with SEM and Dynamic Mechanical Analyses (DMA), justifying the higher flexural behavior of composites made with IM7 fibers. © 2013 Elsevier B.V. All rights reserved.

Experimental RTM manufacturing analysis of carbon/epoxy composites for aerospace application

The success of manufacturing composite parts by liquid composite molding processes with RTM depends on tool designs, efficient heat system, a controlled injection pressure, a stabilized vacuum system, besides of a suitable study of the preform lay-up and the resin system choice. This paper reports how to assemble a RTM system in a laboratory scale by specifying heat, injection and vacuum system. The design and mold material were outlined by pointing out its advantages and disadvantages. Four different carbon fiber fabrics were used for testing the RTM system. The injection pressure was analyzed regarding fiber volume content, preform compression and permeability, showing how these factors can affect the process parameters. The glass transition temperature (Tg) around 203 ºC matched with the aimed temperature of the mold which ensured good distribution of the heat throughout the upper and lower mold length. The void volume fraction in a range of 2% confirmed the appropriate RTM system and parameters choice.

The impact of the addition of iodoform on the physicochemical properties of an epoxy-based endodontic sealer

Due to the low radiopacity of Sealer 26, iodoform is frequently empirically added to this sealer. Thus, the interference of this procedure with the physicochemical properties of Sealer 26 must be evaluated. Objective: This study evaluated the influence of the addition of iodoform on setting time, flow, solubility, pH, and calcium release of an epoxy-based sealer. Material and Methods: The control group was pure Sealer 26, and the experimental groups were Sealer 26 added with 1.1 g, 0.55 g or 0.275 g of iodoform. Setting time evaluation was performed in accordance with the ASTM C266-03 speciflcation. The analysis of flow and solubility was in accordance with the ISO 6876-2001 speciflcation. For the evaluation of pH and calcium ion release, polyethylene tubes were filled with the materials and immersed in flasks with 10 ml of deionized water. After 24 h, 7, 14, 21, 28, and 45 days pH was measured. In 45 days, the calcium released was evaluated with an atomic absorption spectrophotometer. Results: The addition of iodoform increased setting time in comparison with pure sealer (P < 0.05). As for flow, solubility, and calcium release, the mixtures presented results similar to pure sealer (p > 0.05). In the 24 h period, the mixture with 1.1 g and 0.55 g of iodoform showed lower pH than pure sealer and than sealer added with 0.275 g of iodoform (P < 0.05). Conclusions: The iodoform added to Sealer 26 interferes with its setting time and solubility properties. Further studies are needed to address the clinical signiflcance of this interference.

Nanostructured Composites Based on Carbon Nanotubes and Epoxy Resin for Use as Radar Absorbing Materials

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)