Processing and characterization of ablative composites used in rocket motors

The main objective of this research work was to obtain two formulations of ablative composites. These composites are also known as ablative structural composites, for applications in atmospherically severe conditions according to the high-temperature, hot gaseous products flow generated from the burning of solid propellants. The formulations were manufactured with phenolic resin reinforced with chopped carbon fiber. The composites were obtained by the hot compression molding technique. Another purpose of this work was to conduct the physical and chemical characterization of the matrix, the reinforcements and the composites. After the characterization, a nozzle divergent of each formulation was manufactured and its performance was evaluated through the rocket motor static firing test. According to the results found in this work, it was possible to observe through the characterization of the raw materials that phenolic resins showed peculiarities in their properties that differentiate one from the other, but did not exhibit significant differences in performance as a composite material for use in ablation conditions. Both composites showed good performance for use in thermal protection, confirmed by firing static tests (rocket motor). Composites made with phenolic resin and chopped carbon fiber showed that it is a material with excellent resistance to ablation process. This composite can be used to produce nozzle parts with complex geometry or shapes and low manufacturing cost.

Bacterial cellulose-hydroxyapatite composites with osteogenic growth peptide (OGP) or pentapeptide OGP on bone regeneration in critical-size calvarial defect model

This study aimed to evaluate the potential of bacterial cellulose-hydroxyapatite (BC-HA) composites associated with osteogenic growth peptide (OGP) or pentapeptide OGP(10–14) in bone regeneration in critical-size calvarial defects in mice. In this study, the BC-HA, BC-HA-OGP, and BC-HA-OGP(10–14) membranes were analyzed at 3, 7, 15, 30, 60, and 90 days. In each period, the specimens were evaluated by micro-computed tomography (µCT), descriptive histology, gene expression of bone biomarkers by qPCR and VEGFR-2 (vascular endothelial growth factor) quantification by ELISA. Three days post-operative, Runx2, Tnfrsf11b and Bglap bone biomarkers were upregulated mainly by BC-HA OGP and BC-HA OGP(10–14) membranes, suggesting an acceleration of the osteoblast differentiation/activity with the use of these biomaterials. At 60 and 90 days, a high percentage of bone formation was observed by µCT for BC-HA and BC-HA OGP(10–14) membranes. High expression of some bone biomarkers, such as Alpl, Spp1, and Tnfrsf11b, was also observed for the same membranes on days 60 and 90. In conclusion, the BC-HA membrane promoted a better bone formation in critical-size mice calvarial defects. Nevertheless, incorporation of the peptides at the concentration of 10−9 mol L−1 did not improve bone regeneration potential in the long-term.

Mucoadhesive Amphiphilic Methacrylic Copolymer-Functionalized Poly(epsilon-caprolactone) Nanocapsules for Nose-to-Brain Delivery of Olanzapine

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Monitoring the process of densification of 3D and 4D (tridirectional and tetradirectional) carbon/carbon composites

Carbon fiber reinforced carbon composites can be made by iterative liquid impregnation or gas phase carbon deposition routes. In both cases, at the final processing stage the carbon fiber is embedded in carbon matrix which results in unique properties such as low density, high thermal conductivity and thermal shock resistance, low thermal expansion and high modulus, in relation to other refractory materials. In the present study assembled three-directional and four-directional preforms, having 50% volume of pores, were densified by iterative cycles of thermoset resin impregnation followed by pyrolysis under inert atmosphere, until appropriate densities were achieved. The thermoset resin is converted in a carbon matrix during pyrolysis. The iterative manufacturing process of the carbon fiber reinforced carbon composites is evaluated by means of nondestructive techniques based on X-ray computed tomography and electrical resistivity. X-ray computed tomography gives a general mapping view of the filling pores of the preforms which impacts results of the electrical resistivity. After six processing cycles and heat treatments up to 2000?, the final densities of the three-directional and four-directional carbon fiber reinforced carbon composites were 1.16g/cm(3) and an electrical resistivity of approximate to 0.07m. The configuration of preforms, three-directional or four-directional, did not alter the densification profile, in terms of increasing density and reducing porosity during the processing cycles.

Estudo da cinética de decomposição de compósitos nanoestruturados de poli (sulfeto de fenileno) reforçados com nanotubos de carbono

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

Non ohmic gigahertz conductivity in pressed pellets of ClO4 doped poly(3-methylthiophene)

ESR measurements In pressed pellets of doped Poly(3-Methylthiophene)(P3MT) were performed at 10 K and 50 K after cooling the system slowly from room temperature to 110 K, quenching to 77 K and then to 10 K. ESR line asymmetry (A/B) as a function of microwave power was observed and 9.4 GHz conductivity was obtained from Dyson's theory. The data is discussed in terms of Charge-Density Wave (CDW) depinning. At 50 K the threshold electric field is estimated to be less than 1 V/cm. At 10 K a subtle pinning of the CDW was observed around 15 mW.

Effects of age condition on the distribution and integrity of inorganic fillers in dental resin composites

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Nanostructured TiO2-based composites for light absorption

Metal oxide nanocomposites were prepared by two different routes: polyol and sol-gel. Characterization by X ray diffraction showed that the first process produces directly a two-phase material, while the sol-gel powder never showed second phase below 600°C. Light spectroscopy of the treated powders indicated similarities for the processed materials. Although the overall material compositions are about the same, different structural characteristics are found for each processing. With the exception of Ti-Zn materials, all the double metal oxide powders showed higher absorbance than either TiO2 powder.

Tribocorrosion behaviour of hot pressed CoCrMo−Al2O3 composites for biomedical applications

Alumina/alumina wear couple can lower the wear rates and thus metallic ion releasing on load bearing metallic implant materials. However, the low fracture toughness of ceramics is still a major concern. Therefore, the present study aims to process and to triboelectrochemically characterise the 5 and 10 vol.-%Al2O3 reinforced CoCrMo matrix composites. Corrosion and tribocorrosion behaviour of the composites were investigated in 8 g L−1 NaCl solution at body temperature. Corroded and worn surfaces were investigated by a field emission gun scanning electron microscope equipped with energy dispersive X-ray spectroscopy. After tribocorrosion experiments, wear rates were calculated using a profilometer. Results suggest that Al2O3 particle addition decreased the tendency of CoCrMo alloy to corrosion under both static and tribocorrosion conditions. However, no significant influence on the corrosion and wear rates was observed in composites mainly due to increased porosity and insufficient matrix/reinforcement bonding.

Polymer Light Emitting Diode Using PFT-Poly(9,9 `-n-dihexil-2,7-fluorenodiilvinylene-alt-2,5thiophene)

The development of new electroluminescence polymers for specific colour tuning in Polymer Light Emitting Devices (PLEDs) is currently one of the most important fields for organic electronics. This work reports a synthesis of a new electroluminescent polymer and the concomitant test as PLED emissive layer. The polymer, synthesised from fluorene, is poly(9,9`-n-dihexil-2,7-fluorenodiilvinylene-alt-2,5thiophene) or PFT The luminescence shows large bands with maxima around 480 nm in absorption and 560 nm in emission. The device was made in a three layer structure, with PEDOT:PSS as hole transport layer, PFT as emissive layer and butyl-PBD as electron transport layer. The electroluminescence spectrum shows a strong band peaked at 540 nm. For an applied voltage of 12 Volt, the brightness at normal angle of viewing is near 10 cd/m(2) and the luminous efficiency is of 0.01 lm/W. A discussion about carrier transport and the electroluminescence properties is made.

Production and characterization of poly-(3-hydroxybutyrate) from recombinant Escherichia coli grown on cheap renewable carbon substrates

Although the biopolymer poly-(3-hydroxybutyrate), P[3HB], presents physicochemical properties that make it an alternative material to conventional plastics, its biotechnological production is quite expensive. As carbon substrates contribute greatly to P[3HB] production cost, the utilization of a cheaper carbon substrate and less demanding micro-organisms should decrease its cost. In the present study a 23 factorial experimental design was applied, aiming to evaluate the effects of using hydrolysed corn starch (HCS) and soybean oil (SBO) as carbon substrates, and cheese whey (CW) supplementation in the mineral medium (MM) on the responses, cell dried weigh (DCW), percentage P[3HB] and mass P[3HB] by recombinant Escherichia coli strains JM101 and DH10B, containing the P[3HB] synthase genes from Cupriavidus necator (ex-Ralstonia eutropha). The analysis of effects indicated that the substrates and the supplement and their interactions had positive effect on CDW. Statistically generated equations showed that, at the highest concentrations of HCS, SO and CW, theoretically it should be possible to produce about 2 g L(1) DCW, accumulating 50% P[3HB], in both strains. To complement this study, the strain that presented the best results was cultivated in MM added to HCS, SBO and CW ( in best composition observed) and complex medium (CM) to compare the obtained P[3HB] in terms of physicochemical parameters. The obtained results showed that the P[3HB] production in MM (1.29 g L(-1)) was approximately 20% lower than in CM (1.63 g L(-1)); however, this difference can be compensated by the lower cost of the MM achieved by the use of cheap renewable carbon sources. Moreover, using differential scanning calorimetry and thermogravimetry analyses, it was observed that the polymer produced in MM was the one which presented physicochemical properties (Tg and Tf) that were more similar to those found in the literature for P[3HB].

A comparative study between crack analysis and a mechanical test for assessing the polymerization stress of restorative composites

Objectives. To verify the hypothesis that crack analysis and a mechanical test would rank a series of composites in a similar order with respect to polymerization stress. Also, both tests would show similar relationships between stress and composite elastic modulus and/or shrinkage. Methods. Soda-lime glass discs (2-mm thick) with a central perforation (3.5-mm diameter) received four Vickers indentations 500 mu m from the cavity margin. The indent cracks were measured (500x) prior and 10 min after the cavity was restored with one of six materials (Kalore/KL, Gradia/GR, Ice/IC, Wave/WV, Majesty Flow/MF, and Majesty Posterior/MP). Stresses at the indent site were calculated based on glass fracture toughness and increase in crack length. Stress at the bonded interface was calculated using the equation for an internally pressurized cylinder. The mechanical test used a universal testing machine and glass rods (5-mm diameter) as substrate. An extensometer monitored specimen height (2 mm). Nominal stress was calculated dividing the maximum shrinkage force by the specimen cross-sectional area. Composite elastic modulus was determined by nanoindentation and post-gel shrinkage was measured using strain gages. Data were subjected to one-way ANOVA/Tukey or Kruskal-Wallis/Mann-Whitney tests (alpha: 5%). Results. Both tests grouped the composites in three statistical subsets, with small differences in overlapping between the intermediate subset (MF, WV) and the highest (MP, IC) or the lowest stress materials (KL, GR). Higher stresses were developed by composites with high modulus and/or high shrinkage. Significance. Crack analysis demonstrated to be as effective as the mechanical test to rank composites regarding polymerization stress. (c) 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Preparation and characterization of poly(vinyl butyral)-polyaniline-montmorillonite nanocomposites

Poly(vinyl butyral)-polyaniline-sodium montmorillonite nanocomposites were prepared via polymerization of aniline between clay mineral platelets at two different pH levels (2.0 and 5.0), followed by dispersion of the polyaniline-sodium montmorillonite nanocomposite in a poly(vinyl butyral) solution. A comparison was made of the effect of the pH levels and the polyaniline-sodium montmorillonite nanocomposite precursor on the final structures of the poly(vinyl butyral) nanocomposites and their electrical conductivities. X-ray diffraction patterns revealed the formation of nanocomposites at both pH levels. UV-Vis spectra indicated that the polyaniline formed at both pH levels was conductive, with the UV-Vis spectra presenting a band at 420 nm corresponding to the polaronic form and the beginning of a new band at 600 nm indicating the presence of polaronic segments. FTIR spectra revealed the peaks of the groups present in polyaniline and poly(vinyl butyral) nanocomposites. The electrical conductivities of the polyaniline and poly(vinyl butyral) nanocomposites prepared at pH 2.0 were lower than those of the same nanocomposites prepared at pH 5.0, probably due to the lower formation of polyaniline chains in a more acidic dispersion and to the final configuration of polyaniline in the nanocomposites.

In vitro and in vivo evaluation of the biocompatibility of a calcium phosphate/poly(lactic-co-glycolic acid) composite

This study assess the effects of bioceramic and poly(lactic-co-glycolic acid) composite (BCP/PLGA) on the viability of cultured macrophages and human dental pulp fibroblasts, and we sought to elucidate the temporal profile of the reaction of pulp capping with a composite of bioceramic of calcium phosphate and biodegradable polymer in the progression of delayed dentine bridge after (30 and 60 days) in vivo. Histological evaluation of inflammatory infiltrate and dentin bridge formation were performed after 30 and 60 days. There was similar progressive fibroblast growth in all groups and the macrophages showed viability. The in vivo study showed that of the three experimental groups: BCP/PLGA composite, BCP and calcium hydroxide (Ca(OH)(2)) dentin bridging was the most prevalent (90 %) in the BCP/PLGA composite after 30 days, mild to moderate inflammatory response was present throughout the pulp after 30 days. After 60 days was observed dentine bridging in 60 % and necrosis in 40 %, in both groups. The results indicate that understanding BCP/PLGA composite is biocompatible and by the best tissue response as compared to calcium hydroxide in direct pulp capping may be important in the mechanism of delayed dentine bridge after 30 and 60 days.

Is the poly (methylene blue)-modified glassy carbon electrode an adequate electrode for the simple detection of thiols and amino acid-based molecules?

This paper describes the preparation, characterization, and use of poly (methylene blue) (PMB)-modified glassy carbon electrodes (GCE) (GCE-PMB) in the detection of the thiols L-cysteine (L-CySH) and N-acetyl cysteine (Acy), and the herbicide glyphosate (GLYP) in pH 5.3 aqueous solution. The polymer film prepared by electropolymerization showed different characteristics such as robustness, stability, and redox properties satisfactorily. The surface coverage concentration (Gamma) of PMB was found to be 7.90 x 10(-9) - mol cm(-2). Moreover, we observed strong adhesion of the polymer film to the electrode surface. The results using GCE-PMB as a sensor indicated that this modified electrode exhibited electrocatalytic activity toward the detection of thiols and glyphosate in 0.1 mol L-1 KO (pH 5.3). Meanwhile, strong adsorption of the analytes on the GCE-PMB electrodes was also observed. Otherwise, using a low concentration (1 x 10(-4) mol L-1) of L-cysteine and N-acetyl cysteine and 8.9 x 10(-6) mol L-1 of glyphosate, separately, it was possible to observe a well-defined electrochemical response, thus providing an opportunity to further understand the applicability of PMB as a sensor for amino acid-based molecules. (C) 2012 Elsevier B.V. All rights reserved.