Scielo RSS <![CDATA[Materials Research]]> http://www.scielo.br/rss.php?pid=1516-143920140007&lang=en vol. 17 num. lang. en <![CDATA[SciELO Logo]]> http://www.scielo.br/img/en/fbpelogp.gif http://www.scielo.br <![CDATA[<b>Materials Research - Ibero-american Journal of Materials</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700001&lng=en&nrm=iso&tlng=en <![CDATA[<b>Effects of acid treatment on the clay palygorskite</b>: <b>XRD, surface area, morphological and chemical composition</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700002&lng=en&nrm=iso&tlng=en The palygorskite is an aluminum-magnesium silicate that has a fibrous morphology. Their physico-chemical characteristics are the result of high surface area, porosity and thermal resistance which make it an attractive adsorbent. Its adsorption capacity can be increased through chemical reactions and/or heat treatments. The objective of this work is to verify the effects of acid activation on the palygorskite, treated with HCl at 90 ºC at concentrations of 2, 4 and 6 mol L-1 in 2 and 4 hours, with clay/acid solution ratio 1 g 10 mL-1 and characterized by techniques: XRF, XRD and surface area. A significant increase in specific surface area was observed in the sample treated with HCl at the concentration 6 mol L-1. The changes were more pronounced at stricter concentrations of acidity, with decreasing intensity of reflection of the clay indicated in the XRD. These changes were confirmed in the XRF with the leaching of some oxides and with increasing concentration of SiO2. <![CDATA[<b>Synthesis of Co-Al-Cl LDH by cathodic material reprocessing from cellular phone batteries</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700003&lng=en&nrm=iso&tlng=en The aim of this paper was the recovering of the cathodic material from discarded lithium ion batteries for obtainment of the lamellar double hydroxides (LDHs) by the co-precipitation method at variable pH in HCl and H2O2 1:1 (v/v) acid solution containing Co and Al (extracted from cathodic material composed of LiCoO2 and aluminum foil). These metals were precipitated in LiOH at pH 9 or 11, or NH4OH at pH 9 and submitted to the hydrothermal treatment (HT) to improve the structural organization of the LDHs lamellae. After precipitation, the resulting solids were structurally characterized by XRD for phase identification and calculation of the unit cell parameter, thermally by TGA for the identification of the mass loss and morphologically by SEM. The sample obtained by precipitation with LiOH at pH 11 / hydrothermal treatment showed diffraction peaks similar to hydrotalcite, morphological and thermal characteristics similar to the pattern Co-Al-Cl LDH obtained by co-precipitation at constant pH 8. <![CDATA[<b>Polymorphism of CaCO<sub>3 </sub>and microstructure of the shell of a Brazilian invasive mollusc (<i>Limnoperna fortunei</i>)</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700004&lng=en&nrm=iso&tlng=en Applying the theories of Materials Science and Engineering to describe the composition and hierarchy of microstructures that comprise biological systems could help the search for new materials and results in a deeper insight into evolutionary processes. The layered microstructure that makes up the freshwater bivalve Limnoperna fortunei shell, an invasive specie in Brazil, was investigated utilizing SEM and AFM for the determination of the morphology and organization of the layers; and XRD was used to determine the crystalline phases of the calcium carbonate (CaCO3) present in the shell. The presence of the polymorphs calcite and aragonite were confirmed and the calcite is present only on the external side of the shell. The shell of L. fortunei is composed of two layers of aragonite with distinct microstructures (the aragonite prismatic layer and the aragonite sheet nacreous layer) and the periostracum (a protein layer that covers and protects the ceramic part of the shell). A new morphology of the calcite layer was found, below the periostracum, without defined form, albeit crystalline. <![CDATA[<b>Color and shade parameters of ultramarine zeolitic pigments synthesized from kaolin waste</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700005&lng=en&nrm=iso&tlng=en Ultramarine pigments were successful synthesized from zeolite A obtained from kaolin waste. This waste has been used as an excellent source of silicon and aluminum for zeolite synthesis because of its high kaolinite concentrations and low contents of other accessory minerals. The cost is naturally less than the industrialized product. Color additives (Sulfur and Sodium Carbonate) were mixed with different proportions of zeolite A and further calcined for 5 h at 500 °C. They were characterized by XRD and XRF in addition to visual classification by color and shade. These products show colors from blue to green at different shades, both influenced by the amount of additives and cooling rate after calcination. Thus, a different quantity of the same additives in the same zeolitic matrix provides an increase in the color intensity. Cooling rate after calcination induces the color change which is substantially important in the pigments production. <![CDATA[<b>Development and test of a small resistive fault current limiting device based on Hg, Re-1223 and Sm-123 ceramics</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700006&lng=en&nrm=iso&tlng=en Several reports describing Superconducting Fault Current Limiter (SFCL) containing members of the bismuth or yttrium ceramics were already described. However, none of these included the mercury and samarium cuprates. Consequently, we have conducted a study of a resistive-type superconductor fault current limiter based on Hg0.82Re0.18Ba2Ca2Cu3O8+d samples and SmBa2Cu3O7-d ceramics. All polycrystalline samples were prepared by solid-state reaction method using commercial oxide and carbonate powders. The superconducting ceramic with 2.4 × 2.6 × 6.0 mm³ dimensions was set up such that the electrical current flew through the area of 2.6 × 6.0 mm². All measurements were done at 77K and without applied magnetic field (Happ = 0). In the case mercury sample, the fault current of 16.1 Apeak was reduced to 8.1 Apeak by the superconducting element and sustained for 100 ms. The prospective/limited of current ratio observed in this experiment was ~ 2.0, as considered a 2.4 mm pellet thickness. When the test was realized with the samarium sample, the prospective/limited current ratio observed was approximately 1.2, for same ceramic thickness. The tests confirmed the capability of the resistive type SFCL to limit the fault current. These results open the possibility of future investigations into SFCL devices based on those superconducting ceramics in low power electronics and electrical motor. <![CDATA[<b>Scaffolds of PDLLA/bioglass 58S produced via selective laser sintering</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700007&lng=en&nrm=iso&tlng=en Scaffolds of PDLLA were produced to be implemented in maxilofacial surgeries inducing bone repair and regeneration. To prepare these scaffolds, bioglass (BG58S) was synthesized by sol-gel method, in order to be applied as osteoconductive dispersed particles in PDLLA matrix. Once presenting greater facility on parts fabrication, this polymeric matrix enables complex geometries production besides presenting compatible degradation rate for scaffold absorption and bone regeneration. Scaffolds production was performed by selective laser sintering in order to obtain tailored-made parts. FTIR and XRD analyses were carried out to observe the composition and evaluate the presence of crystalized phases in bioglass, obtaining Wollastonite. SEM was used to observe the BG particle distribution in PDLLA matrix and flexural test was performed to evaluate the composite mechanical properties. Results showed that was possible to obtain pieces using SLS method and with addition of 10%wt BG to polymeric matrix, flexural modulus and strength increased regarding to pure polymer. <![CDATA[<b>The production of hydroxyapatite prototypes from solid bodies of gypsum/polyvinyl alcohol composites</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700008&lng=en&nrm=iso&tlng=en Prototypes of porous hydroxyapatite (HAp) were produced from Gypsum/PVA composite, using a mass proportion of 15% polymer. The material was obtained by means of chemical conversion in (NH4)2HPO4 0.5 mol.L-1 solution and NH4OH 6.0 mol.L-1 alkaline medium for pH control, maintained between 6.0 and 9.0. The reaction occurred at a temperature of 100ºC at different test times. The obtained HAp was characterized by several techniques, such as FTIR, which identified the SO4(2-) groups characteristic for the Gypsum block, and the PO4(3-) groups that are attributed to the biomaterial HAp, besides XRD and SEM, which made it possible to confirm a successful conversion of the material. Tests for mechanical resistance to compression (σc) were carried out for both materials as well. <![CDATA[<b>Increasing the compressive strength of Portland cement concrete using flat glass powder</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700009&lng=en&nrm=iso&tlng=en This paper analyzes the compressive strength of Portland cement concrete in response to the incorporation of 5%, 10% and 20% of flat glass powder in place of sand, at w/c (water/cement) ratios of 0.50, 0.55 and 0.58. A statistical analysis of variance (ANOVA) was performed after 7, 14 and 28 days of curing. The compressive strength test results indicate that the concrete containing a w/c ratio of 0.50 can be used for structural applications, regardless of the waste glass content, as can that with a w/c ratio of 0.55 containing 20% of waste glass. We suggest that the use of flat glass powder in place of sand in the abovementioned percentages is feasible for the production of an environmentally appropriate and structurally applicable concrete. However, the concrete's fluidity and void content must be taken into account. <![CDATA[<b>Influence of granitic aggregates from northeast Brazil on the alkali-aggregate reaction</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700010&lng=en&nrm=iso&tlng=en The alkali-aggregate reaction (AAR) in concrete structures is a problem that has concerned engineers and researchers for decades. This reaction occurs when silicates in the aggregates react with the alkalis, forming an expanded gel that can cause cracks in the concrete and reduce its lifespan. The aim of this study was to characterize three coarse granitic aggregates employed in concrete production in northeastern Brazil, correlating petrographic analysis with the kinetics of silica dissolution and the evolution of expansions in mortar bars, assisted by SEM/EDS, XRD, and EDX. The presence of grains showing recrystallization into individual microcrystalline quartz subgrains was associated with faster dissolution of silica and greater expansion in mortar bars. Aggregates showing substantial deformation, such as stretched grains of quartz with strong undulatory extinction, experienced slower dissolution, with reaction and expansion occurring over longer periods that could not be detected using accelerated tests with mortar bars. <![CDATA[<b>Electrical, mechanical, and thermal analysis of natural rubber/polyaniline-Dbsa composite</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700011&lng=en&nrm=iso&tlng=en A composite of natural rubber (NR) with polyaniline (PANI) was obtained by mixing an aqueous dispersion of dodecylbenzenesulfonic acid (DBSA)-doped PANI with NR latex in different concentrations. Films were obtained by the casting method and characterized by ultraviolet visible near-infrared (UV-Vis-NIR) spectroscopy, thermogravimetry/differential thermogravimetry (TG/DTG), stress-strain testing, differential scanning calorimetry (DSC), and DC electrical conductivity measurements. The UV-vis-NIR spectrum showed that PANI remained doped in the composite, and this improved the mechanical and electrical proprieties of NR films and afforded them good thermal stability up to ~200ºC. The percolation threshold did not follow the universal critical exponent, and in this case, conduction preferentially occurs by hopping and tunneling. <![CDATA[<b>X-Ray diffraction technique applied to study of residual stresses after welding of duplex stainless steel plates</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700012&lng=en&nrm=iso&tlng=en Duplex stainless steel is an example of composite material with approximately equal amounts of austenite and ferrite phases. Difference of physical and mechanical properties of component is additional factor that contributes appearance of residual stresses after welding of duplex steel plates. Measurements of stress distributions in weld region were made by X-ray diffraction method both in ferrite and austenite phases. Duplex Steel plates were joined by GTAW (Gas Tungsten Arc Welding) technology. There were studied longitudinal and transverse stress components in welded butt joint, in heat affected zone (HAZ) and in points of base metal 10 mm from the weld. Residual stresses measured in duplex steel plates jointed by welding are caused by temperature gradients between weld zone and base metal and by difference of thermal expansion coefficients of ferrite and austenite phases. Proposed analytical model allows evaluating of residual stress distribution over the cross section in the weld region. <![CDATA[<b>Residual stress analysis of drive shafts after induction hardening</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700013&lng=en&nrm=iso&tlng=en Typically, for automotive shafts, shape distortion manifests itself in most cases after the induction hardening by an effect known as bending. The distortion results in a boost of costs, especially due to machining parts in the hardened state to fabricate its final tolerances. In the present study, residual stress measurements were carried out on automotive drive shafts made of DIN 38B3 steel. The samples were selected in consequence of their different distortion properties by an industrial manufacturing line. One tested shaft was straightened, because of the considerable dimensional variation and the other one not. Firstly, the residual stress measurements were carried out by using a portable difractometer, in order to avoid cutting the shafts and evaluate the original state of the stresses, and afterwards a more detailed analysis was realized by a conventional stationary diffractometer. The obtained results presented an overview of the surface residual stress profiles after induction hardening and displayed the influence of the straightening process on the redistribution of residual stresses. They also indicated that the effects of the straightening in the residual stresses cannot be neglected. <![CDATA[<b>Hybrid films with (trimethoxysilylpropyl) methacrylate (TMSM), poly (methyl methacrylate) PMMA and tetraethoxysilane (TEOS) applied on tinplate</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700014&lng=en&nrm=iso&tlng=en The tetraethoxysilane (TEOS) influences morphological and electrochemical properties of hybrid films by function of concentration. Moreover, the use of acetic acid as a catalyst in the sol enables a more complete hydrolysis of the silane precursors due to the fact that the acetic acid goes through a more complete ionization when in aqueous solution. The aim of this paper is to study the effect of the concentration of tetraethoxysilane (TEOS) on the protective properties of the film on tinplate substrate. The tinplate was coated with a hybrid film obtained from a sol-gel method constituted of the following alkoxide precursors: 3 - (trimetoxisililpropil) methacrylate (TMSM) and poly(methyl methacrylate) PMMA. The effect of tetraethoxysilane (TEOS) concentration has also been evaluated. The films hydrolysis was performed at a pH value of 3. 0 using acetic acid as a catalyst. The films were obtained by dip-coating process, cured for 3 hours at 160 ºC. The film morphology was evaluated by SEM and profilometry. The electrochemical behavior of the films was evaluated by open circuit potential monitoring, potentiodynamic polarization and electrochemical impedance spectroscopy. The film hydrophobicity was determined by contact angle measurements. The studied films have shown good performance as to corrosion resistance on tinplate. The hybrid film which was obtained through the addition of an excessive amount of TEOS (T3A3) showed increased thickness. Nevertheless, due to an intense densification of the film, promoted by the addition of TEOS, a formation of cracks was registered, thereby compromising the corrosion resistance. <![CDATA[<b>Effect of desulfurization of diesel and its blends with biodiesel on metallic contact</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700015&lng=en&nrm=iso&tlng=en The current environmental scenario has required changes in fuel nature, in order to minimize the harmful effects caused by sulfur in diesel. However, reductions in sulfur content promote loss of its lubricity and consequently wear in the injection system of the diesel engine. This study aimed to investigate the influence of sulfur minimization on fuel lubricity and wear of metallic disks. The fuel tribological analysis was carried out in HFRR equipment in accordance with ASTM D 6079 - 04. The tested fuels were diesel oil with 50, 500 and 1800 ppm sulfur, and their blends of soybean and sunflower biodiesel (5, 20 and 100% in volume). The results showed an increase of disks wear with reduction of sulfur content when lubricated with pure diesel. This fact was decreased when biodiesel was added to all concentrations. <![CDATA[<b>Micro and nanometric wear evaluation of metal discs used on determination of biodiesel fuel lubricity</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700016&lng=en&nrm=iso&tlng=en The contact of diesel fuel with engine subsystems demands a good wear resistance. Lubricity is an important feature for integrity of injection system and the sulphur composites are primarily responsible for lubrication of the injector nozzle. Biodiesel is responsible for partially restoring the lubricity of diesel fuel that presents low levels of sulphur composites and, furthermore, it causes less pollution than diesel fuel. The lubricity is measured through the wear scar diameter following the ASTM D 975 standards. However, the friction and wear with light loads of micro/nanocomponents are highly dependent on surface interactions that can be evaluated by microscopy techniques. This study aimed to measure and to analyze the biodiesel lubricity and their blends (B5, B20) with diesel by observing the wear scars of discs using the scanning electronic microscopy (SEM), atomic force microscopy (AFM) and micro roughness techniques. The fuels performance was evaluated using HFRR tribometer. The tests conditions were based on standard ADTM D-6079-04. The coefficient of friction was measure during the test. After the test, the worn ball and disc were analyzed by SEM, AFM and profilometer. The results showed that the addition of biodiesel in diesel improve the tribological performance of fuel. Also, the just WSD value is not sufficient to evaluate the lubrication ability of a fuel. Analysis of the worn disc surfaces proved to be compatible with WSD number and also more sensitive to these kinds of fuels, showing mainly the form and intensity of the wear. <![CDATA[<b>Low-temperature plasma nitriding of sintered PIM 316L austenitic stainless steel</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700017&lng=en&nrm=iso&tlng=en This work reports experimental results on sintered PIM 316L stainless steel low-temperature plasma nitriding. The effect of treatment temperature and time on process kinetics, microstructure and surface characteristics of the nitrided samples were investigated. Nitriding was carried out at temperatures of 350, 380, 410 and 440 ºC , and times of 4, 8 and 16 h, using a gas mixture composed by 60% N2 + 20% H2 + 20% Ar, at a gas flow rate of 5.00 × 10-6 Nm³s-1, and a pressure of 800 Pa. The treated samples were characterized by scanning electron microscopy, X-ray diffractometry and microhardness measurements. Results indicate that low-temperature plasma nitriding is a diffusion controlled process. The calculated activation energy for nitrided layer growth was 111.4 kJmol-1. Apparently precipitation-free layers were produced in this study. It was also observed that the higher the treatment temperature and time the higher is the obtained surface hardness. Hardness up to 1343 HV0.025 was verified for samples nitrided at 440 ºC. Finally, the characterization of the treated surface indicates the formation of cracks, which were observed in regions adjacent to the original pores after the treatment. <![CDATA[<b>Preparation and characterization of hydrogels with potential for use as biomaterials</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700018&lng=en&nrm=iso&tlng=en Hydrogels have been extensively explored for biomedical applications due to their ability to absorb high water content in its structure, which gives excellent biocompatibility. This work aims at obtaining biocompatible hydrogels with potential for use in increasing the mechanical strength of bone substitutes, or controlled drug release. Poly (N-vinyl-2-pyrrolidone) hydrogels were prepared by free radical polymerization with and without the addition of acrylic acid. Azobisisobutyronitrile and ammonium persulfate were used as initiator and N,N-methylenebisacrylamide was used as the crosslinking agent. The characterization of the hydrogels was performed by thermogravimetric analysis, differential scanning calorimetry, infrared spectroscopy and swelling properties. The results obtained demonstrate different degrees of crosslinking and swelling of up to 490 ± 30%. The different properties of the hydrogels suggest different applications. <![CDATA[<b>Microstructure and mechanical properties of two Api steels for iron ore pipelines</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700019&lng=en&nrm=iso&tlng=en This research compares the mechanical behavior of two API steels (X60 and X70) used in the longest pipeline in the world for the conveyance of iron ore. Tensile tests, Charpy impact tests, CTOD tests and fatigue crack growth tests are performed at ambient temperature. Metallographic examination showed a banded microstructure consisting of polygonal ferrite and pearlite in both steels, with smaller grain size and the presence of a small quantity of bainite in the X70 steel. All the mechanical tests revealed a ductile behavior for the two steels. The X70 steel is preferable for the pipeline project, due its better mechanical resistance, with no significant loss of fracture toughness and fatigue resistance. Its performance could be even better, if an appropriate combination of thermomechanical processing parameters were able to produce a microstructure with minor amount of pearlite, where acicular ferrite/bainite are present. <![CDATA[<b>Study of oxo-biodegradable polyethylene degradation in simulated soil</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700020&lng=en&nrm=iso&tlng=en This study aims to evaluate the influence of pro-oxidant additive and accelerated aging on the degradation of polyethylene (PE) samples in simulated soil, in accordance with ASTM G160-03. Films of polyethylene with and without pro-oxidant additive were studied, before and after 72 hours of accelerated aging. The films were initially characterized by analyses of Scanning Electron Microscopy (SEM) and Fourier Transform Infrared Spectroscopy (FTIR) (to evaluate the Carbonyl Index (CI)). The films were exposed for 30, 60 and 90 days in simulated soil, with controlled moisture and soil pH. The results showed the degradation of polyethylene films through an increase of CI in samples with additive and accelerated aging after 30 days of exposure, and a decrease, after 60 and 90 days, indicating the uptake of material oxidation by-products by microorganisms. The polyethylene films without pro-oxidant additive after accelerated aging showed greater structural and surface modifications, as compared to films with the additive. <![CDATA[<b>Electrical percolation, morphological and dispersion properties of MWCNT/PMMA nanocomposites</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700021&lng=en&nrm=iso&tlng=en Nanocomposites of poly (methyl methacrylate) (PMMA) and carbon nanotubes have a high potential for applications where conductivity and low specific weight are required. This piece of work concerns investigations of the level of dispersion and morphology on the electrical properties of in situ polymerized nanocomposites in different concentrations of multi-walled carbon nanotubes (MWCNT) in a PMMA matrix. The electrical conductivity was measured by the four point probe. The morphology and dispersion was analyzed by Transmission Electron Microscopy (TEM) and Small Angle X-ray Scattering (SAXS). The correlation between electrical conductivity and the MWCNT amount, presented a typical percolation behavior, whose electrical percolation threshold determined by power law relationship was 0.2 vol. (%) The exponent t from the percolation power law indicated the formation of a 3D network of randomly arranged MWCNT. SAXS detected that the structures are intermediate to disks or spheres indicating fractal geometry for the MWCNT aggregates instead of isolated rods. HR-TEM images allowed us to observe the MWCNT individually dispersed into the matrix, revealing their distribution without preferential space orientation and absence of significant damage to the walls. The combined results of SAXS and HR-TEM suggest that MWCNT into the polymeric matrix might present interconnected aggregates and some dispersed single structures. <![CDATA[<b>Synthesis and characterization of water-dispersed CdSe/CdS core-shell quantum dots prepared via layer-by-layer method capped with carboxylic-functionalized poly(vinyl alcohol)</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700022&lng=en&nrm=iso&tlng=en The main goal of this work was to synthesize CdSe/CdS (core-shell) nanoparticles stabilized by polymer ligand using entirely aqueous colloidal chemistry at room temperature. First, the CdSe core was prepared using precursors and acid-functionalized poly(vinyl alcohol) as the capping ligand. Next, a CdS shell was grown onto the CdSe core via the layer-by-layer technique. The CdS shell was formed by two consecutive monolayers, as estimated by empirical mathematical functions. The nucleation and growth of CdSe quantum dots followed by CdS shell deposition were characterized by UV-vis spectroscopy, photoluminescent (PL) spectroscopy and transmission electron microscopy (TEM). The results indicated a systematic red-shift of the absorption and emission spectra after the deposition of CdS, indicating the shell growth onto the CdSe core. TEM coupled with electron diffraction analysis revealed the presence of CdSe/CdS with an epitaxial shell growth. Therefore, it may be concluded that CdSe/CdS quantum dots with core-shell nanostructure were effectively synthesized. <![CDATA[<b>Chemical modification of chitosan in the absence of solvent for diclofenac sodium removal: pH and kinetics studies</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700023&lng=en&nrm=iso&tlng=en Chitosan was modified with acetylacetone and ethylenediamine in the absence of solvent. The new biopolymer obtained from the modification was characterized by elemental analysis and NMR 13C and applied in the removal of diclofenac sodium aqueous solution varying the pH and time. Through elemental analysis was possible to verify a decreasing in C/N relation after reaction with acetylacetone and an increasing after modification with ethylenediamine. From NMR analysis was verified the appearance of peaks around 160-210 ppm in both materials due to free carbonyl groups in the first step of the modification, besides the formation of imine bonds. The adsorption tests showed that the highest value occurred at pH 4 and from the results of the kinetic study was found that maximum adsorption occurred within 45 minutes and experimental data adjusted better to linear adjustment, following pseudo second-order model. The results show a material efficient in the removal of emerging pollutants. <![CDATA[<b>Evaluation of sodium diclofenac release using natural rubber latex as carrier</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700024&lng=en&nrm=iso&tlng=en Sodium Diclofenac is a non-steroidal anti-inflammatory drug (NSAID) taken to reduce inflammation and, as an analgesic, reduce pain. Although this drug is widely used in the general population, properties such as the short half-time and some side effects restrict its clinical use. The most common side effects are: gastric irritation, gastritis, peptic ulcer and bleeding. Studies involving biomaterials as carrier for drug release have been proving their efficiency in overcoming those problems and better controling the release rate and targeting of the drug. Natural rubber latex (NRL) has been proven excellent for its biocompatibility and ability to stimulate angiogenesis, cellular adhesion and the formation of extracellular matrix, promoting the replacement and regeneration of tissue. In this work, a NRL membrane is used to deliver sodium diclofenac. Sodium diclofenac (NaDic) was found to be adsorbed on the NRL membrane, with little or no incorporation into the membrane bulk, according to energy dispersive Scanning Electron Microscopy with X-Ray microanalysis (SEM-EDS) spectroscopy. In addition, FT-IR shows that there is no molecular-level interaction between drug and NRL. Already, the X-Ray Diffraction (XRD) of NaDic-NRL shows a broader one spectrum than the sharper halo (amorphous characteristic XRD spectrum) of pure NRL. More importantly, the release time of diclofenac in a NRL membrane in vitro was increased from the typical 2-3 h for oral tablets to ca. 74 h. The kinetics of the drug release could be fitted with a double exponential function, with two characteristic times of 0.899 and 32.102 h. In this study, we demonstrated that the interesting properties provided by NRL membranes combined with a controlled release of drug is relevant for biomedical applications. <![CDATA[<b>Adsorption of a textile dye from aqueous solutions by carbon nanotubes</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700025&lng=en&nrm=iso&tlng=en Multi-walled and single-walled carbon nanotubes were used as adsorbents for the removal of Reactive Blue 4 textile dye from aqueous solutions. The adsorbents were characterised using Raman spectroscopy, N2 adsorption/desorption isotherms and scanning and transmission electron microscopy. The effects of pH, agitation time and temperature on adsorption capacity were studied. In the acidic pH region, the adsorption of the dye was favourable using both adsorbents. The contact time to obtain equilibrium isotherms at 298-323 K was fixed at 4 hours for both adsorbents. For Reactive Blue 4 dye, Liu isotherm model gave the best fit for the equilibrium data. The maximum sorption capacity for adsorption of the dye occurred at 323 K, attaining values of 502.5 and 567.7 mg g-1 for MWCNT and SWCNT, respectively. <![CDATA[<b>Influence of different fuel agents on the combustion synthesis of the nanostructured Li<sub>1.05</sub>Mn<sub>2</sub>O<sub>4 </sub>oxide</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700026&lng=en&nrm=iso&tlng=en In this work nanostructured Li1.05Mn2O4 oxide was obtained by Solution Combustion Synthesis (SCS) using three different fuel agents in order to obtain a unique phase with a crystalline cubic structure belonging to the Fd3m spatial group. The phase of interest could be obtained, following the order: glycine (at 600 °C for 2 h) < urea (at 750 °C for 2 h) < maleic anhydride (at 750 °C for 4 h), with crystallite size in the range from 4.6 to 9.7 nm (nanometric character) and the unit cell parameter of the calcined samples at 750 °C for 2 h were similar to the JCPDS 35-0782 with cubic structure (a = 8.247 Å). Charge and discharge tests from the samples obtained by glycine fuel (at 750 °C for 4 h) presented the highest experimental specific capacities of 115 mA h g-1 and 92% of retention after 10 cycles. <![CDATA[<b>Effect of the processing parameters on the crystalline structure of lanthanide orthotantalates</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700027&lng=en&nrm=iso&tlng=en The influence of the synthesis parameters on the crystalline structures of orthotantalate ceramics has been investigated. Powder materials were prepared by the solid-state reaction route. X-ray diffraction and Raman scattering measurements were employed to investigate the crystal structure of the produced materials. In this work, we analyzed three different examples in which the temperature and time were decisive on the final crystal structure of LnTaO4 compounds besides the lanthanide ionic size. Firstly, the thermal evolution for NdTaO4 samples showed that mixed crystal phases are formed up to 1100 ºC, while well-crystallized M-NdTaO4 (I2/a) materials are obtained in temperatures higher than 1200 ºC. Also, the influence of the synthesis time was investigated for the LaTaO4 ceramics: it was necessary 14 h to obtain samples in the P2(1)/c structure. Finally, two polymorphs could be obtained for the DyTaO4 ceramics: P2/a and I2/a space groups were obtained at 1300 ºC and 1500 ºC, respectively. This study indicated that the temperature, time and lanthanide size are directly correlated with the crystalline arrangement of the orthotantalate materials. <![CDATA[<b>Synthesis and characterization of zeolite NaP using kaolin waste as a source of silicon and aluminum</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700028&lng=en&nrm=iso&tlng=en The synthesis of zeolite NaP using kaolin waste, from the Amazon region, as a predominant source of silicon and aluminum has been studied. The zeolitisation process occurred in hydrothermal conditions using static autoclaving and the effects of time, temperature, and the Si/Al ratio were investigated. The starting material and the phases formed as reaction products were characterized by XRD, SEM and FTIR. The results showed that pure zeolite NaP is hydrothermally synthesized, at 100 °C for 20 hours, using metakaolin waste material in alkaline medium in presence of additional silica. The XRD and SEM analyses indicate that the synthesized zeolite presents good crystallinity. <![CDATA[<b>Development of self-lubricating composite materials of nickel with molybdenum disulfide, graphite and hexagonal boron nitride processed by powder metallurgy</b>: <b>preliminary study</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700029&lng=en&nrm=iso&tlng=en The purpose of this work was to develop nickel self-lubricating composites using solid lubricant as second phase and obtained by powder metallurgy. The work involved the study of chemical stability and chemical interaction between the nickel alloy matrix and solid lubricating additives (molybdenum disulfide, graphite and hexagonal boron nitride). The results showed a thermodynamic stability during sintering for the composites containing the phases of graphite and hexagonal boron nitride. The presence of molybdenum disulfide phase permits a reaction with the matrix, the formation of a liquid phase of nickel sulfide and the solubilization of molybdenum in the matrix. <![CDATA[<b>ECAE processed NiTi shape memory alloy</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700030&lng=en&nrm=iso&tlng=en The current work evaluated the microstructures and martensitic transformation temperatures of NiTi shape memory alloy (SMA) deformed by equal channel angular extrusion (ECAE). The Ti-55.27wt.%Ni alloy was processed by 1 ECAE pass at 250 °C using a die with an intersection angle of 120°. After processing, samples were annealed at 300 °C, 400 °C and 500 °C for 1h to evaluate the microstructural changes. Microstructural characterization was performed by scanning electron microscopy (SEM) equipped with an energy dispersive spectrometer (EDS) device, and Vickers hardness measurement. Martensitic transformations temperatures were analyzed by differential scanning calorimetry (DSC). Results show that the annealing treatments presented no significant change in the microstructure of the ECAE processed samples. Meanwhile, the DSC curves corresponding to the annealing treatments performed at 300 °C and 400 °C show two step martensitic transformation related to B2→R→B19'. For the annealing at 500 °C, the martensitic transformation temperatures returned to the ST condition, indicating a reduction of the processing defects. <![CDATA[<b>Synthesis of stimuli-sensitive copolymers by RAFT polymerization</b>: <b>potential candidates as drug delivery systems</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700031&lng=en&nrm=iso&tlng=en Poly(2-(dimethylamino)ethylmethacrylate-b-methymethacrylate) (PDMAEMA-b-PMMA) poly(2-(dimethylamino)ethylmethacrylate-b-vinylcaprolactam-b-(2-(dimethylamino)ethyl methacrylate) (PDMAEMA-b-PVCL-b-PDMAEMA) and poly(vinylcaprolactam-b-(2-(dimethylamino)ethylmethacrylate-b-vinylcaprolactam) (PVCL-b-PDMAEMA-b-PVCL) block copolymers were obtained by reversible addition-fragmentation chain transfer (RAFT) polymerization, and the effect of the solution pH on the particle size was investigated. In the case of PDMAEMA-b-PMMA, PDMAEMA was first synthesized using 2-cyanoprop-2-yl dithiobenzoate (CPDB) as a chain transfer agent (CTA), which was subsequently used for the RAFT polymerization of MMA. The triblock copolymers were obtained using PDMAEMA or PVCL as macro-CTAs prepared using dibenzyl trithiocarbonate (DBTTC) as a bifunctional RAFT agent. The structure and formation of the copolymers was confirmed through ¹H NMR and SEC analysis. The particle size varied considerably depending on the pH of the aqueous solutions of copolymers indicating that these materials could be potential candidates for biomedical applications. <![CDATA[<b>Evaluation of a nanostructured microwave absorbent coating applied to a glass fiber/polyphenylene sulfide laminated composite</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700032&lng=en&nrm=iso&tlng=en The rapid coating of composites with absorbing paints yields materials that can absorb microwave radiation and still have approximately the same specific mass of the original composites. The use of paints with specific electromagnetic properties together with carbon- nanotube-based materials allows the production of structural materials of interest to the aeronautical industry. Thus, the objective of this study was to produce and characterize the electromagnetic properties of a material consisting of a microwave absorbing coating (carbon nanotubes and polyurethane) applied to a laminated composite made with polyphenylene sulfide and glass fiber. The attenuation of microwaves (8 to 12 GHz) incident on this material was evaluated using the waveguide technique to determine whether this material can be used as an absorbing structural material. The results show that the material absorbs up to 90% of the energy of the incident microwave, indicating that the material is an efficient absorber of microwave radiation. <![CDATA[<b>Influence of coupling agent in compatibility of post-consumer HDPE in thermoplastic composites reinforced with eucalyptus fiber</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700033&lng=en&nrm=iso&tlng=en This study investigates the feasibility of using recycled high density polyethylene (HDPE) and wood fiber from species Eucalyptus grandis (EU) to manufacture experimental composite panels. The use of maleated polyethylene as coupling agent (CA) improved the compatibility between the fiber and plastic matrix. The mechanical properties of the resultant composites were compared with polymer with and without compatibilizer. The influence of the coupling agent (CA) in the polymer matrices and composites were evaluated at different concentrations, checking the physical, mechanical and thermal properties of wood plastic composites (WPC). Results of mechanical, physical and thermal properties showed that concentration of 3% w/w CA in the polymer matrices was that which showed the best results, but in the composites properties were very similar in all formulations. Based on the findings in this work, it appears that recycled materials can be used to manufacture value-added panels without having any significant adverse influence on material properties. <![CDATA[<b>Characterization of polyurethan skin agglomerates for acoustic insulation from impact noise</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700034&lng=en&nrm=iso&tlng=en Polymeric materials are greatly used in industry due to their versatility in application generating therefore, large quantities of solid waste. Population growth in urban areas, with living quarters mainly in residential buildings, face discomfort caused by noise, particularly by impact noise. Aiming at reducing the amount of polymeric material disposed of in the environment and at providing alternatives of reuse, together with the possibility of reducing noise impact from construction works, agglomerates of polyurethane skin (PUs) have been developed. The recycling process of PUs was developed through variations in particle size and pressing temperature of agglomerates. PU agglomerates of coarse particle size, hot pressing process and close cell structure presented reductions in noise level up to 20 dB, showing that it is suitable for acoustic insulation. <![CDATA[<b>Kinetic study of the catalytic pyrolysis of elephant grass using Ti-MCM-41</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000700035&lng=en&nrm=iso&tlng=en This work aimed to study the kinetics of thermal and catalytic pyrolysis using Ti-MCM-41 as catalyst in order to assess the catalytic pyrolysis efficiency compared to thermal pyrolysis of elephant grass. Ti-MCM-41 molecular sieve was synthesized by hydrothermal method from hydrogel with the following molar composition:1.00 CTMABr: 4.00 SiO2:X TiO2: 1 + X Na2O: 200.00 H2O, whichstructure template used was cetyltrimethylammonium bromide (CTMABr). The materials synthesized were characterized by X-ray diffraction, IR spectroscopy, thermogravimetric analysis and specific area by the BET method, for subsequent application in the biomass pyrolysis process. The kinetic models proposed by Vyazovkin and Flynn-Wall were used to determine the apparent activation energy involved in the thermal and catalytic pyrolysis of elephant grass and the results showed that the catalyst used was effective in reducing the apparent activation energy involved in the thermal decomposition of elephant grass.