Scielo RSS <![CDATA[Materials Research]]> http://www.scielo.br/rss.php?pid=1516-143920140003&lang=en vol. 17 num. 3 lang. en <![CDATA[SciELO Logo]]> http://www.scielo.br/img/en/fbpelogp.gif http://www.scielo.br <![CDATA[<b>Surface contact fatigue failure of a case hardened pinion shaft</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300001&lng=en&nrm=iso&tlng=en An investigation was made to determine the causes of surface contact fatigue failure of a case hardened driver pinion located in the intermediate shaft of a reducer gearbox used in a sugar and alcohol mill. The examination of the component revealed the presence of a cemented layer substantially thicker than that generally specified for pinions devised for this application. This, associated with the massive presence of brittle threadlike carbon-rich cementite phase (Fe3C) in prior austenite grain boundaries of the pinion teeth, favored surface crack nucleation and propagation during cyclic loading, leading to spallation of the contact surface with the counterpart gear, which impaired the system's operation. Poor carburization practice was discovered as the root cause of the mechanical failure, thus demanding the implementation of a new manufacturing route to avoid problems in similar load-bearing rotating components. <![CDATA[<b>Synthesis and characterization of Fe<sub>3</sub>O<sub>4</sub> nanoparticles with perspectives in biomedical applications</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300002&lng=en&nrm=iso&tlng=en Nowadays the use of magnetic nanoparticles (MNP) in medical applications has exceeded expectations. In molecular imaging, MNP based on iron oxide coated with appropriated materials have several applications in vitro and in vivo studies. For applications in nanobiotechnology these MNP must present some characteristics such as size smaller than 100 nanometers, high magnetization values, among others. Therefore the MNP have physical and chemical properties that are specific to certain studies which must be characterized for quality control of the nanostructured material. This study presents the synthesis and characterization of MNP of magnetite (Fe3O4) dispersible in water with perspectives in a wide range of biomedical applications. The characterization of the colloidal suspension based on MNP stated that the average diameter is (12.6±0.2) nm determined by Transmission Electron Microscopy where the MNP have the crystalline phase of magnetite (Fe3O4) that was identified by Diffraction X-ray and confirmed by Mössbauer Spectroscopy. The blocking temperature of (89±1) K, Fe3O4 MNP property, was determined from magnetic measurements based on the Zero Field Cooled and Field Cooled methods. The hysteresis loops were measured at different temperatures below and above blocking temperature. The magnetometry determined that the MNP showed superparamagnetic behavior confirmed by ferromagnetic resonance. <![CDATA[<b>Theoretical investigation of geometric configurations and vibrational spectra in citric acid complexes</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300003&lng=en&nrm=iso&tlng=en The performance of advanced electronic ceramics is directly related to the synthesis route employed. Sol-gel methods are widely used for this purpose. However, the physicochemical intermediate steps are still not well understood. Better understanding and control of these processes can improve the final quality of samples. In this work, we studied theoretically the formation of metal complexes between citric acid and lithium or barium metal cations with different citric acid/metal proportions, using Density Functional Theory electronic structure calculations. Infrared and Raman scattering spectra were simulated for the more stable geometric configurations. Using this methodology, we identified some features of complexes formed in the synthesis process. Our results show that the complexes can be distinguished by changes in the bands assigned to C=O, COH-, and COO- group vibrations. An estimate of the most stable complexes is made based on total energy. <![CDATA[<b>Study of Ti-7.5Si-22.5B alloys produced by powder metallurgy</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300004&lng=en&nrm=iso&tlng=en Refractory alloys with silicides and borides have been used in high temperature applications because their elevated melting point, good oxidation resistance and high strength-to-weight ratio. The present study approaches the preparation of Ti-7.5Si-22.5B (at.-%) alloys through high-energy ball milling and sintering. The powders and compacts obtained in these processes were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), density measurements, chemical analyses and Vickers hardness. It was verified that silicon and boron powders are dissolved in the titanium during milling with an iron contamination up to 6.0 at.-%. Furthermore, the use of short milling times and alcohol during the final stages of milling increases the powder yield. Such increasing was obtained even with a high rotary speed (300 rpm), which generally creates higher temperatures and consequently more sticking. After sintering of the as-milled powders, it was indentified mainly the Ti+Ti6Si2B+TiB+Ti5Si3 phases in the Ti-7.5Si-22.5B sintered alloys, which presented hardness values up to 800 HV. The materials produced by the present work can be employed in coating research as sputtering targets. <![CDATA[<b>Preparation and characterization of UV-cured hybrid polyvinyl alcohol nanofiber membranes by electrospinning</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300005&lng=en&nrm=iso&tlng=en The present study investigated the possibility of preparing polyvinyl alcoholic (PVA) organic-inorganic hybrid nanofiber membranes by electrospinning with UV irradiation. To this end, PVA, PVA/SiO2 organic-inorganic hybrid obtained with Geniosil® XL 33 as a SiO2 source, and imidazole-functionalized mesoporous PVA/SiO2/N=N nanofiber membranes were synthesized. These membranes were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, thermogravimetric-differential thermal analysis, and Brunauer - Emmett - Teller analysis. According to results, fine polymeric nanofibers were obtained in the size range of 100-200 nm for pure PVA nanofibers and 150-250 nm for PVA/SiO2 hybrid nanofibers, while imidazole-functionalized PVA/SiO2 nanofibers were less than 100 nm. The membranes produced are suitable for use in various applications, including filtration and adsorption, in the biomedical and textile industries, among others. <![CDATA[<b>Comparative study of the characteristics of nano silica - , silica fume - and fly ash - incorporated cement mortars</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300006&lng=en&nrm=iso&tlng=en The structural characteristics of cement mortars, impregnated with nano silica (NS), silica fume (SF) and fly ash (FA), were comparatively studied using Fourier transform infrared spectrometer (FTIR), thermogravimeter-differential thermogravimeter (TG-DTG) and scanning electron microscope (SEM). The mechanical strengths of the specimens were determined at early (7th day) and standard (28th day) curing ages. The compressive strengths and flexural strengths developed in the mortar specimens containing NS particles were found considerably higher than those of the corresponding specimens of SF and FA over and above the control at both ages. FTIR, TG-DTG and SEM analyses results were consistent with the remarkable increase in the mechanical strength of the mortars with NS. These increases in the strengths of the mortars with NS are attributable to the nano sized particles and extensive surface area of NS. The nano sized particles, as nucleating agents, promoted the hydration of C3S and C2S and the formation of C - S - H phase. Plenty of active sites on the surface of NS particles induced their pozzolanic reactivity and the extent of bond formation between NS particles and free CH. <![CDATA[<b>Microstructural evaluation on shape recovery in stainless Fe-Mn-Si-Cr-Ni-Co SMA processed by wire drawing</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300007&lng=en&nrm=iso&tlng=en The effect of the microstructure on the shape recovery in stainless Fe-8Mn-5Si-13Cr-6Ni-12Co shape memory steel (SSMS) was evaluated using tensile tests and reversion temperature of 600ºC for a pre-strain of 4%. The tests were performed for a solution treated and annealed conditions at different temperatures after wire drawing of 57% area reduction. The best total shape recovery (TSR) was 83% for a sample deformed and annealed at 850ºC. It was concluded that the elastic (or, superelastic) shape recovery (ESR) is high when the austenitic matrix strength is high surpassing the value of shape recovery due to memory effect (SR) and once the austenitic matrix becomes softer, the contribution of SR increases and that of ESR decreases. <![CDATA[<b>Evaluation of piezoresistivity properties of sputtered ZnO thin films</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300008&lng=en&nrm=iso&tlng=en Zinc oxide (ZnO) thin films were deposited by RF reactive magnetron sputtering on silicon (100) substrates under different experimental conditions. ZnO films were studied before and after annealing treatment at 600 °C. The crystallinity, electrical resistivity, stoichiometry, thickness, and elastic modulus of the films were investigated. ZnO piezoresistors were produced using microelectronics processes, such as photolithography, lift-off, and reactive ion etching (RIE). Cantilever method was used to determine the gauge factor, and measurements of Temperature Coefficient of Resistance (TCR) were performed on a hotplate. The optimization of the deposition conditions produced ZnO thin films with controlled stoichiometry (ZnO), crystalline microstructure (phase wurzite, 002), high elastic modulus (156 GPa), and low electrical resistivity (0.072 ohm.cm), which are good properties for application as piezoresistive pressure microsensor. In addition, the ZnO piezoresistors had a GF of 2.6 on the deformation in the plane (100) and TCR of - 1610 ppm/K up to 250 °C. <![CDATA[<b>Markov Chains and reliability analysis for reinforced concrete structure service life</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300009&lng=en&nrm=iso&tlng=en From field studies and the literature, it was found that the degradation of concrete over time can be modelled probabilistically using homogeneous Markov Chains. To confirm this finding, this study presents an application of Markov Chains associated with the reliability analysis of experimental results of the degradation of concrete by chlorides. Experimental results were obtained for chloride penetration originating from non-accelerated tests in concretes in which the water/binder ratio was variable (0.40, 0.50 and 0.60) and that were produced with Pozzolanic Portland cement that was exposed for six months to the action of NaCl. Using a simulation process, the failure and safety probabilities were calculated by reliability and using Markov Chains, a service life project was estimated (a period of corrosion initiation). Compared to a concrete structure itself, the average error of service life predicted using Markov was approximately 14%. The results show a promissory methodology, in combination with the determination of concrete cover thickness, according to the required service life. <![CDATA[<b>Evaluation of a 7050-TAF aluminum alloy submitted to creep age forming</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300010&lng=en&nrm=iso&tlng=en CAF process combines creep and precipitation hardening which are highly dependent on time and temperature. The aging cycle relax the stresses induced during the loading phase. At the end of the process stress relaxation induces shape changes in the part but significant spring back is observed (about 70%). Usually CAF cycles for 7XXX alloys use times around 20 h and temperatures in the range of 120°C to 190°C. In the present work CAF tests were performed using the alloy 7050 in an intermediate condition named Temper to Age Forming (TAF). Using the alloy 7050-TAF resulted in significant process time reduction. From TAF temper, only 8 hours are necessary to achieve properties comparable to T74. Coupons were submitted to CAF in two levels of initial stress, 190 MPa and 290 MPa, resulting in spring back values of 70% and 60 % respectively. In addition, constant load creep tests were performed in the same stress levels and time of CAF tests to find the creep strain values. Creep tests performed under 190 MPa resulted in strain values around 0,1% after 8 h. On the other hand creep tests performed under 290 MPa failed after 7 h with creep strain values of 1,7%. Results obtained are close to that found in previous studies and it is possible to conclude that the use of alloy 7050 in TAF condition allows CAF to be done in 8 hours, since the initial stress is lower than 290 MPa. <![CDATA[<b>Corrosion behavior and characterization of plasma nitrided and borided AISI M2 steel</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300011&lng=en&nrm=iso&tlng=en This study investigates the corrosion behaviors of plasma nitrided (PN) and borided AISI M2 steels. The PN process was carried out in a dc-plasma system at a temperature of 923K for 6 h in a gas mixture of 80%N2-20%H2 under a constant pressure of 5 mbar. The boriding process was carried out in Ekabor-II powder at a temperature of 1223K for 6 h. X-ray diffraction analysis on the surface of the PN and borided steels revealed the presence of FeB, Fe2B, CrB, MoB, WB, FeN, Fe2N, Fe3N and Fe4N compounds. Corrosion surfaces of the samples were analyzed using a SEM microscopy and X-ray energy dispersive spectroscopy EDS. The corrosion resistance of PN and borided AISI M2 steel is higher compared with that of untreated AISI M2 steel. Corrosion resistances of the PN and borided AISI M2 steel increased the 4-6- fold. <![CDATA[<b>Synthesis and characterization of a novel terpolymer based on L-lactide, D,L-lactide and trimethylene carbonate</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300012&lng=en&nrm=iso&tlng=en Terpolymers of L-lactide, D,L-lactide and trimethylene carbonate (TMC) were synthesized via the ring-opening polymerization reaction for cyclic monomers using stannous octoate as the initiator at a ratio of ~0.05 mol% (monomers/(SnOct)2). Synthesis was done at 130 ºC for 48 h. The inclusion of TMC, an aliphatic elastomeric polycarbonate, alongside polymer chain segments containing L-lactide and D,L-lactide, was expected to yield a material with improved properties such as increased elongation; this would overcome the limitation of copolymers consisting entirely of lactide and D,L-lactide. The terpolymer properties were assessed by Nuclear magnetic resonance spectroscopy ¹H and 13C NMR, infrared spectroscopy, differential scanning calorimetry and thermogravimetry, with particular attention being given to the effect of TMC on the copolymer of L-lactide-co-D,L-lactide. The mixing of these polymers resulted in material with a high molar mass (10(5) g/mol). The mechanical properties of the terpolymer were assessed using pins of this material that were tested by mechanical flexion at three points. When compared with results for the copolymer PLDLA there was a decrease in Young's modulus for the TMC-containing terpolymer. <![CDATA[<b>Microstructural evidence of beryllium in commercial dental Ni-Cr alloys</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300013&lng=en&nrm=iso&tlng=en The focus of this work was to determine microstructural features in commercial Ni-Cr alloys which could be used to identify indirectly the presence of beryllium. Thus, eight commercial alloys were characterized by chemical analysis, thermal analysis, X-ray diffraction (XRD), scanning electron microscopy - back-scattered electron images (SEM/BSE), energy-dispersive spectroscopy (EDS). The results indicate that the presence of beryllium can be inferred from microstructural analysis via XRD and SEM/BSE. The X-ray diffractograms of the beryllium-containing alloys showed clearly the existence of the NiBe intermetallic phase. SEM/BSE images of these alloys show a very characteristic eutectic microstructure which also indicates the presence of this element. These characteristics are not observed in the beryllium-free alloys. <![CDATA[<b>The effect of voltage on the arc stud welding of microwave sintered Fe+Al powder mixture</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300014&lng=en&nrm=iso&tlng=en The joining of powder metallurgy products is of importance because of high demand in many industrial applications. In this study, the effect of welding voltage on the joint quality has been investigated using discharge arc stud welding, a low heat input welding method, without gas protection to join steel stubs to microwave sintered compacts containing a powder mixture of 26 atomic % Al and Fe (balance). It has been shown that welds with steel stubs are prone to side cracking in the weld zone and they also suffer from the oxidation of metal powders adjacent to weld zone. The forms of oxides are continuous and laminar type in welds with steel stubs and the composition of weld zone changes with increasing arc voltage. <![CDATA[<b>Cartilage reconstruction using self-anchoring implant with functional gradient</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300015&lng=en&nrm=iso&tlng=en This study presents an innovative and original biomaterial designed to substitute for articular cartilage and mimic its mechanical behavior, including elastic cushioning and the characteristics of fiber-reinforced gel. The material was composed of polyurethane and bioglass microfiber 45S5. It was designed to present a tribological surface to the cartilage of the tibial plateau, and to convert over a functional gradient to an osteointegrable region for self-anchorage to the subchondral bone. The biomaterial samples showed no toxicity and promoted cell spreading. Subsequent in vivo studies in rabbits demonstrated the formation of a rigid structure similar to bone trabeculae in the distal region of the tribological surface of the implant. The tribological surface of the proximal region showed a fibrocartilaginous tissue with highly vascularized chondrocytes, thus validating the proposed concept for the design of the implant incorporating a functional gradient and auto-stability. <![CDATA[<b>Preparation and characterization of paclitaxel-loaded PLDLA microspheres</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300016&lng=en&nrm=iso&tlng=en Paclitaxel (Taxol®), is a drug used to treat ovarian, breast, lung and bladder cancer. However, the low solubility of this drug in water is a major limitation in its clinical use. One strategy to overcome this limitation would be to encapsulate paclitaxel in polymeric microspheres that are biocompatible and can be used as drug carriers. The aim of this study was to use the bioresorbable, biocompatible copolymer poly-L-co-D,L-lactic acid (PLDLA) in the 70:30 rate to produce and characterize microspheres containing paclitaxel. The simple emulsion technique was used to obtain spherical microspheres that were studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The average size of PLDLA microspheres without and with paclitaxel was 10.3 ± 1.7 μm and 12.7 ± 1.3 μm, respectively, as determined by laser light scattering (LLS). Differential scanning calorimetry (DSC) showed that pure paclitaxel had an endothermic peak corresponding to a melting point of 220 °C, which indicated its crystalline nature. The same peak was observed in a physical mixture of PLDLA + paclitaxel in which both components were present in the same proportions used to prepare the microspheres . In contrast, this peak was not observed for the drug, indicating that paclitaxel did not crystallize in PLDLA microspheres. Differential scanning calorimetry (DSC) indicated that paclitaxel was homogeneously dispersed in the PLDLA microspheres, the incorporation of paclitaxel into the microspheres did not alter the thermal properties of PLDLA. The Fourier transform infrared spectroscopy (FTIR) analysis seems to indicate the absence of chemical interaction between polymer and drugs in microspheres and the presence of drugs as a molecular dispersion in the polymer matrix. The efficiency of paclitaxel encapsulation in PLDLA microspheres was 98.0 ± 0.3%, as assessed by high performance liquid chromatography (HPLC). A kinetic study of drug release in vitro using HPLC showed an initial burst release followed by a slower release characteristic of large diameter distribution systems. PLDLA microspheres released 90 ± 4% of the drug over a 30-day period. These findings indicate that PLDLA microspheres are promising carriers for paclitaxel, with a potential for future applications in drug delivery systems. <![CDATA[<b>Particleboard manufactured from Tauari (<i>Couratari</i><i> oblongifolia</i>) wood waste using castor oil based polyurethane resin</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300017&lng=en&nrm=iso&tlng=en Several wood species from the Amazon region are used in the manufacture of furniture, which leaves behind large amounts of waste (slabs, sawdust, sanding dust and bark), thus causing serious environmental impacts. An interesting alternative for the use of these wastes is the manufacture of particleboards. However, few studies have focused on the behavior of Amazonian tree species and the wastes resulting from production with this type of material. This paper discusses the potential use of Tauari (Couratari oblongifolia) wood waste as a raw material for the production of particleboards, using castor oil-based bi-component polyurethane adhesive. Experimental boards were prepared with dry wood particles and a castor-oil polyurethane adhesive content of 16%. The boards, whose nominal density was 1000 kg·m-3, were subjected to uniaxial compression (5 MPa) at 90, 110 and 130ºC for ten minutes. The particleboards were characterized by performing the following tests: Apparent density (D AP), Moisture (M), Water Absorption (WA), Thickness Swelling (TS), Static bending strength: MOR (Modulus of rupture) and MOE (Modulus of elasticity), Perpendicular Tensile Strength (IB - internal bonding) and Screw Pullout (SP), according to the Brazilian NBR 14.810:2006 standard. The results indicate that, regardless of the processing temperature, the average density of Tauari particleboard is 930 to 941 kg·m-3, with higher IB and TS than those specified by the NBR 14810-2 and ANSI A208.1 standards, enabling this product to be classified as high-density particleboard suitable for industrial and commercial use. <![CDATA[<b>Effect of hot pressing variables on the microstructure, relative density and hardness of sterling silver (Ag-Cu alloy) powder compacts</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300018&lng=en&nrm=iso&tlng=en The purpose of this work was to investigate the influence of the hot pressing variables, namely pressure, time and temperature, on the microstructure, density and hardness in a sterling silver alloy. Powders were hot pressed under different combinations of pressures (25MPa, 35MPa and 45MPa), times (10 min, 30 min and 60 min) and temperatures (250 ºC, 300 ºC, 400 ºC, 500 ºC and 700 ºC). The microstructures of hot pressed compacts were analyzed by the means of SEM/EDS and optical microscopy. The density and hardness of specimens were assessed. The microstructure of all specimens consisted in Cu-rich precipitates of different sizes dispersed in a Ag-rich matrix. Of the variables that were examined, only temperature produced significant (p<0.05) differences in the density and hardness of the compacts. Full density of powders compacts was achieved for temperatures above 400 ºC, irrespective of the hot pressing time. A hardness peak (~120HV) was observed for the specimens hot pressed at 400 ºC. <![CDATA[<b>Corrosion behavior of friction stir welded lap joints of AA6061-T6 aluminum alloy</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300019&lng=en&nrm=iso&tlng=en In this work, the corrosion behaviors of friction-stir lap welding of 6061-T6 Al-alloy are studied. The friction-stir lap welding was performed under different welding conditions (rotation speed and welding speed). The corrosion behavior of the parent alloy, the weld nugget zone (WNZ), and the heat affected zone (HAZ) of each welded sample working as an electrode, were investigated by the Tafel polarization test in 3.5 wt. (%) NaCl at ambient temperature. The morphology of the corroded surface of each region was analyzed by scanning electron microscopy together with energy dispersive spectroscopy (SEM-EDS). The results showed that the corrosion resistance of the parent alloy was better than the WNZ and the HAZ in both welding conditions. Localized pit dissolution and intergranular corrosion were the dominant corrosion types observed in the parent alloy, WNZ, and HAZ. The parent alloy, WNZ, and HAZ exhibited similar corrosion potentials (Ecorr) after T6 heat treatment. This treatment had a better effect on the corrosion resistance of the welded regions than the parent alloy. <![CDATA[<b>Physical and mechanical properties of particleboard manufactured from wood, bamboo and rice husk</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300020&lng=en&nrm=iso&tlng=en In this work, the physical-mechanical properties of particleboards manufactured with wood (Eucalyptus grandis), bamboo (Bambusa vulgaris) and/or rice husk (Oryza sativa) particles, combined or not, were assessed. They were produced in the following proportions: 100% wood; 100% bamboo; 100% rice; 50% wood and 50% bamboo; 50% wood and 50% rice husk. In order to characterize the manufactured particleboards, their physical (density; moisture content; water absorption and thickness swelling) and mechanical properties (static bending; internal bonding and screw withdrawal) were assessed. The results indicated that the use of rice husk caused reduction in particleboard quality. Particleboards manufactured with bamboo showed better quality than those using rice husk as raw material. For most parameters, the particleboards manufactured exclusively with wood particles showed similar performance to bamboo and wood-bamboo particleboards. <![CDATA[<b>Ag ion decoration for surface modifications of multi-walled carbon nanotubes</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300021&lng=en&nrm=iso&tlng=en The production of high performance metal matrix composites depends on a proper design of the surface of the reinforcing phase, ensuring a good contact with a metal phase. In the present work, two Ag decorating procedures to modify the surface of multi-walled carbon nanotubes (MWCNT) were evaluated for further production of aluminum matrix composites. The procedures consisted in a two steps route based on acid oxidation of carbon nanotubes (CNT) followed by suspension in an Ag ion solution; and a single step route, based on the effect of n-dimethylformamide (DMF) as an activation agent of CNT surface, in presence of Ag ions. Transmission and scanning-transmission electron microscopy, Raman and Fourier-transformed infrared spectroscopy were employed in order to characterize the results. The two steps route resulted in Ag nano-particles homogeneously deposited over the CNT surface. The mechanism for the deposition is based on carboxyl and probably hydroxyl functional groups formed in the first step, acting as nucleation sites for Ag precipitation in the second step. The single step route resulted in the formation of sub-micrometric Ag particles heterogeneously mixed to CNT bundles. <![CDATA[<b>Microstructural</b><b> characterization and mechanical behavior of a low-carbon 17%Mn steel</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300022&lng=en&nrm=iso&tlng=en Steels containing high levels of Mn, Si and Al exhibit high plasticity when deformed, owing to twinning-induced plastitity (TWIP) and transformation-induced plasticity (TRIP) effects. In this study, we investigated the microstructural evolution of samples of samples of a 17%Mn steel subjected to war rolling at 700º and 800ºC. We also studied the effects of the microstructure of the steel samples on their mechanical behavior. Using a mathematic model the stacking fault energy of the steel was estimated to be 14.5 mJ/m². This value was indicative of a martensitic transformation. The presence of martensite and twinned austenite was verified using optical microscopy, scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) analyses. The presence of austenite and ε- and α'-martensites was confirmed using X-ray diffraction (XRD) analyses and dilatometry. Increasing the rate of cold reduction resulted in the formation of a α'-martensite phase and a decrease in the volume fraction of the ε-martensite phase. The volume fractions of the various phases were measured by integrating the areas under the XRD peaks. The sample subjected to a cold-rolling reduction of 81% and a subsequent annealing treatment did not contain a α'-martensite phase, indicating that it was fully recrystallized. The Vickers microhardness of the samples increased with an increase in the cold-rolling reduction rate. However, the microhardness values of the cold-rolled samples decreased after the annealing treatment. <![CDATA[<b>Synthesis and characterization of novel ZrO<sub>2</sub>-SiO<sub>2</sub> mixed oxides</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300023&lng=en&nrm=iso&tlng=en In this study the mixed oxides ZrO2-SiO2, were synthesized by the sol-gel method with a molar ratio of 95:5 (Si/metal) and characterized by X-ray diffraction, absorption-desorption of N2, Fourier transform infrared spectroscopy, thermal gravimetric analysis, temperature-programmed desorption of ammonia, and acidity test by titration. The synthesized materials, which are amorphous to X-rays, are composed of a mixture of micro- and mesopores. They show a higher acid strength than the separate oxides, indicating that the ZrO2 is highly dispersed in the silica matrix. <![CDATA[<b>Nitriding of AISI 1020 steel</b>: <b>comparison between conventional nitriding and nitriding with cathodic cage</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300024&lng=en&nrm=iso&tlng=en Cylindrical samples of AISI 1020 steel were nitrided, using the techniques of conventional plasma nitriding and cathodic cage. In the latter, the samples are kept at floating potential, inside of a cage that works as a cathode and to shield the samples from the cathodic potential. A systematic study was conducted in order to evaluate the efficiency of this technique in the elimination of edge effect, in comparison with conventional plasma nitriding. In addition, another comparative study of the phases obtained using the conventional plasma nitriding and nitriding with cathodic cage was performed. Two metallic cages were used, one made of austenitic stainless AISI 316 and other one made of AISI 1020 steel, to prove the effect of deposition in nitriding with cathodic cage. The samples which were nitrided by this new technique had shown nitriding rates, crystalline phases, and microhardness, similar to those samples which were nitrided conventionally. However, it was possible to confirm the elimination of edge effect through the characterization by optical microscopy and by microhardness test along the samples surfaces. The samples were characterized by optical microscopy, microhardness tests and X-ray diffraction. <![CDATA[<b>Synthesis and characterization of sulfonated poly(ether imide) with higher thermal stability and effect on CO<sub>2</sub>, N<sub>2</sub>, and O<sub>2</sub> permeabilities</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300025&lng=en&nrm=iso&tlng=en An experimental design in different reaction conditions was applied to modify poly(ether imide), PEI, by sulfonation using acetyl sulfate. Higher temperatures and reaction times led to higher ion exchange capacity. The thermal analysis showed that our sulfonation approach accomplished preparing sulfonated PEI maintaining the thermal stability of its parent material even for the film with highest degree of sulfonation, and assessed the effect of this change on CO2, O2 and N2 permeabilities. The permeability results pointed out that our sulfonation approach is an effective way to produce high performance engineered polymers for fuel cell electrolyte membranes and for CO2 separation from air. These results also suggest that the use of milder reactive medium at higher temperatures and for longer reaction times seems to be a more promising approach to achieve thermal stability than use more aggressive sulfonation agents. <![CDATA[<b>Marine-friendly antifouling coating based on the use of a fatty acid derivative as a pigment</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300026&lng=en&nrm=iso&tlng=en This study was devoted to examining the application of copper dodecanoate as a non-contaminant antifouling pigment due to its low copper content and fatty acid nature. For this purpose, antifouling paints with mono-component epoxy resin and rosin matrixes were formulated, and their antifouling efficiency was evaluated. Before its incorporation into the different formulations, the synthesized pigment was characterized. Immersion tests in a marine environment were carried out for 12 months to evaluate the antifouling efficiency of the developed paints; the results were compared with those from a commercial paint. The antifouling efficiency of the new epoxy formulation was found to be considerably higher than that of the rosin formulation and very similar to that of the commercial paint. Most importantly, the release of copper from the epoxy paint formulated with copper dodecanoate was 73.5% lower than that of the commercial paint, suggesting prolonged activity of the developed paint. <![CDATA[<b>Effect of ZnO addition on the structure, microstructure and dielectric and piezoelectric properties of K<sub>0.5</sub>Na<sub>0.5</sub>NbO<sub>3</sub> ceramics</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300027&lng=en&nrm=iso&tlng=en Microstructure, structure and electrical and dielectric properties of ZnO-doped K0.5Na0.5NbO3 (KNN) ceramics were investigated. Powders were obtained by the conventional solid-state method. Samples doped with 0 to 1 mol% of ZnO were sintered at 1125 °C for 2 h. Through XRD spectra, the perovskite structure was detected, in addition to small peaks corresponding to secondary phases. It was also observed that zinc changed the microstructure and grain size of KNN ceramics. The addition of 0.5 mol% of Zn2+ produced a softening effect in the ferroelectric properties of the material, and increased its final density. Conversely, the addition of 1 mol% of Zn2+ reduced the sample densification. <![CDATA[<b>Synthesis of zinc aluminate (ZnAl<sub>2</sub>O<sub>4</sub>) spinel and its application as photocatalyst</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300028&lng=en&nrm=iso&tlng=en ZnAl2O4 spinel was synthesized by co-precipitation using ammonia as precipitating agent, followed by thermal treatment at 750 ºC. The structural properties of particles were investigated by X-ray diffraction (XRD), atomic force microscopy (AFM), differential thermal analysis (DTA), and N2 adsorption/desorption isotherms (BET) techniques. The photocatalytic activity was evaluated in the degradation of organic pollutant in aqueous solution under sunlight. The results showed that the ZnAl2O4 particles exhibited a mesoporous structure, and a promising photocatalytic activity for the degradation of pollutant molecules. <![CDATA[<b>Optimization of ethanol flow rate for improved catalytic activity of Ni particles to synthesize MWCNTs using a CVD reactor</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300029&lng=en&nrm=iso&tlng=en During synthesis of MWCNTs using CVD, role of carbonaceous material and catalyst, besides other process parameters, has considerable influence on the structure and yield of pristine nanotubes. In present study, different flow rates (i.e. 10, 25, 40 and 55 sccm) of precursor ethanol were used for the synthesis of MWCNTs at 750 ºC in a CVD reactor, where nickel particles were supported on quartz as catalyst. Further, these nanotubes were characterized using XRD, SEM, TGA and Raman spectroscopy to investigate the effect of ethanol flow rate on the catalytic activity of nickel for optimum production of MWCNTs. It was observed that at different ethanol flow rates, variations in synthesis products (i.e. CNTs, amorphous carbon and carbon nanoparticles) were associated with catalytic activity. Maximum catalytic activity of nickel particles was attained by optimizing ethanol flow rate (at 25 sccm). At the optimum flow rate a maximum purity of MWCNTs (&gt;83%) was attained along with other relevant structures i.e. amorphous carbon <1.5% and SWCNT <10% balancing with retained catalytic particles. Any increase from the optimum limit caused not only defects within the CNTs' structure but also increased the impurities which were correlated with the reduction in activity of the nickel particles due to the saturation of active sites. <![CDATA[<b>Geometric effects of sustainable auxetic structures integrating the particle swarm optimization and finite element method</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300030&lng=en&nrm=iso&tlng=en The development of new materials based on industrial wastes has been the focus of much research for a sustainable world. The growing demand for tyres has been every year exacerbating environmental problems due to indiscriminate disposal in the nature, making a potentially harmful waste to public health. The incorporation of rubber particles from scrap tyres into polymeric composites has achieved high toughness and moderate mechanical properties. This work investigates the geometric effects (thickness, width and internal cell angle) of auxetic structures made of recycled rubber composites based on experimental and numerical data. The response surface models integrated with the swarm intelligence and finite element analysis were proposed in order to obtain a range of solutions that provides useful information to the user during the selection of geometric parameters for reentrant cells. The results revealed the cell thickness ranges from 39-40 mm and 5.98-6 mm, and the cell angle range from -0.01 to -0.06º maximize the ultimate strength. The same parameters were able to optimize the modulus of elasticity of rubber auxetic structures, excepting for the angle factor which must be set between -30º and 27.7º. The optimal Poisson's ratio was found when the cell angle ranged from -30º to -28.5º, cell width ranged from 5-5.6 mm and 2 mm in thickness. <![CDATA[<b>Evaluating the influence of defects on the young's modulus of carbon nanotubes using stochastic modeling</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300031&lng=en&nrm=iso&tlng=en The main goal of this research is to investigate the influence of structural defects on the mechanical properties of single-walled carbon nanotubes (CNTs). Two different types of the structural defects called Stone-Wales and vacancy defect are studied. While the former is categorized under the process-induced defect and it appears during the growth process of CNT, the later is caused when chemical functionalization is applied to CNT for fabrication carbon nanotube reinforced nanocomposite providing better bonding between CNT and surrounding resin. The number of broken C-C bonds, distributions and their orientations are all taken into account as random variables accounting for full stochastic analysis. Therefore, a computer code is provided for the stochastic modeling. The finite element (FE) model of the CNT is built using nanoscale continuum mechanics approach and then structural defects are applied randomly to the CNT. The Young's modulus of defected CNTs are obtained and compared with non-defected ones. It is revealed that the importance of vacancy defect is considerably higher than that of Stone-Wales defects implying on the drawback of chemical functionalization process. A detailed study is carried out on the topology of the defect and also continuous probability density functions of defect CNT Young's modulus are characterized. <![CDATA[<b>Effects of cellular growth on fatigue life of directionally solidified hypoeutectic Al-Fe Alloys</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300032&lng=en&nrm=iso&tlng=en Al-Fe hypoeutectic alloys are a family of casting alloys characterized by cell growth, low cost and appreciable formability. It is well known that fatigue strength is a requirement of prime importance considering the nature of load typically observed during operations involving the risers used in oil extraction. The aim of this study is to examine the influence of cell size and its intercellular phase distribution on the fatigue life (Nf) of the directionally solidified Al-0.5, 1.0 and 1.5wt% Fe alloys. A water-cooled vertical upward unidirectional solidification system was used to provide the castings. Microscopy light and SEM microscopy were used. It was found that fatigue life decreases as cell spacing (λ c) increases. Smaller cell spacing allows a homogeneous distribution of Al-Fe fibers to happen within the intercellular regions, which tends to improve the mentioned fatigue property. Hall-Petch type correlations [Nf= Nf0+A(λc -1/2)-B(λc -1); where A and B are constants] seems to be able to encompass the fatigue life variation along the Al-Fe alloys. <![CDATA[<b>Effect of Equal Channel Angular Pressing (ECAP) on microstructure and properties of Al-FeAlCr intermetallic phase composites</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300033&lng=en&nrm=iso&tlng=en An aluminium matrix composite was prepared by mixing commercial aluminium powders and 15 vol % of FeAlCr powders and consolidation by hot extrusion. The extruded composite was subjected to severe plastic deformation by equal channel angular pressing (ECAP) at room temperature and at 150°C. The extruded composite presents a uniform distribution of particles although some defects are observed such as residual pores and particle agglomerates. The particle distribution does not show a significant change due to ECAP. The extruded composite exhibits a relatively fine grain size of the order of 1-2 μm that was refined to 550 nm after three ECAP passes at room temperature by route A and to 636 nm after four passes at 150°C by route Bc. The yield stress of the composites was increased by 140 to 180% after ECAP as compared with the extruded condition. <![CDATA[<b>A novel technology for minimizing the synthesis time of nanostructured powders in planetary mills</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300034&lng=en&nrm=iso&tlng=en A key objective in processing of nanostructured powders via high energy ball milling is to minimize the synthesis time. This paper presents the application of imperialist competitive algorithm (ICA) for optimization of milling parameters in order to minimize the synthesis time of nanostructured powders in planetary mills. At first a direct relationship between the inverse of the milling time and the power of the planetary mill was established, which allows the validation of theoretical models proposed in the literature for the energy transfer in milling devices and the comparison of milling equipment efficiencies. Afterwards based on the obtained relation, eight design parameters in milling, namely, number of balls, ball diameter, vial radius, vial height, ball diameter distribution coefficient, plate spinning rate, vial spinning rate and distance between the center of the plate and the center of the vial were optimized. Using these optimized variables in milling process the energy transferred to the raw materials was maximized or in the equivalent expression the synthesis time of nanostructured powders was minimized. At the end a test case was solved to demonstrate the effectiveness and accuracy of the proposed design. Computational results showed that the proposed optimization algorithm is quite effective and powerful in optimizing the planetary mills. <![CDATA[<b>Characterization of the complex metal-clay obtained in the process of lead adsorption</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392014000300035&lng=en&nrm=iso&tlng=en This study aims to characterize the complex metal-clay formed by adsorption of lead. In this work, the bentonite clay named Fluidgel was calcined at 750 ºC and was used as adsorbent for lead removal. The characterization of this clay and complex metal-clay was carried out by X-ray diffraction (XRD), Fourier transformer infrared spectroscopy (FTIR), surface area (BET method), scanning electron microscopy (SEM) and chemical composition by energy dispersive X-ray (EDX). The removal of lead from aqueous solution was carried out in a fixed bed. Dynamic experiments were performed to evaluate the effect of flowrate on adsorption efficiency. The experiments were accomplished at room temperature, the clay adsorbent particle diameter was of 0.855 mm and the flow rate varied from 0.6 to 2 mL/min. The feed concentration of lead was about 0.24 mmol/L. Comparing the chemical compositions of the clays obtained by EDX before and after removal of the lead, it was concluded that the ion exchange process might be important to lead removal. From the semi-quantitative analysis of chemical composition in clays with and without adsorbed lead it was observed a reduction of the amount of Ca2+, K+ cations and the disappearance of Na+ cations, which was caused by cation exchange process.