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Materials Research, Volume: 16, Número: 4, Publicado: 2013
  • Facile preparation of Mn-doped CeO2 Submicrorods by composite-hydroxide-salt-mediated approach and their magnetic property Regular Articles

    Tan, Jie; Zhang, Wei; Lv, Yao-Hui; Xia, Ai-Lin

    Resumo em Inglês:

    Mn-CeO2 submicrorods have been obtained from anomalous CeO2 particles though a novel composite-hydroxide-salt-mediated (CHSM) approach. This method is based on a reaction between a metallic salt and a metallic oxide in a solution of composite-hydroxide-salt eutectic at ~225 ºC and normal atmosphere without using an organic dispersant or capping agent. The magnetic measurement of the Mn-CeO2 submicrorods exhibits an enhanced ferromagnetic property at room temperature with a remanence magnetization (Mr) of 1.4 × 10-3 emu.g-1 and coercivity (Hc) of 75 Oe. The UV-visible spectra reveal that the absorption peak of the CeO2 shifts from ultraviolet region to visible light region after being doped with Mn ions. The room temperature ferromagnetic properties and light absorption of the Mn-CeO2 submicrorods would have wide applications in spintroics and photocatalysis field.
  • Benefits of oxygen and nitrogen plasma treatment in Vero cell affinity to poly(lactide-co-glycolide acid) Regular Articles

    Esposito, Andrea Rodrigues; Kamikawa, Camila Mika; Lucchesi, Carolina; Ferreira, Betina Mara Pereira; Duek, Eliana Aparecida de Rezende

    Resumo em Inglês:

    Cell adhesion on materials surface is critical because this phenomenon occurs before other events, as cell spreading, cell migration and cell differentiation. it is commonly accepted that the adhesion of cells on solid substrate is influenced by several substratum surface properties, such as wettability, surface charge, roughness and topography. plasma technique is a convenient method for modifying surface properties of materials without affecting physical properties. in this study, poly(lactide-co-glycolide), plga, membranes were modified by oxygen and nitrogen plasma to improve polymer hydrophilicity and verify their effect on vero cells culture. the plga membranes, which were characterized by sem and contact angle, showed increased surface rugosity and narrower contact angles. cell adhesion, cytotoxicity assay, sem and cytochemistry analysis showed that plasma treatment was beneficial to cell growth by improving cell-polymer interaction. Cell adhesion on materials surface is critical because this phenomenon occurs before other events, as cell spreading, cell migration and cell differentiation. It is commonly accepted that the adhesion of cells on solid substrate is influenced by several substratum surface properties, such as wettability, surface charge, roughness and topography. Plasma technique is a convenient method for modifying surface properties of materials without affecting physical properties. In this study, poly(lactide-co-glycolide), PLGA, membranes were modified by oxygen and nitrogen plasma to improve polymer hydrophilicity and verify their effect on Vero cells culture. The PLGA membranes, which were characterized by SEM and contact angle, showed increased surface rugosity and narrower contact angles. Cell adhesion, cytotoxicity assay, SEM and cytochemistry analysis showed that plasma treatment was beneficial to cell growth by improving cell-polymer interaction.
  • Cell response of calcium phosphate based ceramics, a bone substitute material Regular Articles

    Marchi, Juliana; Ribeiro, Christiane; Bressiani, Ana Helena de Almeida; Marques, Márcia Martins

    Resumo em Inglês:

    The aim of this study was to characterize calcium phosphate ceramics with different Ca/P ratios and evaluate cell response of these materials for use as a bone substitute. Bioceramics consisting of mixtures of hydroxyapatite (HAp) and β-tricalcium phosphate (β-TCP) powders in different proportions were pressed and sintered. The physical and chemical properties of these bioceramics were then characterized. Characterization of the biological properties of these materials was based on analysis of cell response using cultured fibroblasts. The number of cells attached to the samples was counted from SEM images of samples exposed to cell culture solution for different periods. These data were compared by analysis of variance (ANOVA) complemented by the Tukey's test. The TCP sample had higher surface roughness and lower density. The adherence and growth of FMM1 cells on samples from all groups was studied. Even though the different calcium based ceramics exhibited properties which made them suitable as bone substitutes, those with higher levels of β-TCP revealed improved cell growth on their surfaces. These observations indicated two-phase calcium phosphate based materials with a β-TCP surface layer to be a promising bone substitute.
  • Viscoelastic behavior of multiwalled carbon nanotubes into phenolic resin Regular Articles

    Botelho, Edson Cocchieri; Costa, Michelle Leali; Braga, Carlos Isidoro; Burkhart, Thomas; Lauke, Bernd

    Resumo em Inglês:

    Nanostructured polymer composites have opened up new perspectives for multi-functional materials. In particular, carbon nanotubes (CNTs) have the potential applications in order to improve mechanical and electrical performance in composites with aerospace application. This study focuses on the viscoelastic evaluation of phenolic resin reinforced carbon nanotubes, processed by using two techniques: aqueous-surfactant solution and three roll calender (TRC) process. According to our results a relative small amount of CNTs in a phenolic resin matrix is capable of enhancing the viscoelastic properties significantly and to modify the thermal stability. Also has been observed that when is used TRC process, the incorporation and distribution of CNT into phenolic resin is more effective when compared with aqueous solution dispersion process
  • Application of ANFIS for modeling of microhardness of high strength low alloy (HSLA) steels in continuous cooling Regular Articles

    Khalaj, Gholamreza; Nazari, Ali; Livary, Akbar Karimi

    Resumo em Inglês:

    The paper presents some results of the research connected with the development of new approach based on the Adaptive Network-based Fuzzy Inference Systems (ANFIS) of predicting the Vickers microhardness of the phase constituents occurring in five steel samples after continuous cooling. The independent variables in the model are chemical compositions, initial austenite grain size and cooling rate over the temperature range of the occurrence of phase transformations. To construct these models, 114 different experimental data were gathered from the literature. The data used in the ANFIS model is arranged in a format of twelve input parameters that cover the chemical compositions, initial austenite grain size and cooling rate, and output parameter which is Vickers microhardness. In this model, the training and testing results in the ANFIS systems have shown strong potential for prediction of effects of chemical compositions and heat treatments on hardness of microalloyed steels.
  • Preparation of refractory calcium aluminate cement using the sonochemical process Regular Articles

    Lourenço, Rafaela Roberta; Angélica, Rômulo Simões; Rodrigues, José de Anchieta

    Resumo em Inglês:

    Calcium aluminate cements (CAC) were prepared using the sonochemical process, followed by heat treatment. A study was made of the action of ultrasonic waves and the influence of thermal treatment conditions on two initial molar compositions of 1:1 and 1:2 of calcia:alumina. The aqueous suspension containing the raw materials (A-50 alumina and CaO) was subjected to an ultrasonic bath, followed by drying and burning at 1000, 1200 and 1300 ºC. These cements were characterized by SEM, XRD and the mechanical strength was evaluated by splitting tensile tests, using commercial cement as a reference. Furthermore, the phases were semi-quantified using the Rietveld method. The results show that hydration and sonochemical action increased the reactivity of the raw materials during firing and that phase formation is dependent on the thermal treatment conditions. The CAC cements were obtained at temperatures at least 200 ºC lower than those used in conventional methods, indicating the potential of this route of synthesis.
  • A dilatometric study of the phase transformations in 300 and 350 maraging steels during continuous heating rates Regular Articles

    Carvalho, Leandro Gomes de; Andrade, Margareth Spangler; Plaut, Ronald Lesley; Souza, Fabrício Mendes; Padilha, Angelo Fernando

    Resumo em Inglês:

    The influences of the chemical composition and heating rate have been studied in 300 and 350 maraging steels using dilatometry. For these tests, heating was carried out with heating rates of 1, 10 and 28 °C/s. The results have shown that the precipitation mechanism for both materials in the studied range is by lattice diffusion. Furthermore, Co and Ti contents influence strongly the precipitation. The lattice diffusion mechanism in the martensite reversion is influenced by Ni and Co contents and heating rate. For small heating rates ( ~1 °C/s) this mechanism prevails in the 300 maraging steel while for the 350 maraging steel has a minor importance. The mechanism of martensite reversion for 350 maraging steel in the studied range is mainly by shear mechanism. For higher heating rates (~28 ºC/s) the shear mechanism prevails in both maraging steels.
  • Study on the adsorption of heavy metal ions from aqueous solution on modified SBA-15 Regular Articles

    Giraldo, Liliana; Moreno-Piraján, Juan Carlos

    Resumo em Inglês:

    Amino-functionalized SBA-15 mesoporous silica was prepared, characterized, and used as an adsorbent for heavy metal ions. The organic - inorganic hybrid material was obtained by a grafting procedure using SBA-15 silica with 3-aminopropyl-triethoxysilane and bis(2,4,4-trimethylpentyl) phosphinic acid (Cyanex 272), respectively. The structure and physicochemical properties of the materials were characterized by means of elemental analysis, X-ray diffraction (XRD), nitrogen adsorption - desorption, thermogravimetric analysis, FTIR spectroscopy and immersion calorimetry. The organic functional groups were successfully grafted onto the SBA-15 surface and the ordering of the support was not affected by the chemical modification. The behavior of the grafted solids was investigated for the adsorption of heavy metal ions from aqueous solutions. The hybrid materials showed high adsorption capacity and high selectivity for zinc ions. Other ions, such as cooper and cobalt were absorbed by the modified SBA-15 material.
  • Studies on Cross-linking of succinic acid with chitosan/collagen Regular Articles

    Mitra, Tapas; Sailakshmi, G.; Gnanamani, A.; Mandal, A. B.

    Resumo em Inglês:

    The present study summarizes the cross-linking property of succinic acid with chitosan /collagen. In detail, the chemistry behind the cross-linking and the improvement in mechanical and thermal properties of the cross-linked material were discussed with suitable instruments and bioinformatics tools. The concentration of succinic acid with reference to the chosen polymers was optimized. A 3D scaffold prepared using an optimized concentration of succinic acid (0.2% (w/v)) with chitosan (1.0% (w/v)) and similarly with collagen (0.5% (w/v)), was subjected to surface morphology, FT-IR analysis, tensile strength assessment, thermal stability and biocompatibility. Results revealed, cross-linking with succinic acid impart appreciable mechanical strength to the scaffold material. In silico analysis suggested the prevalence of non-covalent interactions, which played a crucial role in improving the mechanical and thermal properties of the cross-linked scaffold. The resultant 3D scaffold may find application as wound dressing material, as an implant in clinical applications and as a tissue engineering material.
  • Effect of cage configuration in structural and optical properties of tin films grown by cathodic cage discharge Regular Articles

    Daudt, Natália de Freitas; Barbosa, Júlio César Pereira; Macêdo, Marina de Oliveira Cardoso; Pereira, Marcelo Barbalho; Alves Junior, Clodomiro

    Resumo em Inglês:

    Cathodic cage discharge was developed recently in order to eliminate phenomena as edge effect and overheating, which occurs during conventional processes. In this study, the effect of cage configuration in active species during the deposition process and optical properties of TiN film were studied. TiN compound was chosen because its optical properties are very sensitive to slight variations in microstructure and film thickness, becoming a good monitoring tool in fabrication process control. Cages were made of titanium and have different holes numbers and holes diameter. Electrical efficiency of the system and optical properties of TiN films were strongly influenced by experimental conditions. It was found that with more holes at the top of cage, deposition rate and crystallinity were higher, if compared to cages with a small number of holes at the top. On the other hand, the opposite behavior was observed when more holes were located at the sidewall of cage.
  • Normalizing effect on fatigue crack propagation at the heat-affected zone of AISI 4140 steel shielded metal arc weldings Regular Articles

    Vargas-Arista, B.; Teran-Guillen, J.; Solis, J.; García-Cerecero, G.; Martínez-Madrid, M.

    Resumo em Inglês:

    The fractography and mechanical behaviour of fatigue crack propagation in the heat-affected zone (HAZ) of AISI 4140 steel welded using the shielded metal arc process was analysed. Different austenitic grain size was obtained by normalizing performed at 1200 °C for 5 and 10 hours after welding. Three point bending fatigue tests on pre-cracked specimens along the HAZ revealed that coarse grains promoted an increase in fatigue crack growth rate, hence causing a reduction in both fracture toughness and critical crack length, and a transgranular brittle final fracture with an area fraction of dimple zones connecting cleavage facets. A fractographic analysis proved that as the normalizing time increased the crack length decreased. The increase in the river patterns on the fatigue crack propagation in zone II was also evidenced and final brittle fracture because of transgranular quasicleavage was observed. Larger grains induced a deterioration of the fatigue resistance of the HAZ.
  • Simultaneous incorporation of magnesium and carbonate in apatite: effect on physico-chemical properties Regular Articles

    Sader, Marcia S.; Lewis, Kanthi; Soares, Gloria A.; LeGeros, Racquel Z.

    Resumo em Inglês:

    Synthetic apatites are widely used both in the dental and the orthopaedic fields due to their similarity in composition with the inorganic phase of hard tissues. Biologic apatites are not pure hydroxyapatite (HA), but are calcium-deficient apatites with magnesium and carbonate as minor but important substituents. The aim of the present study was to produce a more soluble biomaterial through the simultaneous substitution of magnesium and carbonate in the apatite structure to accelerate the degradation time in the body. The physico-chemical and dissolution properties of unsintered magnesium and carbonate-substituted apatite (MCAp) with similar Mg/Ca molar ratio (0.03) and varying C/P molar ratio were evaluated. The resultant powders were characterised using several techniques, such as FTIR, TGA, XRD, ICP and SEM, while the release of calcium ions in a pH 6 solution was monitored using a Ca-ion selective electrode. The results showed a decrease of crystallite size and an increase in the release of calcium to the medium as the carbonate content in the samples increased.
  • The improved arrhenius model with variable parameters of flow behavior characterizing for the as-cast AZ80 magnesium alloy Regular Articles

    Quan, Guo-zheng; Shi, Yu; Yu, Chun-tang; Zhou, Jie

    Resumo em Inglês:

    In order to study the hot working behaviour of as-cast AZ80 magnesium alloy, a series of isothermal upsetting tests with height reduction of 60% were performed at the temperature range of 523-673 K and the strain rate range of 0.01-10 s-1 on a servo-hydraulic Gleeble-1500 machine simulator. Based on the regression analysis for Arrhenius type equation of flow stress, the activation energy of deformation was determined to be Q = 168.6606 KJ·mol-1, and material constants , n and α in the equation also were calculated respectively to predict the peak stress during hot deformation. A 7th order polynomial was used to represent the influence of strain on these parameters (i.e Q, ln, n and α). The Arrhenius equation was further developed by taking account of the effect of strain on the flow stress to describe the flow behavior during the whole experimental temperature and strain rate range. Then comparison between the predicted results and test results shows that the correlation coefficient and average absolute relative error is 0.99 and 6.63%, respectively. The flow stress predicted by developed equation can give an accurate and precise description of the flow behaviour for AZ80 magnesium alloy.
  • FTIR study of the relation, between extra-framework aluminum species and the adsorbed molecular water, and its effect on the acidity in ZSM-5 steamed zeolite Regular Articles

    Isernia, Luis Fioravanti

    Resumo em Inglês:

    The infrared spectroscopy study of zeolite samples, obtained by steam treatment at 560‑960 °C of the ZSM‑5 catalyst (framework Si/Al ratio of 13), suggests an association between adsorbed molecular water and extra‑framework aluminum hydroxyls generated after treatment. Moreover, infrared spectroscopy of adsorbed pyridine shows the reduction of the densities of Brönsted and Lewis sites, when treatment temperature rises, with contradicts the frequently accepted mechanism of the transformation of two bridged Si‑OH‑Al groups for each Lewis site generated. The gradual conversion of the octahedral extra-framework aluminum (Lewis‑associated) in polymeric species with low acidity is the most probable cause of this behavior. On the other hand, the apparent decline of the acid Brönsted strength, with the increase in the temperature of the hydrothermal treatment, has two possible causes: a) the decreasing accessibility, of the pyridine molecular probe to bridged Si-OH-Al groups with the strongest Brönsted acidity, inside the channels, and b) the gradual transformation of these groups into extra framework species of weak acidity.
  • Effects of austenitization temperature on the microstructure of 15BCr30 and PL22 boron steels Regular Articles

    Suski, C. A.; Oliveira, C.A.S de

    Resumo em Inglês:

    This paper studies boron precipitation and segregation at austenitic grain boundaries for low carbon boron steels types: PL22 and 15BCr30. The following parameters were evaluated: percentage of martensite/bainite, size and nucleation sites of austenitic grains and precipitates sizes. Three austenitization temperatures were studied (870, 1050 and 1200 °C). The highest martensite percentage occurred for 1050 °C. Iron-borocarbides were detected at grain boundaries for all tested temperatures. At 870 °C the coarse iron-borocarbides are due to non-solubility and coalescence. The highest martensite percentage at 1050 °C is caused by the discrete precipitation of iron-borocarbides at austenitic grains boundaries. The discrete precipitation was due to the low non-equilibrium segregation of boron at grain boundaries. The low non-equilibrium segregation and the small grain size at 1050 °C reduce the total boron concentration at grain boundaries.
  • Determination of crystallization kinetics parameters of a Li1.5Al0.5Ge1.5(PO4)3 (LAGP) glass by differential scanning calorimetry Regular Articles

    Rodrigues, A. M.; Narváez-Semanate, J. L.; Cabral, A. A.; Rodrigues, A. C. M.

    Resumo em Inglês:

    Crystallization kinetics parameters of a stoichiometric glass with the composition Li1.5Al0.5Ge1.5(PO4)3 were investigated by subjecting parallelepipedonal samples (3 × 3 × 1.5 mm) to heat treatment in a differential scanning calorimeter at different heating rates (3, 5, 8 and 10 °C/min). The data were analyzed using Ligero's and Kissinger's methods to determine the activation energy (E) of crystallization, which yielded, respectively, E = 415 ± 37 kJ/mol and 378 ± 19 kJ/mol. Ligero's method was also employed to calculate the Avrami coefficient (n), which was found to be n = 3.0. A second set of samples were heat-treated in a tubular furnace at temperatures above the glass transition temperature, Tg, to induce crystallization. The X-ray diffraction analysis of these samples indicated the presence of LiGe2(PO4)3 which displays a NASICON-type structure. An analysis by optical microscopy revealed the presence of spheric crystals located primarily in the volume, in agreement with the crystallization mechanism predicted by the Avrami coefficient.
  • Microstructural and topographic characterization of concrete protected by acrylic paint Regular Articles

    Ribeiro, Carmen Couto; Pinto, Joana Darc da Silva; Godoy, G. Cristina; Buono, Vicente Tadeu Lopes; Starling, Tadeu

    Resumo em Inglês:

    Concrete structures must be designed and constructed so as to resist the conditions established in the project design and suffer no deterioration for many years. In highly aggressive environments, in addition to the minimum layer covering the framework, the concrete must receive a protective coating. In this work, the efficiency of acrylic paint as a protective coating, while the concrete was placed in an aggressive environment, was assessed utilizing a profilometric and microstructural characterization. The concrete was dosed using the ACI - American Concrete Institute method. The specimens were prepared with 370 kg.m-3 of cement and the water-binder ratio of 0.50 corresponds to the value established in NBR6118¹ types for concrete subjected to highly aggressive environments. With the use of profilometry, 3D topographical images and surface roughness parameters were generated, which allowed for the identification of the degradation process and the minimization of the effect of this attack on concrete that had received surface protection. The topographic roughness parameters, as well as the images and chemical components identified using SEM/EDS, made it possible to identify the process of deterioration of the concrete under acid attack and to minimize such effect in the coated concrete. The methodology adopted demonstrates that the application of acrylic paint as a protective coating for concrete in an aggressive environment minimizes its surface degradation and increases its durability.
  • Synthesis and characterisation of polymeric nanofibers poly (vinyl alcohol) and poly (vinyl alcohol)/silica using indigenous electrospinning set up Regular Articles

    Sasipriya, K.; Suriyaprabha, R.; Prabu, P.; Rajendran, V.

    Resumo em Inglês:

    Indigenous design and fabrication horizontal of electrospinning set up was developed to facilitate with double drum conveyor belt system to make ease in harvesting nanofibers rapidly. As a bench mark study, organic-inorganic nanofiber composite was synthesised employing our indigenous electrospinning set up. The aqueous solution of poly (vinyl alcohol) and poly (vinyl alcohol)/silica sol were employed to produce nanofiber mats in order to vary the experimental parameters such as voltage, solvent effect and the effect of catalyst. The synthesised pure electro spun poly (vinyl alcohol) and poly (vinyl alcohol)/silica sol fibers were characterized by Scanning electron microscopy (SEM), Atomic force microscopy (AFM) and Fourier transform infra red spectroscopy (FTIR). According to the results, the fine polymeric nanofibers were achieved in the size range of 100-500 nm for pure poly (vinyl alcohol) fiber and 100-700 nm for polyvinyl alcohol/silica and the constitution of silica in rendering better fiber mats with this double drum set up.
  • Photo-Induced conductivity of heterojunction GaAs/Rare-Earth doped SnO2 Regular Articles

    Bueno, Cristina de Freitas; Machado, Diego Henrique de Oliveira; Pineiz, Tatiane de Fátima; Scalvi, Luis Vicente de Andrade

    Resumo em Inglês:

    Rare-earth doped (Eu3+ or Ce3+) thin layers of tin dioxide (SnO2) are deposited by the sol-gel-dip-coating technique, along with gallium arsenide (GaAs) films, deposited by the resistive evaporation technique. The as-built heterojunction has potential application in optoelectronic devices, because it may combine the emission from the rare-earth-doped transparent oxide, with a high mobility semiconductor. Trivalent rare-earth-doped SnO2 presents very efficient emission in a wide wavelength range, including red (in the case of Eu3+) or blue (Ce3+). The advantage of this structure is the possibility of separation of the rare-earth emission centers, from the electron scattering, leading to an indicated combination for electroluminescence. Electrical characterization of the heterojunction SnO2:Eu/GaAs shows a significant conductivity increase when compared to the conductivity of the individual films. Monochromatic light excitation shows up the role of the most external layer, which may act as a shield (top GaAs), or an ultraviolet light absorber sink (top RE-doped SnO2). The observed improvement on the electrical transport properties is probably related to the formation of short conduction channels in the semiconductors junction with two-dimensional electron gas (2DEG) behavior, which are evaluated by excitation with distinct monochromatic light sources, where the samples are deposited by varying the order of layer deposition.
  • Nanofibers obtained by electrospinning of BaTiO3 particles dispersed in polyvinyl alcohol and ethylcellulose Regular Articles

    Ávila, Humar A.; Reboredo, María M.; Castro, Miriam; Parra, Rodrigo

    Resumo em Inglês:

    Barium titanate particles (100-300 nm) synthesized by hydrothermal method were dispersed in both polyvinyl alcohol (PVA) and ethylcellulose (EC) solutions. These suspensions were processed by electrospinning. When no particles were added, homogeneous polymeric nanofibers were obtained. Under certain conditions, polymeric suspensions of barium titanate particles were electrospun generating polymeric fibers with BT particles. The effect of a surfactant was also assessed over the formation of nanofibers. The BaTiO3 particles synthesized by hydrothermal method were characterized by X-Ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and Raman spectroscopy. Fibers were characterized by scanning electron microscopy (SEM).
  • Thermal stability and microstructure characterization of MgAl2O4 nanoparticles synthesized by reverse microemulsion method Regular Articles

    Fu, Ping; Lu, Wenzhong; Lei, Wen; Wu, Ke; Xu, Yong; Wu, Jiamin

    Resumo em Inglês:

    Magnesium aluminate (MgAl2O4) spinel nanoparticles were synthesized by reverse microemulsion process in cyclohexane by using two kinds of surfactants, n-amyl alcohol as cosurfactant and mixture of aluminic/magnesic salt aqueous solution as basic reagents. The effects of surfactant types and titration methods on the morphologies and sizes of the MgAl2O4 nanoparticles were characterized by TEM, TGA-DTA, XRD, HR-TEM and FT-IR. TEM images show that the particles prepared by forward-titration method with SPAN-80/Triton X-100 compound emulsifier have uniform spherical shape and good monodispersity with an average size of 9.5 nm. However, the average size of the particles prepared by reverse-titration method was about 10 nm and some particles have irregular platelike appearance. The products prepared with NP-40 surfactant and forward-titration method were agglomerated with an average size of 13 nm. TGA and XRD results show that the reverse microemulsion method has dramatically lowered the calcination temperature of MgAl2O4 with a degree of 700 °C, and the precursor can transform to single spinel phase at 900 °C.
  • Study of indium nitride and indium oxynitride band gaps Regular Articles

    Sparvoli, M.; Mansano, R. D.; Chubaci, J. F. D.

    Resumo em Inglês:

    This work shows the study of the optical band gap of indium oxynitride (InNO) and indium nitride (InN) deposited by magnetron reactive sputtering. InNO shows multi-functionality in electrical and photonic applications, transparency in visible range, wide band gap, high resistivity and low leakage current. The deposition processes were performed in a magnetron sputtering system using a four-inches pure In (99.999%) target and nitrogen and oxygen as plasma gases. The pressure was kept constant at 1.33 Pa and the RF power (13.56 MHz) constant at 250 W. Three-inches diameter silicon wafer with 370 micrometer thickness and resistivity in the range of 10 ohm-centimeter was used as substrate. The thin films were analyzed by UV-Vis-NIR reflectance, photoluminescence (PL) and Hall Effect. The band gap was obtained from Tauc analysis of the reflectance spectra and photoluminescence. The band gap was evaluated for both films: for InNO the value was 2.48 eV and for InN, 1.52 eV. The relative quantities obtained from RBS spectra analysis in InNO sample are 48% O, 12% N, 40% In and in InN sample are 8% O, 65% N, 27% In.
  • Effect of the mechanical properties and mode loading on the mechanical behaviour of weldment: a numerical analysis Regular Articles

    Miloud, Meddah Hadj; Bahri, Ould chikh; Ali, Benhamena; Mohamed, Benguediab; Benattou, Bouchouicha

    Resumo em Inglês:

    Welding is used to realize permanent assembly in mechanical structures to assure the continuity of the parts to be assembled contrary to the other assembly techniques which have physical or chemical discontinuities. Generally, crack evolution depends on several intrinsic and extrinsic parameters of material. The aim of this work is to analyse the severity of crack defects on the mechanical behaviour of Welded joints. The cracks are considered located in the weld metal. The J-integral method was used to analyse the fracture behaviour of these structures by the two-dimensional finite element method using Cast3M code. The effect of the mechanical properties, the mismatching and the crack size on the J-integral values was highlighted. A good correlation between the FEM simulations and the literature analysis results was observed. We note that the loading mode affects directly the J-integral value and consequently on the mechanical behaviour of the weldment.
  • Castor oil and commercial thermoplastic polyurethane membranes modified with polyaniline: a comparative study Regular Articles

    Almeida Júnior, José Humberto Santos; Bertuol, Daniel Assumpção; Meneguzzi, Alvaro; Ferreira, Carlos Arthur; Amado, Franco Dani Rico

    Resumo em Inglês:

    The study of conducting polymeric membranes is decisive in some areas, as in fuel cells and electrodialysis. This work aims the study of membranes using conventional and conductive polymers blends. Two types of polyurethane were used as conventional polymers, commercial thermoplastic polyurethane and polyurethane synthesized from castor oil and 4-4-dicyclohexylmethane isocyanate. Two kinds of conducting polymers were used, polyaniline doped with organic acid and a self doped polyaniline. The polymers and the membranes were characterized by electrical conductivity, Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), dynamic mechanical analysis (DMA) and scanning electron microscopy (SEM). The synthesis of the membranes produced was proper, featuring a complete reaction, analyzed by FTIR. The membranes also showed good mechanical properties and thermal stability (≈ 220 °C). Among the membranes studied, the polyaniline doped with p-toluenesulphonic acid obtained higher thermal and viscoelastic properties. Thus they can be used in separation techniques using membranes.
  • Analysis of parameters effects on crack breathing and propagation in shaft of rotor dynamic systems Regular Articles

    Serier, M.; Lousdad, A.; Refassi, K.; Megueni, A.

    Resumo em Inglês:

    In this paper the design of experiment method is used to investigate and explain the effects of the rotor parameters on crack breathing and propagation in the shaft. Three factors are considered which have an influence on the behavior and the propagation of the crack: the rotational speed, the length of the rotor and the diameter of the shaft. The elaborated mathematical model allows determining the effects and interaction of speed, diameter and length on crack breathing mechanism.The model also determines the optimal values of the parameters to achieve high performance.
  • Characterization of the Al-3wt.%Si alloy in unsteady-state horizontal directional solidification Regular Articles

    Carvalho, Diego Brito; Guimarães, Emanuelle Casseb; Moreira, Antonio Luciano; Moutinho, Daniel Joaquim; Dias Filho, José Marcelino; Rocha, Otávio Lima da

    Resumo em Inglês:

    The main purpose of this paper is to investigate both the columnar to equiaxed transition and primary dendritic arm spacings of Al-3wt.%Si alloy during the horizontal directional solidification. The transient heat transfer coefficient at the metal-mold interface is calculated based on comparisons between the experimental thermal profiles in castings and the simulations provided by a finite difference heat flow program. Simulated curve of the interfacial heat transfer coefficient was used in another numerical solidification model to determine theoretical values of tip growth rates, cooling rates and thermal gradients that are associated with both columnar to equiaxed transition and primary dendritic arm spacings. A good agreement was observed between the experimental values of these thermal variables and those numerically simulated for the alloy examined. A comparative analysis is carried out between the experimental data of this work and theoretical models from the literature that have been proposed to predict the primary dendritic spacings. In this context, this study may contribute to the understanding of how to manage solidification operational parameters aiming at designing the microstructure of Al-Si alloys.
  • Metallurgical response of an AISI 4140 steel to different plasma nitriding gas mixtures Regular Articles

    Skonieski, Adão Felipe Oliveira; Santos, Giovanni Rocha dos; Hirsch, Thomas Karl; Rocha, Alexandre da Silva

    Resumo em Inglês:

    Plasma nitriding is a surface modification process that uses glow discharge to diffuse nitrogen atoms into the metallic matrix of different materials. Among the many possible parameters of the process, the gas mixture composition plays an important role, as it impacts directly the formed layer's microstructure. In this work an AISI 4140 steel was plasma nitrided under five different gas compositions. The plasma nitriding samples were characterized using optical and scanning electron microscopy, microhardness test, X-ray diffraction and GDOES. The results showed that there are significant microstructural and morphological differences on the formed layers depending on the quantity of nitrogen and methane added to the plasma nitriding atmosphere. Thicknesses of 10, 5 and 2.5 µm were obtained when the nitrogen content of the gas mixtures were varied. The possibility to obtain a compound layer formed mainly by γ'-Fe4N nitrides was also shown. For all studied plasma nitriding conditions, the presence of a compound layer was recognized as being the responsible to hinder the decarburization on the steel surface. The highest value of surface hardness - 1277HV - were measured in the sample which were nitrided with 3vol.% of CH4.
  • Inorganic-organic hybrids originating from organosilane anchored onto leached vermiculite Regular Articles

    Alves, Ana P. M.; Fonseca, Maria G.; Wanderley, Albaneide Fernandes

    Resumo em Inglês:

    The reactivity of clay minerals leached in grafting reactions was investigated. Precursor solids were prepared by treating the sodium vermiculites with nitric acid solutions at several concentrations. The lixiviation produced the restructured porous solids with surface area over a wide range, varying from 133 to 673 m² g- 1. The sodium and lixiviated vermiculites reacted covalently with silylating agent, 3-aminopropyltrimethoxysilane, to attach this agent onto the inorganic surface, through the free available silanols. The products were characterized by CNH elemental analysis, infrared spectroscopy, X-ray diffraction, nuclear magnetic resonance in the solid state for carbon and silicon. CHN data expressed by significant contents of anchored organic chains, up to 2.14 mmol g- 1, as the degree of leaching was increased. The success of this investigation is directly related to the leaching of the natural vermiculite, which is strongly influenced by the reactivity of the abundant original source.
  • Hardness and degree of conversion of dental restorative composites based on an organic-inorganic hybrid Regular Articles

    Venter, Sandro Aurélio de Souza; Fávaro, Silvia Luciana; Radovanovic, Eduardo; Girotto, Emerson Marcelo

    Resumo em Inglês:

    This paper presents a factorial design (mixture design) used to analyze the hardness and degree of monomer conversion into composites containing conventional monomers and an organic-inorganic hybrid polymer-based methacryloyloxypropyl trimethoxysilane (MEMO). For this purpose, resins (composites with SiO2) were formulated with the hybrid polymer (polycondensed, pMEMO), and two conventional monomers used in dentistry, bisphenol-A dimethacrylate (Bis-GMA) and triethyleneglycol dimethacrylate (TEGDMA). The resins were characterized through the degree of monomer conversion and Vickers hardness, and the pMEMO by means of FTIR and ¹H NMR. The results showed an increase in hardness for resins containing the hybrid material relative to the resins containing only conventional monomers. The mathematical model adjusted to the experimental data yielded an optimized formulation, which presented a higher hardness value (48.88 HV).
  • Treatments of non-wood plant fibres used as reinforcement in composite materials Regular Articles

    Arsène, Marie-Ange; Bilba, Ketty; Savastano Junior, Holmer; Ghavami, Khosrow

    Resumo em Inglês:

    This paper presents a summary of the knowledge on fibres and pulps of non wood tropical plants used as reinforcement in cementitious composites accumulated during the recent years by Guadeloupean and Brazilian teams participating in collaborative work. Vegetable fibres represent a good alternative as non-conventional materials for the construction of ecological and sustainable buildings. The use of such renewable resources contributes to the development of sustainable technologies. The main objective of the paper is to emphasize the use of agricultural wastes in the production of cement based composites. The botanical, chemical, physical, morphological and mechanical properties of fibres from various plants are described. The effects of different treatments on physical, chemical and mechanical properties of fibres are presented. The most effective treatments in influencing the mechanical and physical properties are pyrolysis and alkaline ones, according to the type of plant. The final choice will have to consider fibre availability, and treatment costs.
  • The increase of surface area of a Brazilian palygorskite clay activated with sulfuric acid solutions using a factorial design Regular Articles

    Oliveira, R. N.; Acchar, W.; Soares, G. D. A.; Barreto, L. S.

    Resumo em Inglês:

    Palygorskite is fibrous clay in which the structural tetrahedral and octahedral layers are organized in a way that structural channels are formed, leading to high surface area. However, impurities inside the channels and aggregated ones considerably reduce the available area. In order to increase the surface area, an activation treatment can be considered useful. The goal of this work is the activation of palygorskite from Guadalupe, Piauí, via sulfuric acid treatment using a two-level factorial design. The influence of three parameters (solution molarity, temperature and time) on BET surface area was determined. Moreover, samples were characterized via X-ray diffraction (XRD) and fluorescence (XRF), Fourier-transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM). The largest surface area (282 m²/g) without considerable changes in clay structure and morphology was found in a sample treated with 5M H2SO4 at 70°C for 1h. The main parameters that favored the improvement of the surface area were the solution's molarity, temperature and their interaction.
  • Effect of carbon dioxide and temperature on passive film parametersof superduplex stainless steel Regular Articles

    Costa, Emandro Vieira da; Mesquita, Thiago José; Ferreira, Ariane; Nogueira, Ricardo Pereira; Bastos, Ivan Napoleão

    Resumo em Inglês:

    Superduplex stainless steel has been frequently employed in new sites of Brazilian Pre-Salt. In these environments, chloride concentration, temperature and carbon dioxide are normally present in higher levels than those at sea water at room temperature. In these conditions, it is expected that the passive films of stainless steel also show modifications. To better understand such modifications, samples of superduplex stainless steel UNS S32750 were submitted to electrochemical impedance measurements in brine media, at two temperatures and under presence/absence of carbon dioxide. The electrochemical impedance results were initially tested using the Kramers-Kronig transform and subsequently fitted by equivalent circuit employing constant phase elements - CPE. Moreover, to quantify the effect of each factor (temperature, chloride, carbon dioxide and microstructure) on the equivalent circuit, their parameters were tested applying statistical analysis. Significant effect of carbon dioxide and temperature was found on related parameters of passive film for heat-treated samples.
  • Studies on the properties of cdS films deposited from pH-controlled growth solutions Regular Articles

    Ortuño-López, M.B.; Ochoa-Landín, R.; Sandoval-Paz, M.G.; Sotelo-Lerma, M.; Flores-Acosta, M.; Ramírez-Bon, R.

    Resumo em Inglês:

    In this work we have studied the properties of CdS films obtained by the chemical bath deposition technique. We studied the influence of pH control of the reaction solution on the structural and optical properties of chemically deposited CdS films. For this, we deposited two sets of CdS films on glass substrates using two different reaction solutions. The main difference between the solutions was that one included the use of a pH-10 NH4OH/NH4Cl controller solution or buffer, which produces a more uniform pH of the reaction solution during the film-growth process. Using each reaction solution, five CdS films were deposited at 80 °C, varying the deposition time from 15 to 120 minutes. The structural and optical properties of both sets of films were determined by X-ray diffraction and by absorption, transmission and reflection spectroscopy. The differences in the properties of the films were analyzed in terms of pH control.
  • Analysis of the transformations temperatures of helicoidal Ti-Ni actuators using computational numerical methods Regular Articles

    Oliveira, Carlos Augusto do N.; Villa, Alvaro Antonio Ochoa; Gonzalez, Cezar Henrique; Guimarães, Pablo Batista; Ferreira, Rodrigo José; Urtiga Filho, Severino Leopoldino; Silva, Niedson José da; Rocha, José Orlando Silveira

    Resumo em Inglês:

    The development of shape memory actuators has enabled noteworthy applications in the mechanical engineering, robotics, aerospace, and oil industries and in medicine. These applications have been targeted on miniaturization and taking full advantage of spaces. This article analyses a Ti-Ni shape memory actuator used as part of a flow control system. A Ti-Ni spring actuator is subjected to thermomechanical training and parameters such as transformation temperature, thermal hysteresis and shape memory effect performance were investigated. These parameters were important for understanding the behavior of the actuator related to martensitic phase transformation during the heating and cooling cycles which it undergoes when in service. The multiple regression methodology was used as a computational tool for analysing data in order to simulate and predict the results for stress and cycles where the experimental data was not developed. The results obtained using the training cycles enable actuators to be characterized and the numerical simulation to be validated.
  • In situ polymerized wood polymer composite: effect of additives and nanoclay on the thermal, mechanical properties Regular Articles

    Devi, Rashmi R; Maji, Tarun K

    Resumo em Inglês:

    This study concerns the preparation and characterization of wood polymer nanocomposites based on impregnation of styrene acrylonitrile co-polymer-nanoclay intercalating system in presence of glycidyl methacrylate (GMA), a cross linking agent, and vinyl trichloro silane (VTCS) as additives into Simul (Bombex ceiba, L.), a soft wood. The effect of nanoclay and VTCS on the properties of the resultant wood polymer nanocomposites (WPNC) has been evaluated. FTIR spectroscopy shows the interaction among wood, polymers, GMA, nanoclay and VTCS. The penetration of polymer and nanoclay into the wood cell wall is supported by SEM study. The distribution of nanoclay in the SAN polymer matrix present within the wood cell wall has been evidenced by TEM study. TGA results show an improvement in the thermostability of the resultant composites. The inclusion of VTCS enhances the self extinguishing behaviour of the WPNC as revealed by limiting oxygen index (LOI) test. Due to treatment, the resultant WPNC exhibits an improvement in all the properties like water repellancy, dimensional stability, hardness, flexural, tensile and thermal stability compared to untreated wood.
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