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Materials Research, Volume: 10, Número: 2, Publicado: 2007
  • Materials Research - Ibero-american Journal of Materials: judicious, fair and educative!

    Zanotto, Edgar Dutra
  • On the prediction of fatigue crack retardation using Wheeler and Willenborg models Regular Articles

    Pereira, Marcos Venicius Soares; Darwish, Fathi Aref Ibrahim; Camarão, Arnaldo Freitas; Motta, Sérgio Henrique

    Resumo em Inglês:

    The aim of this work is to evaluate the applicability of the Wheeler and Willenborg models to predicting fatigue crack growth retardation in a flash welded structural steel subjected to a single overload during constant amplitude (CA) fatigue crack propagation test. Compact tension specimens, in different microstructural conditions, were subjected to a single overload at a given crack length during CA fatigue loading and crack growth rate da/dN vs. the stress intensity factor range deltaK was monitored, evidencing the retardation in crack propagation over an interval of crack length. The size of the delay zone as well as the number of the delay cycles were predicted by both the Wheeler and Willenborg models and then compared with the experimental data. Finally, the results are presented and discussed focusing on the comparison between the predictions made by the two models in the light of the experimental data.
  • Development of graphite-polymer composites as electrode materials Regular Articles

    Calixto, Carolina Maria Fioramonti; Mendes, Renata Kelly; Oliveira, Aline Carlos de; Ramos, Luiz Antonio; Cervini, Priscila; Cavalheiro, Éder Tadeu Gomes

    Resumo em Inglês:

    Graphite powder was mixed to polyurethane, silicon rubber and Araldite® (epoxy) in order to prepare composite materials to be used in the preparation of electrodes. Results showed that voltammetric response could be obtained when at least 50% of graphite (w.w-1) is present in the material. SEM and thermogravimetry were also used in the characterization of the composites.
  • Synthetic tooth enamel: SEM characterization of a fluoride hydroxyapatite coating for dentistry applications Regular Articles

    Oliveira, Marise; Mansur, Herman Sander

    Resumo em Inglês:

    An alternative to etching enamel for retention of an adhesive is to grow crystals on the enamel surface. The potential advantages of crystal growth include easy procedure and less damage to the enamel. These crystals retain the adhesive or are the actual dental restoration. In this work, a paste of synthetic enamel was used to grow crystals of fluoride hydroxyapatite (F-HA) onto the human tooth surface. This technique can be used for several dentistry applications like enamel whitening, strengthening and restoration of early carie lesions. The low cost of reagents and simplicity of the technique along with the biocompatibility of the paste render possible the utilization on the market. The samples were prepared through the application of the paste by the incremental technique. The results obtained by scanning electron microscope (SEM)/EDX have indicated the deposition of a homogeneous layer of calcium phosphate that was grown onto the enamel substrate. The average thickness of the deposited film was in the range of 50-100 µm and with a similar density from the natural enamel observed by radiographic images.
  • Attachment of inorganic moieties onto aliphatic polyurethanes Regular Articles

    Ayres, Eliane; Vasconcelos, Wander Luiz; Oréfice, Rodrigo Lambert

    Resumo em Inglês:

    Polyurethanes have been used in a series of applications due basically to their versatility in terms of controlling the behavior by altering basically the type of reagents used. However, for more specific and advanced applications, such as in membranes, biomaterials and sensors, well-organized and defined chemical functionalities are necessary. In this work, inorganic functionalities were incorporated into aliphatic polyurethanes (PU) having different macromolecular architectures. Polyurethanes were synthesized using a polyether diol and dicyclohexylmethane 4,4' diisocyanate (H12-MDI). Polyurethanes having carboxylic acid groups were also produced by introducing 2,2- bis (hydroxymethyl) propionic acid in the polymerization process. Inorganic functionalities were inserted into polyurethanes by reacting isocyanate end capped chains with aminopropyltriethoxysilane followed by tetraethoxysilane. PU having carboxylic acid groups yielded transparent samples after the incorporation of inorganic entities, as an evidence of smaller and better dispersed inorganic entities in the polymer network. FTIR and swelling measurements showed that polyurethanes having carboxylic acid groups had inorganic domains less packed, condensed and cross-linked when compared to polyurethanes with no carboxylic acid groups. Results also suggested that the progressive incorporation of inorganic moieties in both types of polyurethanes occurred in regions previously activated with inorganic functionalities, instead of by the creation of new domains. The temperatures of thermal decomposition and glass transition were also shifted to higher temperatures when inorganic functionalities were incorporated into polyurethanes.
  • Porosity dependence of elastic constants in aluminum nitride ceramics Regular Articles

    Yoshimura, Humberto Naoyuki; Molisani, André Luiz; Narita, Nilson Eiji; Cesar, Paulo Francisco; Goldenstein, Hélio

    Resumo em Inglês:

    Aluminum nitride is a relatively new engineering ceramic and its mechanical properties have not been extensively studied. In this work, the effects of porosity (~0 to 38%) on sonic velocities, Poisson's ratio, and elastic moduli of partially sintered A1N, both pure and with additives, were investigated. The elastic constants, determined by the ultrasonic pulse-echo method, were significantly influenced by the porosity, but not by the different types of additives used (2 wt. (%) of CaCO3, CaO, and Y2O3). All elastic constants evaluated decreased with increasing porosity, but the rates of decrease were higher for elastic moduli compared do sonic velocities and Poisson's ratio. The results were analyzed in the light of stress concentration and loading bearing area models proposed in the literature.
  • Elaboration and characterization of nanostructured biocements for biomedical applications Regular Articles

    Camargo, Nelson Heriberto Almeida; Soares, Cristina; Gemelli, Enori

    Resumo em Inglês:

    Biocements formed from the composition Ca/P have been studied and developed since 1983. These biomaterials are promissing and have aroused great interest to biomedical surgery applications, fixation of prostheses and filling and reconstruction of bones. They can be employed as an element of load to fix implant and bone structure. In addition, biocements are easily shaped during surgical processes and favor early bone habitation, absorption, osseointegration, and osteoconduction of bone structure into the microstructure of the biocement thus favoring regeneration and reconstruction of bone tissue. This paper aims to develop biocements formed from calcium phosphate through the aqueous precipitation method by means of the dissolution-precipitation reaction, which involves solid/ liquid phase of CaO and phosphoric acid to form the calcium phosphate. The biocements investigated were synthesized when the molar ratios of Ca/P = 1.4, 1.5, 1.6, 1.7 and 1.8. The present results indicate that the aqueous precipitation method allowed nanostructured powder of calcium phosphate to form. Thermal treatment at 1300 °C for 2 hours provided biocements formed from calcium phosphate and hydroxyapatite. The study of hydration behaviour from 1 to 28 days in a solution, which contained 0.4% of sodium phosphate, emphasized phase modification and the presence of a microporous microstructure made of crystalline fibers. It was found that the shape and size of the crystalline fiber had a direct influence on the resulting mechanical properties. Investigating more carefully the behaviour of the specimens with a Ca/P molar ratio of 1.5, there was an increase in the strength value under compression as a function of time so that it reached the maximum value of strength ±45 MPa to specimens that had been hydrated for 28 days.
  • Analysis of transformations nucleated on non-random sites simulated by cellular automata in three dimensions Regular Articles

    Rios, Paulo Rangel; Pereira, Luciana de Oliveira; Oliveira, Flávio Faria de; Assis, Weslley Luiz da Silva; Oliveira, Valmir Torres de

    Resumo em Inglês:

    Cellular automata simulation in three dimensions is carried out to simulate microstrutural evolution for nuclei distribution ranging from a periodic arrangement to clusters of nuclei. The effect of clustering in three dimensions is found to be much more difficult to detect using conventional microstructural path analysis than in two dimensions. Microstructural path equations fit simulated data well, even when the nuclei are non-randomly located. However, the parameters obtained by means of this fitting lead to erroneous time dependent velocities. Therefore, measuring a descriptor that is sensitive to non-randomness such as the contiguity is even more important in three than in two dimensions.
  • Poly(borosiloxanes) as precursors for carbon fiber ceramic matrix composites Regular Articles

    Siqueira, Renato Luiz; Yoshida, Inez Valéria Pagotto; Pardini, Luiz Claudio; Schiavon, Marco Antônio

    Resumo em Inglês:

    Ceramic matrix composites (CMCs), constituted of a silicon boron oxycarbide (SiBCO) matrix and unidirectional carbon fiber rods as a reinforcement phase, were prepared by pyrolysis of carbon fiber rods wrapped in polysiloxane (PS) or poly(borosiloxane) (PBS) matrices. The preparation of the polymeric precursors involved hydrolysis/condensation reactions of alkoxysilanes in the presence and absence of boric acid, with B/Si atomic ratios of 0.2 and 0.5. Infrared spectra of PBS showed evidence of Si-O-B bonds at 880 cm-1, due to the incorporation of the crosslinker trigonal units of BO3 in the polymeric network. X ray diffraction analyses exhibited an amorphous character of the resulting polymer-derived ceramics obtained by pyrolysis up to 1000 °C under inert atmosphere. The C/SiBCO composites showed better thermal stability than the C/SiOC materials. In addition, good adhesion between the carbon fiber and the ceramic phase was observed by SEM microscopy
  • Evaluation of microstructural parameters of human dentin by digital image analysis Regular Articles

    Coutinho, Eduardo Tavares; d’Almeida, José Roberto Moraes; Paciornik, Sidnei

    Resumo em Inglês:

    Digital image analysis was used to fully characterize the microstructure of human dentin. With the automatic routine implemented, field and region parameters related to human dentin characterization were obtained in significant statistical quantities. The results obtained for the density, area fraction, distance between neighbors, tilt angle, area and average diameter of the dentinary tubules are presented for unerupted third molars. The results, grouped per class of dentin or per tooth, are discussed in the light of the previous data found on the literature.
  • Quantitative analysis of lead in polysulfide-based impression material Regular Articles

    Braga, Aparecida Silva; Braga, Sebastião Roberto Silva; Catirse, Alma Blásida Concepción Elizaur Benitez; Vaz, Luis Geraldo; Mollo Junior, Francisco de Assis

    Resumo em Inglês:

    Permlastic® is a polysulfide-based impression material widely used by dentists in Brazil. It is composed of a base paste and a catalyzer containing lead dioxide. The high toxicity of lead to humans is ground for much concern, since it can attack various systems and organs. The present study involved a quantitative analysis of the concentration of lead in the material Permlastic®. The lead was determined by plasma-induced optical emission spectrometry (Varian model Vista). The percentages of lead found in the two analyzed lots were 38.1 and 40.8%. The lead concentrations in the material under study were high, but the product’s packaging contained no information about these concentrations.
  • Bioartificial polymeric materials based on collagen and poly(N-isopropylacrylamide) Regular Articles

    Mano, Valdir; Ribeiro e Silva, Maria Elisa Scarpelli

    Resumo em Inglês:

    Films of collagen (CLG) and poly(N-isopropylacrylamide), PNIPAAm, were prepared by casting from water solutions. These bioartificial polymeric materials were studied to examine the influence of PNIPAAm content and glutaraldehyde vapor cross-linking on the thermal and biological stability of CLG. Mixtures, ranging from 20-80 wt% CLG composition, were cross-linked through exposure to glutaraldehyde vapors. Thermal and morphological properties of the films, cross-linked or not, were investigated by differential scanning calorimetry, thermogravimetry, and scanning electron microscopy, with the aim of evaluating miscibility, thermal stability, and interactions among the constituents. The experimental results indicated that the homopolymers are not thermodynamically compatible. However, there is good evidence that effective interactions, probably due to hydrogen bond formation, takes place between the constituents. These interactions are more evident on the samples that were not cross-linked. DSC studies revealed that PNIPAAm exerts a thermal stabilizing effect on uncross-linked CLG, while the cross-linking with glutaraldehyde affects only the biological polymer, preventing the interactions with PNIPAAm. SEM micrographs of the uncross-linked mixtures showed that the morphology, in all compositions studied, remains similar to the pure collagen. In the corresponding cross-linked samples, a more compact aggregation is observed although no appreciably changes can be seen.
  • Preparation of PtRu/carbon hybrids by hydrothermal carbonization process Regular Articles

    Tusi, Marcelo Marques; Brandalise, Michele; Correa, Olandir Vercino; Oliveira Neto, Almir; Linardi, Marcelo; Spinacé, Estevam Vitorio

    Resumo em Inglês:

    PtRu/Carbon hybrids were prepared by hydrothermal carbonization process using glucose or starch as carbon sources and reducing agents and platinum and ruthenium salts as catalysts of carbonization process and metals source. The obtained PtRu/Carbon materials were characterized by SEM/EDX, TGA, XRD and cyclic voltammetry. The electro-oxidation of methanol was studied by cyclic voltammetry using the thin porous coating technique aiming fuel cell application. The catalytic activity was dependent of carbon source and time used in the synthesis.
  • Sol-Gel SiO2-CaO-P2O5 biofilm with surface engineered for medical application Regular Articles

    Federman, Sonia Regina; Costa, Vilma Conceição; Vasconcelos, Daniela Cordeiro Leite; Vasconcelos, Wander Luiz

    Resumo em Inglês:

    Sol-gel film in the SiO2-CaO-P2O5 system was prepared from TEOS, TEP, alcohol and hydrated calcium nitrate in an acidic medium. The coatings were deposited on stainless steel using the dip-coating technique. After deposition, the composite was submitted to heat treatment, at different temperatures and exposure times to investigate the influence of such parameters on the surface morphology of the composite. The coated surfaces were characterized by AFM, SEM and FTIR. The present study showed that the formation of different textures (an important parameter in implant fixation) could be controlled by temperature and time of heat treatment.
  • Surface area, crystal morphology and characterization of transition alumina powders from a new gibbsite precursor Regular Articles

    Vieira Coelho, Antonio Carlos; Souza Santos, Helena de; Kiyohara, Pedro Kuniiko; Marcos, Kelly Nanci Pinto; Souza Santos, Pérsio de

    Resumo em Inglês:

    A new procedure was used to prepare a microcrystalline powder constituted by thin euhedral hexagonal gibbsite plates, 0.2 to 0.6 µm in diameter and 32 nm thick. The powder, fired between 200 and 1000 °C, produced chi and kappa transition aluminas. Alpha-alumina is formed from 1000 °C and recrystallized up to 1500 °C. At 1000 °C, kappa- and alpha-alumina coexisted, but kappa-alumina could only be characterized by SAED. The details of the internal organization of the transition alumina pseudomorphs were clearly observable in TEM due to the great thinness of the I-gibbsite plates. The specific surface area varied from pristine I-gibbsite (24.9 m².g-1) to chi- and kappa transition aluminas (25.4 m².g-1) at 1000 °C to alpha-alumina (4.0 m².g-1) at 1500 °C. The maximum value of specific surface area is 347 m².g-1 in chi-alumina powder at 300 °C, a difference from Bayer gibbsite, in which the chi-alumina highest surface area is 370 m².g-1 at 400 °C.
  • Degree of conversion and molecular weight of one denture base and three reline resins submitted to post-polymerization treatments Regular Articles

    Urban, Vanessa Migliorini; Machado, Ana Lucia; Vergani, Carlos Eduardo; Jorge, Érica Gouveia; Santos, Luís Presley Serejo dos; Leite, Edson Roberto; Canevarolo, Sebastião Vicente

    Resumo em Inglês:

    The effect of post-polymerization treatments (MW-microwave irradiation and WB-water-bath) on the degree of conversion (DC) of three reline resins (Ufi Gel hard-U, Kooliner-K, and Tokuso Rebase Fast-T) and one denture base resin (Lucitone 550-L), submitted to two polymerization cycles (LS-short and LL-long), was evaluated by using FT-Raman spectroscopy (n = 5). The molecular weight (Mw) of the powder of all materials and of K polymerized specimens (control; MW; and WB; n = 3) was analyzed using GPC. DC data were analyzed using Kruskal-Wallis test (a = .05). For control specimens, there were no significant differences between U (68%) and LL (77%) and among LL, K (81%), and T (84%). LS (92%) had the highest DC (P < 0.05). Only material K exhibited an increased DC after WB (P < 0.05). All powders had Mw from 4.0 x 10(5) to 6.5 x 10(5) and narrow Mw distributions (2.1 to 3.6). Polymerization and post-polymerization produced K specimens with Mw similar to that of K powder.
  • Effect of mechanical alloying and Ti addition on solution and ageing treatment of an AA7050 aluminium alloy Regular Articles

    Cardoso, Kátia Regina; Travessa, Dilermando Nagle; Escorial, Asunción García; Lieblich, Marcela

    Resumo em Inglês:

    In this work, solution heat treatments at different temperatures were performed in a commercial based AA7050 aluminium alloy, with and without titanium addition, produced by mechanical alloying and hot extrusion with the aim to investigate the effect of titanium addition and mechanical alloying in the precipitates stability. The same heat treatment conditions were used in a reference sample obtained from a commercial AA7050 alloy. Solution heat treated samples were characterised by differential scanning calorimetry (DSC), optical microscopy and hardness test. Once the better temperature for the solution treatment of modified alloys was defined, the ageing curve at 120 °C was obtained to verify the effect of milling and Ti addition in the precipitation and in the maximum values of hardness obtained for the alloys.
  • Corrosion control of aluminum surfaces by polypyrrole films: influence of electrolyte Regular Articles

    Liu, Andréa Santos; Oliveira, Maria Auxiliadora Silva

    Resumo em Inglês:

    Polypyrrole (PPy) films were galvanostatically deposited on 99.9 wt. (%) aluminum electrodes from aqueous solutions containing each carboxylic acid: tartaric, oxalic or citric. Scanning Electron Microscopy (SEM) was used to analyze the morphology of the aluminum surfaces coated with the polymeric films. It was observed that the films deposited from tartaric acid medium presented higher homogeneity than those deposited from oxalic and citric acid. Furthermore, the corrosion protection of aluminum surfaces by PPy films was also investigated by potentiodynamic polarization experiments.
  • Rapid manufacturing of polyethylene parts with controlled pore size gradients using selective laser sintering Regular Articles

    Salmoria, Gean Vitor; Ahrens, Carlos Henrique; Klauss, Pricila; Paggi, Rodrigo Acacio; Oliveira, Rafael Galet; Lago, Alexandre

    Resumo em Inglês:

    In this study HDPE specimens were fabricated by selective laser sintering using different particle sizes to obtain controlled variations in the porosity. Electron microscopy, density measurements and mechanical analyses were conducted for the characterization of the specimens. Parts with controlled pore gradients were also manufactured and characterized. The specimens with larger particle sizes had a high sintering degree and a significant level of close pores, as shown by microscopy and density analyses. However, the mechanical properties of specimens prepared with large particles had low values due to the limited density of union points, i.e., low neck number/area. HDPE parts with pore gradients were prepared by selective laser sintering demonstrating that this technique can be used to easily control the structure and the properties of the parts manufactured. This technology may have applications in areas such as drug delivery devices and scaffolds for tissue engineering.
  • Study of the aluminothermic reduction of niobium pentoxide through thermal analysis experiments and high energy milling processing Regular Articles

    De Lazzari, Claudio Parra; Simões, Danielle Goya; Capocchi, José Deodoro Trani

    Resumo em Inglês:

    Aluminothermic reduction of niobium pentoxide was studied through thermal analysis techniques such as differential thermal analysis (DTA) and thermogravimetry (TG) as well as through high energy milling processing. Reactants mixtures were composed by powders of Nb2O5 and Al. In the case of DTA-TG experiments, different molar ratios Nb2O5:Al were heated in a dynamic atmosphere of synthetic air under controlled conditions. The high energy milling runs were carried out via SPEX vibratory mill under argon atmosphere and with milling power equal to 7:1 (ratio of mass of balls to mass of mixture) with 10 pct excess of Al over the stoichiometric mass of aluminum necessary. In both kinds of experiments, X ray diffraction was used in order to identify the products of reaction. From DTA-TG experiments, it was possible to determine the experimental value of the enthalpy change (-595.9 kJ.mol-1), which is near to the theoretical one. From the milling experiments, it was possible to verify the possibility of the occurance of aluminothermic reducion of niobium pentoxide via this kind of processing.
  • Characterization of commercial ceramic adsorbents and its application on naphthenic acids removal of petroleum distillates Regular Articles

    Silva, Juliana Pereira; Senna, Lilian Ferreira de; Lago, Dalva Cristina Baptista do; Silva Jr., Paulo Ferreira da; Dias, Elton Gonçalves; Figueiredo, Marco Antônio Gaya de; Chiaro, Sandra Shirley Ximenes

    Resumo em Inglês:

    The mixture of carboxylic acids present in petroleum oil and directly responsible for its acidity and corrosiveness in liquid phase during the refine process is denominated "naphthenic acids". These acids are also present in distilled fraction of petroleum, causing several problems in final products quality. A possible way to remove the carboxilic acids from petroleum distilled fractions is the adsorption in porous materials. However, the results obtained until now indicate that ion exchange resins would be the best adsorbents for this process, which would probably increase its cost. In this work, two commercial adsorbents (clay and activated alumina) were characterized by a set of physical-chemistry techniques and evaluated concerning their capacity of removing naphthenic acids from a light petroleum fraction. It was verified the influence of a thermal treatment previous to the adsorption in its physical-chemistry characteristics and its properties. A high reduction of the TAN values was verified in the residual oils from both adsorbent, although there was a competition among all the compounds present in the light oil fraction for the adsorption sites, which can be probably related to the thermal pre-treatment. These results were related to corrosion yield experiments, and it was observed that the adsorbent pretreatment also affected the reduction in corrosion yields for both alumina and clay.
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