Editorial Editorial |
Articles presented at the 1º Congresso da Sociedade Brasileira de Pesquisa em Materiais, Rio de Janeiro, julho de 2002 Preparation and biocompatibility of poly (methyl methacrylate) reinforced with bioactive particles Pereira, Marivalda de Magalhães Oréfice, Rodrigo Lambert Mansur, Herman Sander Lopes, Miriam Teresa Paz Turchetti-Maia, Regina Maria De Marco Vasconcelos, Anilton Cesar Abstract in English: Calcium phosphates and bioactive glasses have been used in many biomedical applications for more than 30 years due basically to their bioactive behavior. However, ceramics are too brittle for applications that require high levels of toughness and easy processability. In this work, a biphasic calcium phosphate (BCP) and a bioactive glass composition (BG) were combined with polymers to produce composites with tailorable properties and processability. The BCP particles were synthesized by a precipitation technique. The BG particles were produced by sol-gel processing. The BCP particles were treated with a silane agent to improve the compatibility between particles and the polymer matrix. Dense samples were produced by hot pressing (200 °C) a mixture of 30 wt.% of particles in poly (methyl methacrylate). The samples produced were characterized by X-ray diffraction, infrared spectroscopy and scanning electron microscopy. Mechanical properties were evaluated by a three point bending test. Samples were also submitted to in vitro bioactivity test and in vivo toxicity test. Results showed that the production of the composites was successfully achieved, yielding materials with particles well dispersed within the matrices. Evaluation of the in vivo inflammatory response showed low activity levels for all composites although composites with silane treated BCP particles led to milder inflammatory responses than composites with non-treated particles. |
Teste in vitro de citotoxicidade: estudo comparativo entre duas metodologias Rogero, Sizue Ota Lugão, Ademar Benévolo Ikeda, Tamiko Ichikawa Cruz, Áurea Silveira Abstract in Portuguese: A avaliação in vitro da biocompatibilidade de diferentes tipos de biomateriais foi realizada pelo teste de citotoxicidade em cultivo de células de tecido conectivo de camundongos, NCTC Clone 929 da American Type Culture Collection. O estudo comparativo do ensaio de citotoxicidade foi realizado com duas metodologias: 1) ensaio de difusão em ágar e 2) ensaio de incorporação do vermelho neutro. Os resultados obtidos demonstraram que ambas as metodologias podem ser utilizadas, de acordo com o tipo de amostra a ser analisada. |
Articles presented at the 1º Congresso da Sociedade Brasileira de Pesquisa em Materiais, Rio de Janeiro, julho de 2002 Mechanical characterisation of porous glass reinforced hydroxyapatite ceramics: Bonelike® Silva, Marcelo Henrique Prado da Lemos, Alexandra Fernandes Ferreira, José Maria da Fonte Santos, José Domingos Abstract in English: In the present study, mechanical properties of porous glass reinforced hydroxyapatite bioceramics were assessed by microhardness, bending and compression tests and fracture toughness determination. Porous discs were produced by a dry method using wax spheres as pore formers. Green bodies were sintered and the final microstructure of the composites consists of hydroxyapatite, alpha and beta tricalcium phosphate (alpha and <FONT FACE=Symbol>b</font>-Ca3(PO4)2)due to the reaction between the glassy phase and the hydroxyapatite matrix. The results of the mechanical tests showed that the glassy phase yielded higher fracture toughness and bending strength when comparing with literature data for single hydroxyapatite. There is a compromise between mechanical properties and the porosity level for bioceramics: for example, according to Weibull statistics for composites with 65% porosity the maximum bending stress level is 0.2 MPa for 100% survival probability whereas this stress level increases to 2.5 MPa for composites with 40%. However, only the 65% porosity composite samples seem to have the complete adequate morphology for bone ingrowth. |
Articles presented at the 1º Congresso da Sociedade Brasileira de Pesquisa em Materiais, Rio de Janeiro, julho de 2002 A new route to process diamond wires Filgueira, Marcello Bobrovnitchii, Guerold Pinatti, Daltro Garcia Abstract in English: We propose an original route to process diamond wires, denominated In Situ Technology, whose fabrication involves mechanical conformation processes, such as rotary forging, copper tubes restacking, and thermal treatments, such as sintering and recrystallisation of a bronze 4 wt.% diamond composite. Tensile tests were performed, reaching an ultimate tensile strength (UTS) of 230 MPa for the diameter of <FONT FACE=Symbol>Æ</FONT> = 1.84 mm. Scanning electron microscopy showed the diamond crystals distribution along the composite rope during its manufacture, as well as the diamond adhesion to the bronze matrix. Cutting tests were carried out with the processed wire, showing a probable performance 4 times higher than the diamond sawing discs, however its probable performance was about 5 to 8 times less than the conventional diamond wires (pearl system) due to the low abrasion resistance of the bronze matrix, and low adhesion between the pair bronze-diamond due to the use of not metallised diamond single crystals. |
Articles presented at the 1º Congresso da Sociedade Brasileira de Pesquisa em Materiais, Rio de Janeiro, julho de 2002 Dye incorporation in polyphosphate gels: synthesis and theoretical calculations Del Nero, Jordan Galembeck, André Silva, Sidicleia Bezerra Costa Siva, José Augusto Pereira da Abstract in English: In this work we described theoretical calculations on the electronic structure and optical properties of the dyes crystal violet and malachite green based in semiempirical methods (Parametric Method 3 and Intermediate Neglect of Differential Overlap / Spectroscopic - Configuration Interaction) and the synthesis of a new hybrid material based upon the incorporation of these dyes in an aluminum polyphosphate gel network. The samples are nearly transparent, free-standing thick films. The optical properties of the entrapped dyes are sensitive to chemical changes within the matrix caused either by gel aging or external stimulli such as exposition to acidic and basic vapors that can percolate within the matrix. Our theoretical modeling is in good agreement with the experimental results for the dyes. |
Articles presented at the 1º Congresso da Sociedade Brasileira de Pesquisa em Materiais, Rio de Janeiro, julho de 2002 Modeling of alkynes: synthesis and theoretical properties Rosseto, Renato Torres, José Celso Del Nero, Jordan Abstract in English: In this paper we present the synthesis and simulation of alkynes derivatives. Semiempirical calculations were carried out for the ground and first excited states, including the spectroscopic properties of the absorption and emission (fluorescence and phosphorescence) spectra by INDO/S-CI and DNdM-INDO/S-CI methods with geometries fully optimized by PM3/CI. The fact that the theoretical spectra are in accord with the experimental absorption spectra gives us a new possible approach on how structure modifications could affect the non-linear optical properties of alkynes. |
Articles presented at the 1º Congresso da Sociedade Brasileira de Pesquisa em Materiais, Rio de Janeiro, julho de 2002 Effect of viscosity and temperature on the microstructure of BBT thin films Costa, Gustavo Carneiro da Simões, Alexandre Zirpoli Gasparotto, Gisele Zaghette, Maria Aparecida Stojanovic, Biljana Cilense, Mario Varela, José Arana Abstract in English: Thin films of BBT were deposited on silicate and Pt/Ti /SiO2 (111) substrates by spin- coating from the polymeric precursor method (Pechini process). The obtained films were characterized by optical microscopy, X-ray diffraction and atomic force microscopy. The influence of viscosity on the morphology of BBT thin films as well as the influence of temperature on crystallization, morphology and properties of BBTare discussed. Surface roughness and crystallization of these films are strongly dependent on the annealing conditions. |
Articles presented at the 1º Congresso da Sociedade Brasileira de Pesquisa em Materiais, Rio de Janeiro, julho de 2002 Superficial modifications in TiO2 and Al2O3 ceramics Santos, Flávio de Paula Campos, Elson de Costa, Marcelo Melo, Francisco Cristóvão Lourenço Honda, Roberto Yzumi Mota, Rogério Pinto Abstract in English: The properties of hydrophilicity or hydrophobicity of materials are defined mainly, though not exclusively, by their composition, morphology and surface energy. In this work, titanium dioxide (TiO2) and aluminum oxide-alumina (Al2O3) ceramics prepared by uniaxial pressing were studied in terms of surface energy. The surfaces of these ceramics were treated with nitrogen plasma, using a stainless steel reactor excited by a 13,6 MHz radio frequency operating at 50 W input power and 13 Pa nitrogen pressure. The surface morphology was investigated by scanning electron microscopy (SEM) analysis. Surface energy and contact angle measurements were taken using a RAMÉ-HART goniometer. These measurements were taken as function of time, over a 21-day period. The contact angle and surface energy values were found to change by almost 34% in comparison to their initial values immediately following plasma treatment. Nonetheless, the hydrophilic character of the Al2O3 and TiO2 remained constant throughout the test period. |
Blendas biodegradáveis de poli(3-hidroxibutirato)/poli(e-caprolactona): obtenção e estudo da miscibilidade Vogelsanger, Nilton Formolo, Michele Cristina Pezzin, Ana Paula Testa Schneider, Andréa Lima dos Santos Furlan, Sandra Aparecida Bernardo, Heloísa Pinna Pezzin, Sérgio Henrique Pires, Alfredo Tibúrcio Nunes Duek, Eliana Aparecida de Rezende Abstract in English: Due to its biodegradability, poly(3-hydroxybutyrate) P(3-HB) has attracted much attention in the environmental sector. However, some characteristics of this polymer, such as high crystallinity, poor processability and high brittleness, have lead several research groups to study polymeric blends in order to modify P(3-HB) properties. Poly(epsilon-caprolactone) (PCL) is a synthetic polyester which is completely degraded after about one year when buried in soil. In general, it acts as a polymeric plasticizer lowering the elastic modulus and enhancing the processability of the blend. Blends of two biodegradable polymers, P(3-HB) and PCL have been prepared by casting in different compositions. Miscibility, thermal behavior and morphology of these blends were studied using modulated differential scanning calorimetry (MDSC), scanning electron microscopy (SEM) and polarizing light microscopy (PLM). The two glass transition temperatures, detected by MDSC, suggest the immiscibility of the system. Phase separation was confirmed by PLM. |
Articles presented at the 1º Congresso da Sociedade Brasileira de Pesquisa em Materiais, Rio de Janeiro, julho de 2002 Microhardness and chemical composition of human tooth Gutiérrez-Salazar, Maria del Pilar Reyes-Gasga, Jorge Abstract in English: Hardness of human tooth, both in enamel and dentin, has been measured at different sites using a Vicker's diamond. In this work we show that these values are almost constant all along the enamel and dentin thicknesses. Indentations were done from outer enamel surface to inner dentin layer, going through the enamel-dentin junction, both in transverse and longitudinal samples. Geometrical well-shape indentation uniformity was checked both with light and with scanning electron microscopes, and the chemical composition of the tooth was analyzed with characteristic X-ray energy dispersive spectroscopy. Hardness measurements were in the range from 270 to 360 VHN for enamel and 50 to 60 VHN for dentin. Cervical zone in longitudinal section showed the lowest value while in transverse sections the highest. All the hardness values were statically significative. Tour results indicate that the difference between enamel and dentin hardness has nothing to do with the content of Na, Cl and Mg, but the percentage of organic and inorganic materials in enamel and dentin. |
Articles presented at the 1º Congresso da Sociedade Brasileira de Pesquisa em Materiais, Rio de Janeiro, julho de 2002 Large scale low cost production of submicrometric powder through biomass refinery Pinatti, Daltro Garcia Conte, Rosa Ana Borlini, Mônica Castoldi Santos, Benedito Celso dos Marcondes, Marco Aurélio Oliveira, Isaías de Montanha, Renata Garcia Oliveira Soares, Álvaro Guedes Romão, Érica Leonor Ferreira, João Carlos Pereira, Maria Luiza Gonçalves Abstract in English: Biomass Refinery (BR) is a null pollution thermochemical sequential cracking of any biomass and some petrochemical products, which generates chemicals, liquid or solid fuels and inorganic submicrometric/nanometric powders (SM/NM) such as ashes, silica, and carbon black. The processing route, powder characterisation and addition of some ashes to red clay resulting a grès-type ceramics will be presented. Rupture strengths of the vitrified ceramics were respectively 36 MPa for pure clay, 44 MPa for clay + 13.5% MOL ash (organic matter of municipal solid waste), 50 MPa for clay + 20% F+20% CL* ash (50% MOL + 50% wood) and 42 MPa for clay + 40% feldspar (used for comparison). The reason why the BR-ashes are better than feldspar is due to their submicrometric and partially nanometric nature. The impact of BR-ash technology can be evaluated by its national potential production of 2 × 10(6) ton/year only from municipal solid waste (MSW) compared to 350,000 ton/year of national consumption. The first BR is under installation in Lorena - SP, Brazil. |
Regular Articles Properties and structural features of iron doped BABAL glasses Reis, Signo Tadeu dos Pontuschka, Walter M. Yang, Jinbo B. Faria, Dalva L A. Abstract in English: The chemical durability, density and structure of the BABAL glasses with batch compositions (100-x)(0.30BaO·0.50B2O3·0.20Al2O3)·xFe 2O3 (1 < x < 10 mol%), were investigated using Mössbauer spectroscopy, electron paramagnetic resonance (EPR), X-ray diffraction, Raman and differential thermal analysis (DTA). The chemical durability for the glass of composition 27BaO·45B2O3·18Al 2O3·10Fe2O3 (mol%) at 90 °C in distilled water was 700 times lower than that of iron phosphate glass 40Fe2O3·60P2O 5 (mol%). The Mössbauer spectra indicate the presence of iron (II) and iron (III) in tetrahedral or octahedral coordination. The results obtained from the g ef = 4.3 EPR line are typical of the occurrence of iron (III) occupying substitutional sites and the line g ef = 2.0 is related to the association of two or more Fe ions found in the interstices (or holes occupied by the glass modifier cations) of the glass network. The paths of X-ray diffraction are typical for glasses based in borate glasses. The Raman spectra showed that the boroxol ring disappears with the increase of iron content, concomitant with the appearance of BO4 and tetraborate structural units. At these conditions, an increase of dissolution rate and clustering of iron ions is observed. |
Regular Articles Hydrothermal method for preparing calcium phosphate monoliths García Carrodeguas, Raúl Morejón Alonso, Loreley García-Menocal, José Angel Delgado Morejón Alonso, Lizette Ginebra Molins, María Pau Martínez Manent, Salvador Gil Mur, Javier Toledo Pérez, Jorge Planell Estany, José Antonio Abstract in English: A new hydrothermal route for preparing biphasic calcium phosphate monoliths is proposed. Firstly, a slurry of beta-tricalcium phosphate/ortho-phosphoric acid (<FONT FACE=Symbol>b</font>-TCP/H3PO4) is cast into the desired final shape and size to obtain a block composed of dicalcium phosphate dihydrate (DCPD) and <FONT FACE=Symbol>b</font>-TCP. This block is then treated in 1.0 M Na2HPO4 at 60 °C in order to hydrolyze the DCPD into Ca10-x(HPO4)x(PO4) 6-x(OH)2-x (CDHA) and Ca8H2(PO4)6 .5H2O (OCP). The result is a monolithic piece which preserves the initial shape and size, but which is composed instead of CDHA, OCP, and <FONT FACE=Symbol>b</font>-TCP. During the initial stage, when the pH is slightly alkaline, the product of DCPD hydrolysis is CDHA. However, when a neutral or slightly acidic pH is reached OCP is formed. Test samples processed by this method showed complete conversion of DCPD into CDHA and OCP after 112 h of hydrolysis, and with a compressive strength of 16.2 MPa, similar to cancellous bone. |
Regular Articles Characterization of corrosion products formed on steels in the first months of atmospheric exposure Antunes, Renato Altobelli Costa, Isolda Faria, Dalva Lúcia Araújo de Abstract in English: The corrosion products of carbon steel and weathering steel exposed to three different types of atmospheres, at times ranging from one to three months, have been identified. The steels were exposed in an industrial site, an urban site (São Paulo City, Brazil), and a humid site. The effect of the steel type on the corrosion products formed in the early stages of atmospheric corrosion has been evaluated. The corrosion products formed at the various exposure locations were characterized by Raman microscopy, X-Ray diffraction (XRD) and their morphology was observed by Scanning Electron Microscopy (SEM). Three regions of different colours (yellow, black and red) have been identified over the steel coupons by Raman microscopy. Analysis carried out on each of these areas led to the characterization of the correspondent oxide/hydroxide phases. The main phases present were lepidocrocite (g-FeOOH) and goethite (a-FeOOH). Small amounts of magnetite (Fe3O4) were also eventually encountered. |
Regular Articles Optical storage properties in cast films of an azopolymer Neves, Ubaldo Martins das Santos Junior, David Sotero dos Giacometti, José Alberto Zílio, Sergio Carlos Misoguti, Lino Balogh, Débora Terezia Oliveira Junior, Osvaldo Novais de Mendonça, Cleber Renato Abstract in English: In this paper we discuss the properties of optically induced birefringence in DR19-MDI cast films that may be used in optical storage applications. The selection of DR19-MDI cast films was based on a comparative study of optical storage properties of Langmuir-Blodgett (LB) films from various azopolymers. DR19-MDI possesses a high residual fraction of optical birefringence and good environmental stability, which was corroborated by the data from optical storage experiments. DR19-MDI cast films maintain a reasonable level of birefringence after the initial decay due to chromophore relaxation, thus making them promising candidates for optical storage devices. |
Regular Articles Ageing of the DGEBA/TETA epoxy system with off-stoichiometric compositions d'Almeida, José Roberto Moraes Menezes, Gustavo Wagner de Monteiro, Sérgio Neves Abstract in English: An investigation was carried out on the room temperature ageing of off-stoichiometric DGEBA/TETA epoxy formulations. The results obtained show that the epoxy rich mixtures have their inherent brittleness increased by the ageing treatment due to recrystalization of the unreacted epoxy monomers, although homopolymerization could also play a minor role. The initial reaction steps dominated by the amine addition reactions control the macromolecular structure and the mechanical performance of the stoichiometric and near stoichiometric formulation with excess of epoxy monomer. Plasticization due to absorbed -OH results on a significant increase of the deformability of these formulations. The amine rich mixtures have the more stable structures, although plasticization due to moisture absorption from the surrounding environment also produces an increase on the deformability of all, but one, of the formulations investigated. |
Regular Articles Internal friction due to long-range diffusion of hydrogen in the Nb-46 wt.% Ti alloy Grandini, Carlos Roberto Florêncio, Odila Jordão, José Alberto Rodrigues Abstract in English: The Gorsky Effect was investigated by internal friction measurements in the Nb-46 wt.% Ti-H system. The internal friction measurements were performed in a torsion pendulum with frequency of 3.8 Hz in a temperature range from 80 to 700 K. An interpretation of the experimental data showed that the hydrogen diffusion coefficient D obeys the Arrhenius' law in the temperature interval of 300 to 700 K, with D0 = 7.4 × 10-4 cm²/s and activation energy E = (0.102 ± 0.005) eV. At low temperatures, Do and E were found to be respectively 2.0 × 10-4 cm²/s and (0.063 ± 0.005) eV, with a deviation of the Arrhenius law of higher temperatures. |
Regular Articles Evaluation of the relevant features of welding defects in radiographic inspection Carvalho, Antonio Alves de Suita, Raphael Carlos de Sá Brito Silva, Romeu Ricardo da Rebello, João Marcos Alcoforado Abstract in English: The use of X-ray as an inspection technique to ensure the integrity of industrial products dates from the beginning of the 20th century. Therefore, it is a tool of non-destructive inspection widely known. Nowadays, however, there are several researches forward on the optimization of such inspection technique, mainly for the development of an automatic system of radiographic image analysis. That is, a system that can identify and classify the defects in the radiography. An important step in the construction of this system is the classification of defects, which is usually done by using some of their features. The purpose of this work is to study the relevance of some defect features in order to classify some of the main classes of defects. The employed technique is the linear correlation between the defect features and the classes of defects. A non-linear pattern classifier is used, implemented by a neural network, to evaluate the performance in the classification. The results showed the efficiency of the method used. |
Evaluación de la dureza superficial en amalgamas en función de tipos de aleaciones, momentos y tipos de pulimentos Ramos, Juliana Panazzolo Benitez Catirse, Alma Blásida Concepción Elizaur Corona, Silmara Aparecida Milori Abstract in English: The aim of this study was to analyze in vitro surface hardness (micro-indentation tester Wolpert) of different types of amalgam alloys varying the technique and polishing time. Tested were the amalgam: Velvalloy, Permite e Dispersalloy. For each material, 2 polishing techniques were accomplished: T1 (bladed finishing burs + abrasive rubber points + pumice-water slurry in Robinson polishing brush) and; T2 (abrasive rubber points + pumice-water slurry in Robinson polishing brush), at 2 periods of time: P1 (immediately - 15 min after condensation) and P2 (after 24 h). For each experimental condition, 5 samples were prepared. For each sample, 2 indentations were taken and the average was determined. Were made analysis using ANOVA and Tukey test. Were concluded that: a) using the Permite alloy with polishing after 24 h the surface hardness of restoration will be higher; b) the technique T2 enhances the hardness of dental amalgams and c) alloy Permite with polished immediately were statisticaly equal than Velvalloy polished after 24 h. |