Estudo da sinterização e oxidação anódica na produção de um capacitor eletrolítico de nióbio

It seeks to find an alternative to the current tantalum electrolytic capacitors in the market due to its high cost. Niobium is a potential replacement for be lighter and cheaper than tantalum. They belong to the same table group periodically and thus exhibit several physical and chemical properties similar. Niobium is used in many technologically important applications, and Brazil has the largest reserves, around 96%. These electrolytic capacitors have high specific capacitance, so they can store high energy in small volumes compared to other types of capacitors. This is the main attraction of this type of capacitor because is growing demand in the production of capacitors with capacitance specifies increasingly high, this because of the miniaturization of various devices such as GPS devices, televisions, computers, phones and many others. The production route of the capacitor was made by powder metallurgy. The initial niobium poder was first characterized by XRD, SEM and laser particle size to then be sieved into particle size 400mesh. The powder was then compacted at pressure of 150MPa and sintered at 1400, 1450 and 1500°C using two sintering time 30 and 60min. Sintering is an important part of the process as it affects properties as porosity and surface cleaning of the samples, which greatly affected the quality of the capacitor. After sintering the samples were underwent a process of anodic oxidation (anodizing), which created a thin film of niobium pentoxide over the whole surface of the sample, this film is the dielectric capacitor. The anodizing process variables influenced a lot in film formation and consequently the capacitor. The samples were characterized by electrical measurements of capacitance, loss factor and ESR (equivalent series resistance). The sintering has affected the porosity and in turn the specific area of the samples. The capacitor area is directly related to the capacitance, that is, the higher the specific area is the capacitance. Higher sintering temperatures decrease the surface area but eliminate as many impurities. The best results were obtained at a temperature of 1400°C with 60 minutes. The most interesting results were compared with the specific capacitance and ESR for all samples.

Avaliação tribológica de novas modificações superficiais para cilindros de laminação a frio

The present work analyzed the tribological behavior of coatings/surface modifications traditionally used in cold rolling mill rolls and new coatings/surface modificationswith potential to replace the carcinogenic hard chrome. The study started with identification of wear mechanisms occurring in real coldrollingmill rolls. Due the high cost and dimensions of the rolls, thereplication technique was used. Replicas were obtained from 4 different rolling millBrazilian companies before and after a normal rolling campaign. Initial sliding tests were conducted using spherical and cylindrical counter bodies in order to verifywhichtribological conditions allowed to reproduce the wear mechanisms found in the replicas. These tests indicated the use of reciprocating sliding tests with cylindrical counter bodies (line contact), normal load of 100 N, and test times of and 1 h and 5 h. Different surface modifications were carried out on samples produced from a fragment of a rolling mill roll. The specimens were heat treated and ground on both sides. After, some specimens were surface textured by electrical discharge texturing (EDT). For both groups (ground and EDT), subsequent treatments of chromium plating, electroless NiP coating and plasma nitriding were carried out. The results of the reciprocating tests showed that specimens with electroless NiP coating presented the lowest friction coefficients, while plasma nitrided specimens showed the highest. In general, previous surface texturing before the coating/surface modification increased the wear of the counter bodies. Oneexceptionwas for EDT with subsequent electroless NiP coating, which presented the lowest counter bodies wear rate. The samples withelectroless NiP coating promoted a tribolayer consisting of Nickel, Phosphorus and Oxygen on both the specimens andthecounter bodies, which was apparently responsible for the reduction of friction coefficient and wear rate. The increase of the test time reduced the wear rate of the samples, apparently due the stability of the tribolayers formed, except for the nitrided samples. For the textured specimens, NiP coating showed the best performance in maintaining the surface topography of the specimens after the sliding tests.

Retificação plana tangencial dos ferros fundidos nodular, vermicular e cinzento em várias condições de corte

In a scenario of increasing competitiveness of the global industrial sector and with a consumer market increasingly demanding, there is an increased demand for new materials and, consequently, possibilities to explore new research and technological advances towards the development of new manufacturing methods or the improvement of existing technologies. In the case of cast irons, new grades of them have been developed so that their mechanical properties have been improved, making them more competitive with steel, expanding the applications and thus represents great economic gain for metallurgy and manufacturing sectors. This increases the interest and creates new opportunities to study these materials and identify how they respond in terms of the surface integrity, tool wear, cutting forces, among others, when machined by grinding operation. In this context, due to the lack of results from grinding of cast irons and studies comparing grindability among several grades of cast irons found in the literature, this work aims to generate scientific and technological contribution to the metallurgical and metal working sector through roughness results (Ra and Rz parameters) and evaluation and analysis of the subsurface integrity of three cast iron grades (gray, compacted graphite and nodular). The machining trials were performed on a surface grinding machine with silicon carbide grinding wheel at different cutting conditions. The input variables were the radial depth of cut (15 and 30 μm), worktable speed, vw (5 and 10 m/min) and the abrasive grain size of the grinding wheel. The results showed that surface roughness increased with the radial depth of cut for all materials tested; and the lowest values were obtained for gray cast iron. Also, roughness was sensitive to variation of worktable speed and the lowest values were obtained after machining with vw = 5 m/min. With respect to the abrasive grain size, as it decreased the roughness values increased to gray and nodular cast iron grades. Furthermore, grinding burns marks were observed on the surfaces of nodular cast iron and compacted graphite iron grades after grinding the smallest grain size, contrary to what is usually reported in literature. However, no evidence of severe thermal damages below the machined surfaces of all cast iron grades was observed after analyzing the results of hardness and the SEM micrograph images.

Las estatuas-menhir noroccidentales en contexto: conectividad y conexiones materiales durante el Bronce Tardío/Final

Este artículo analiza las estatuas-menhir noroccidentales que se distribuyen en el área comprendida entre los valles del río Duero y el río Miño, pero que descubrimientos recientes han extendido a regiones fuera de este área nuclear. Partiendo de tres aspectos claves para su interpretación (la cronología, su relación con el paisaje y su sentido iconográfico), se examinan las relaciones entre estas formas materiales y un paisaje socio-material de acción específico (las formas socio-materiales de interacción propias del Bronce final atlántico). Para ello, se tiene en cuenta diferentes conexiones materiales (presencia, encuentro, coexistencia, hibridación, etc.) que permiten contextualizar las estatuasmenhir dentro de un proceso histórico particular: la integración del noroeste de la península Ibérica en un contexto de relaciones mediterráneo-atlánticas, en la segunda mitad del II milenio a.C.

Source Provenance of Pre-Historic Granitic Grindstones: The Case Study of the Cogotas I Archaeological Site of Arroyo Mucientes/San Lázaro (Castronuño, Valladolid) and a Proposal on the General Methodological Flow Process

The occurrence of hand grindstones at the Cogotas I archaeological sites is considered to be a common feature. Given that a distant-provenance raw material is frequently involved, determination of its source is a basic factor in the search for a better understanding of resource management and for any Political Economy approach. To progress in these directions an overall study should be planned, using selected grindstones with a view to covering diverse sub-zones of the Cogotas I dispersal area, especially because of its considerable distance from the granite basement source. Such a study may today includes diverse analytical procedures combining successive geographic, petrographic, mineralogical and geochemical criteria. To check the plausibility of the proposed methodology, a preliminary test has been carried out on two granite grindstones, obtained at the archaeological excavation at the Castronuño (Valladolid) Cogotian site, which is fifty km away from an inferred source area that was presumably located at Peñausende (Zamora). The result obtained validates the proposed operational process, yielding a generalizable knowledge to other similar situations.

Late Bronze Age in Eastern Iberian Peninsula: Archaeological Bases and Periodization

Research surrounding the transition from II to I millennium cal BC in Eastern Iberian Peninsula has a large and extensive tradition of investigation. However, the chances to do research on this historical process have been limited by the lack of a well contextualized and dated stratigraphic sequence. For this reason, recent studies in this topic have followed the periodic proposals which were developed in closer regions and areas, especially in the South East and North East of the Peninsula. The investigation perspective about the Late Bronze in Eastern Iberian has however now improved, with the development of several archaeological investigations, the increase in the number of sites being dated and more recent studies into the region helping to bring about this change. As such, it is now in the correct state to be able to propose a new periodization and delve into the changes which occurred in the transition between 1500 and 725 cal BC.

Preliminary results of the roman camp of La Cabeza del Cid (Hinojosa, Guadalajara, Spain)

The recent archaeological works in Hinojosa, allowed us to discover a camp from Roman republic period. It is located in the center of the Celtiberian area and its study could open interesting perspectives to study this historical period. This paper shows the results of its preliminary studies.

Los emigrantes en las áreas mineras y las ciudades de Hispania: religión, identidades y difusión cultural

En el presente artículo analizamos los desplazamientos de cultos indígenas hispanos desde distintas áreas de la Península Ibérica hacia los principales lugares de inmigración en Hispania: las áreas mineras y las ciudades. Proponemos que estos grupos de emigrantes rendían culto en su nueva residencia a las deidades que veneraban en sus regiones de procedencia como un medio de preservar su cohesión social y su identidad cultural. La dureza de la vida laboral en las áreas mineras reforzaba la necesidad de fortalecer los lazos culturales.

Caracterização elementar de ligas metálicas em implantes dentários

An ideal biomaterial for dental implants must have very high biocompatibility, which means that such materials should not provoke any serious adverse tissue response. Also, used metal alloys must have high fatigue resistance due the masticatory force and good corrosion resistance. These properties are rendered by using alpha and beta stabilizers, such as Al, V, Ni, Fe, Cr, Cu, Zn. Commercially pure titanium (TiCP) is used often for dental and orthopedic implants manufacturing. However, sometimes other alloys are employed and consequently it is essential to research the chemical elements present in those alloys that could bring prejudice for the health. Present work investigated TiCP metal alloys used for dental implant manufacturing and evaluated the presence of stabilizing elements within existing limits and standards for such materials. For alloy characterization and identification of stabilizing elements it was used EDXRF technique. This method allows to perform qualitative and quantitative analysis of the materials using the spectra of the characteristic X-rays emitted by the elements present in the metal samples. The experimental setup was based on two X- rays tubes (AMPTEK Mini X model with Ag and Au targets), a X-123SDD detector (AMPTEK) and a 0.5mm Cu collimator, developed due to the sample characteristics. The other experimental setup used as a complementary technique is composed of an X-ray tube with a Mo target, collimator 0.65mm and XFlash (SDD) detector - ARTAX 200 (BRUKER). Other method for elemental characterization by energy dispersive spectroscopy (EDS) applied in present work was based on Scanning Electron Microscopy (SEM) EVO® (Zeeis). This method also was used to evaluate the surface microstructure of the sample. The percentual of Ti obtained in the elementary characterization was among 93.35 ± 0.17% and 95.34 ± 0.19 %. These values are considered below the reference limit of 98.635% to 99.5% for TiCP, established by Association of metals centric materials engineers and scientists Society (ASM). The presence of elements Al and V in all samples also contributed to underpin the fact that are not TiCP implants. The values for Al vary between 6.3 ± 1.3% and 3.7 ± 2.0% and for V, between 0.26 ± 0.09% and 0.112 ± 0.048%. According to the American Society for Testing and Materials (ASTM), these elements should not be present in TiCP and in accordance with the National Institute of Standards and Technology (NIST), the presence of Al should be <0.01% and V should be of 0.009 ± 0.001%. Obtained results showed that implant materials are not exactly TiCP but, were manufactured using Ti-Al-V alloy, which contained Fe, Ni, Cu and Zn. The quantitative analysis and elementary characterization of experimental results shows that the best accuracy and precision were reached with X-Ray tube with Au target and collimator of 0.5 mm. Use of technique of EDS confirmed the results of EDXRF for Ti-Al-V alloy. Evaluating the surface microstructure by SEM of the implants, it was possible to infer that ten of the thirteen studied samples are contemporaneous, rough surface and three with machined surface.

Influência da temperatura de calcinação do fosfogesso no desempenho de cimentos supersulfatados

The supersulfated cement (CSS) basically consist of up to 90% blast furnace slag, 10-20% of a source of calcium sulfate and a small amount of alkali activator, covered by European standard EN 15743/2010. Because of this SSC are considered "green cement" low environmental impact. The source of calcium sulfate used in the preparation of CSS can be obtained from natural sources, such as gypsum or from alternative sources (industrial products), such as phosphogypsum. The phosphogypsum is a by-product of the fertilizer industry, used in the production of phosphoric acid. In this process the phosphate rock is treated with sulfuric acid to give as the major product phosphoric acid (H3PO4), gypsum and a small amount of hydrofluoric acid. The chemical composition of gypsum is basically calcium sulfate dihydrate (CaSO4.2H2O), similar to gypsum, because it can be used in this type of cement. To become anhydrous, the calcination of gypsum is necessary. The availability of the source of calcium sulfate to react with the slag is dependent on its solubility that is directly related to its calcination temperature. The solubility of the anhydrous gypsum decreases with increasing calcination temperature. This study investigated the influence of temperature of calcination of phosphogypsum on the performance of CSS. Samples were prepared with 10 and 20% of phosphogypsum calcinated at 350 to 650 ° C using KOH as an alkaline activator at three different concentrations (0.2, 0.5 and 0.8%). The results showed that all mortars presented the minimum values required by EN 15743/2010 for 7 and 28 days of hydration. In general CSS containing 10% phosphogypsum showed slightly better compressive strength results using a lower calcination temperature (350 °C) and curing all ages. The CSS containing 20% of calcined gypsum at 650 °C exhibit satisfactory compressive strenght at 28 days of hydration, but at later ages (56 to 90 days) it strongly reduced. This indicates that the calcination temperature of phosphogypsum has a strong influence on the performance of the CSS.

Modelizado molecular de nanocomposites de matriz polimérica reforzados con nanotubos de carbono

135 p.

A Baixa Estremadura dos finais do IV milénio a.C. até à chegada dos romanos : um ensaio de história regional

Esta obra trata da sucessão cultural registada na Estremadura portuguesa desde a emergência das sociedades complexas do Calcolítico até à chegada dos Romanos, correspondendo a um lapso de tempo entre os finais do IV milénio e os finais do século II a.C. Embora corresponda apenas a intervalo temporal de aproximadamente três mil anos, é o que, no registo material da nossa Pré-História e Proto-História, se afigura mais rico e diversificado de informação, com o desenvolvimento e fixação de regionalismos culturais, que na Estremadura cunharam identidades próprias, as quais persistiram nalguns casos até época recente, no quotidiano dos seus habitantes. A percepção geral desta evolução, bem como as suas determinantes, é o primeiro, e talvez mais importante objectivo desta obra, a par de outros a seguir enunciados: – a génese dos povoados fortificados calcolíticos, em resultado da crescente intensificação económica e da especialização das produções – a Revolução dos Produtos Secundários (RPS), que decorreu ao longo de boa parte do III milénio a.C. – a par do crescimento demográfico, que determinou, por seu turno, a competição inter-grupos, com a consequente necessidade de fortificação; – a monumentalização / fortificação de alguns dos sítios habitados como expressão da coesão social da respectiva comunidade, acompanhada da emergência de diferenciações inter e intra-comunitárias, indício de diferenciação social, em crescente afirmação, decorrente do processo de desenvolvimento económico complexo, característico do Calcolítico; – as arquitecturas defensivas do III milénio a.C., como expressão pública indissociável da monumentalização acima referida: exemplos mais importantes no território estremenho, distribuição geográfica, características principais, semelhanças e diferenças; neste âmbito, importa conhecer as diversas teorias explicativas para o seu surgimento, desde o modelo difusionista e orientalista vigente em Portugal (dos anos 40 aos anos 70), passando pelo modelo indigenista (anos 80), até às formas difusionistas mitigadas, de expressão regional, dos finais da década de 80 em diante, e principais argumentos invocados; – a desarticulação do modelo de sociedade calcolítica, caracterizada pela concentração da população em sítios fortificados ou pelo menos implantados predominantemente em locais altos e defensáveis; – os moldes em que se processou a acentuação das influências mediterrâneas no decurso do Calcolítico (em especial na metade meridional do território): a generalização do comércio transregional calcolítico e a intensificação e especialização das produções, no quadro da Revolução dos Produtos Secundários (RPS), exemplificada pela exploração de jazidas cupríferas, como veículo de difusão de novas técnicas (metalurgia), matérias-primas exógenas (marfim) e artefactos ideotécnicos de características até então desconhecidas (generalização do culto da divindade feminina e correspondentes expressões simbólicas, algumas de âmbito estritamente regional), acompanhada da difusão, de Sul para Norte, de novas arquitecturas funerárias (tholoi); – sobre o Campaniforme, fenómeno cultural com identidade própria da fase média e tardia do Calcolítico estremenho, serão discutidas as características e cronologia da sua emergência, na Estremadura (um dos pólos mais importantes, a nível europeu) no quadro da sociedade calcolítica pré-existente: tipo de povoamento e de necrópoles, bem como as relações estabelecidas com as comunidades de tradição cultural mais antiga; o faseamento interno do “fenómeno”, com base nas diferenças identificadas no registo material (em particular a tipologia das cerâmicas); e principais tipos artefactuais que o integram. O campaniforme deverá ser entendido como uma expressão material específica, associada a um novo tipo de povoamento, que resultou do decréscimo do interesse oferecido pelos sítios fortificados edificados no início do Calcolítico. Neste sentido, corresponde a período de transição para a Idade do Bronze: existem argumentos, com base no registo arqueológico (jóias de ouro, artefactos de prestígio) que ilustram o incremento do processo de diferenciação social, então verificado, ao contrário do que uma abordagem mais superficial, com base simplesmente no reordenamento demográfico, faria supor; – o registo arqueológico do Bronze Pleno configura a acentuação dos regionalismos, apesar de similitudes do sistema de povoamento face ao período imediatamente anterior, o que indicia realidades socioeconómicas comparáveis. Importa, assim, conhecer as principais características dos escassos povoados identificados, bem como a organização social a ele subjacente, a partir dos testemunhos arqueológicos conhecidos, incluindo os de carácter funerário; – segue-se o Bronze Final, período dominado pela plena afirmação do comércio transregional atlântico-mediterrâneo, favorecido pela própria realidade geográfica do território português. Devem valorizar-se os testemunhos materiais desse período e as respectivas balizas cronológicas: Assim, deverão os leitores ficar familiarizados com as produções de carácter atlântico, como as armas, objectos utilitários e respectivas tipologias e com as de cunho mediterrâneo (com destaque para objectos de indumentária e de carácter cultual, embora estes últimos quase se desconheçam na área estremenha), cujo comércio e difusão foi suportado pela existência de solidariedades económicas transregionais, baseadas em prováveis pactos formalmente estabelecidos entre comunidades vizinhas. Os respectivos territórios, de norte a sul do País, apresentar-se-iam cada vez melhor delimitados; o mesmo deverá ter-se verificado na Estremadura. A caracterização da respectiva economia será, por isso, objecto da análise e discussão; embora de base agro-pastoril (com importância evidente na Estremadura dadas as características dos solos e a quase inexistência de minérios de cobre ou de estanho), a produção de peças metálicas de bronze assumiu importância crescente, como se conclui pelas ocorrências conhecidas. O reforço e a consolidação das elites então verificada, eram necessários para a boa gestão de grandes povoados muralhados que despontam no Bronze Final; na Estremadura, embora os testemunhos de tais centros demográficos não sejam particularmente evidentes, no fim da Idade do Bronze desponta um vigoroso povoamento de altura; seria a partir desses locais que as elites da época, de cunho guerreiro, administrariam territórios bem delimitados. Também a existência de outros testemunhos arqueológicos são concorrentes para a percepção da realidade social: as jóias auríferas, tornadas então relativamente frequentes, deixam transparecer influências ora atlânticas ora mediterrâneas, por vezes reunidas numa única peça (técnicas e tipologias decorativas), expressivas das correntes culturais que, então, se faziam sentir na Estremadura; também as armas, são testemunho da afirmação das elites guerreiras, encontrando-se representadas por exemplares cujas principais características devem ser conhecidas. As diversas práticas funerárias, apesar de escassamente representadas, revelam influências continentais (cremação e campos de urnas, já fora da área estremenha, mas dela próxima: caso dos campos de urnas de Tanchoal e de Meijão, Alpiarça) e mediterrâneas (inumações na tholos da Roça do Casal do Meio, Sesimbra), que traduzem um mosaico cultural complexo, reforçando a ideia de se tratar de região receptora de influxos culturais de diversas áreas geográficas em simultâneo: é, no essencial, a comprensão global desta realidade, a um tempo económica, social e cultural, coroando um longo processo de diferenciação social, por um lado e, por outro, de intensificação económica e interacção cultural, que lhe está subjacente, que deverá ter-se presente. Por último, segue-se o estudo e caracterização das principais estações e materiais da Idade do Ferro, de início (I Idade do Ferro) profundamente marcadas pela presença, directa ou indirecta, de colonizadores fenícios; depois, pelos comerciantes de origem púnica (II Idade do Ferro) e, enfim, pelos exércitos itálicos. Trata-se, em suma, de processo de características próprias, sempre determinado pelas influências mediterrâneas, largamente dominantes face às originárias do interior peninsular, as quais cunharam uma realidade cultural com características próprias, que persistiu no decurso da dominação romana.

As ferrarias del rey na Fábrica da Pólvora de Barcarena : as intervenções arqueológicas

As Ferrarias del Rey, em Barcarena, foram o mais bem sucedido dos empreendimentos metalúrgicos reais portugueses dos séculos XV a XVII. Vocacionadas para a metalurgia do ferro e com data de fundação documentada no ano de 1487, constituem o mais antigo complexo oficinal português orientado exclusivamente para a produção de armamento. Para além da sua dimensão, ímpar à época em Portugal, foi a sua componente tecnológica que verdadeiramente diferenciou as Ferrarias das restantes oficinas então existentes.

Estudo e desenvolvimento de um capacitor eletrolítico de nióbio

It seeks to find an alternative to the current tantalum electrolytic capacitors in the market due to its high cost. Niobium is a potential substitute, since both belong to the same group of the periodic table and because of this have many similar physical and chemical properties. Niobium has several technologically important applications, and Brazil has the largest reserves, around 96%. There are including niobium in reserves of tantalite and columbite in Rio Grande do Norte. These electrolytic capacitors have high capacitance specifies, ie they can store high energy in small volumes compared to other types of capacitors. This is the main attraction of this type of capacitor because is growing demand in the production of capacitors with capacitance specifies increasingly high, this because of the miniaturization of various devices such as GPS devices, televisions, computers, phones and many others. The production route of the capacitor was made by powder metallurgy. The initial niobium powder supplied by EEL-USP was first characterized by XRD, SEM, XRF and laser particle size, to then be sieved into three particle size, 200, 400 e 635mesh. The powders were then compacted and sintered at 1350, 1450 and 1550°C using two sintering time 30 and 60min. Sintering is one of the most important parts of the process as it affects properties as porosity and surface cleaning of the samples, which greatly affected the quality of the capacitor. The sintered samples then underwent a process of anodic oxidation, which created a thin film of niobium pentóxido over the whole porous surface of the sample, this film is the dielectric capacitor. The oxidation process variables influence the performance of the film and therefore the capacitor. The samples were characterized by electrical measurements of capacitance, loss factor, ESR, relative density, porosity and surface area. After the characterizations was made an annealing in air ate 260ºC for 60min. After this treatment were made again the electrical measurements. The particle size of powders and sintering affected the porosity and in turn the specific area of the samples. The larger de area of the capacitor, greater is the capacitance. The powder showed the highest capacitance was with the smallest particle size. Higher temperatures and times of sintering caused samples with smaller surface area, but on the other hand the cleaning surface impurities was higher for this cases. So a balance must be made between the gain that is achieved with the cleaning of impurities and the loss with the decreased in specific area. The best results were obtained for the temperature of 1450ºC/60min. The influence of annealing on the loss factor and ESR did not follow a well-defined pattern, because their values increased in some cases and decreased in others. The most interesting results due to heat treatment were with respect to capacitance, which showed an increase for all samples after treatment

Synthesis and characterization of biodegradable thermoplastic elastomers for medical applications: Novel copolyesters as an alternative to polylactide and poly (e-caprolactone)

421 p.