Obtenção de ferrita de cobalto através de dois métodos de síntese: método de complexação combinando EDTA/Citrato e método hidrotérmico

In this work it was synthesized and characterized the cobalt ferrite (CoFe2O4) by two methods: complexation combining EDTA/Citrate and hydrothermal investigating the influence of the synthesis conditions on phase formation and on the crystallite size. The powders were mainly characterized by x-ray diffraction. In specific cases, it was also used scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), x-ray fluorescence (XRF) and isotherms of adsorption and desorption of nitrogen (BET method). The study of the crystallite size was based on the interpretation of x-ray diffractograms obtained and estimated by the method of Halder-Wagner-Scherrer and Langford. An experimental design was made in order to assist in quantifying the influence of synthesis conditions on the response variables. The synthesis parameters evaluated in this study were: pH of the reaction medium (8, 9 and 10), the calcination temperature (combined complexation method EDTA/Citrate 600°C, 800°C and 1000°C), synthesis temperature (hydrothermal method 120°C, 140°C and 160°C), calcination time (combined complexation method EDTA/Citrate - 2, 4 and 6 hours) and time of synthesis (hydrothermal method 6, 15 and 24 hours). By the hydrothermal method was possible to produce mesoporous powders with high purity, with an average crystallite size up to 7 nm, with a surface area of 113.44 m²/g in the form of pellets with irregular morphology. By using the method of combined complexation EDTA/Citrate, mesoporous powders were produced with greater purity, crystallite size up to 22nm and 27.95 m²/g of surface area in the form of pellets with a regular morphology of plaques. In the experimental design was found that the hydrothermal method to all the studied parameters (pH, temperature and time) have significant effect on the crystallite size, while to the combined complexation method EDTA/Citrate, only temperature and time were significant

Avaliação do comportamento em fadiga de juntas estruturais de ligas de Al2024T3 coladas com adesivo epóxi

Ligas de alumínio são extensamente usadas em partes aeronáuticas devido às boas propriedades mecânicas e baixa densidade. Estas partes devem ser unidas para formar conjuntos maiores. Uma junta estrutural é definida como um segmento de estrutura que provê um meio de transferir carga de um elemento estrutural para outro. A maioria das juntas aeronáuticas é mecanicamente fixada com múltiplos prendedores (parafusos ou rebites). Estas juntas apresentam uma alta concentração de tensões ao redor do prendedor, porque a transferência de carga entre elementos da junta acontece em uma fração da área disponível. Por outro lado, as cargas aplicadas em juntas adesivas são distribuídas sobre toda a área colada e reduz os pontos de concentração de tensão. Juntas são a fonte mais comum de falhas estruturais em aeronaves e quase todos os reparos envolvem juntas. Portanto, é importante entender todos os aspectos de projeto e análise de juntas. O objetivo deste trabalho é comparar estaticamente juntas estruturais de ligas de Al2024-T3 em três condições: juntas mecanicamente rebitadas, juntas coladas e uma configuração híbrida rebitada e colada. Foi usada a norma NASM 1312-4 para confecção dos corpos-de-prova. Além disso, foram conduzidos testes de fadiga, sob amplitude de carregamento constante e razão de tensão igual a 0,1 para avaliar a eficiência dos elementos estruturais durante sua vida em serviço. Os resultados mostraram que a configuração híbrida apresenta maior resistência estática e uma vida em fadiga superior à configuração colada.

Desenvolvimento de um novo complexo macrocíclico do sistema cobalto cyclam

In this work were synthesized and studied the spectroscopic and electrochemical characteristics of the coordination compounds trans-[Co (cyclam)Cl2]Cl, trans- Na[Co(cyclam)(tios)2], trans-[Co(en)2Cl2]Cl and trans-Na[Co(en)2(tios)2], where tios = thiosulfate and en = ethylenediamine. The compounds were characterized by: Elemental Analysis (CHN), Absorption Spectroscopy in the Infrared (IR), Uv-Visible Absorption Spectroscopy, Luminescence Spectroscopy and Electrochemistry (cyclic voltammetry). Elemental Analysis (CHN) suggests the following structures for the complex: trans- [Co(cyclam)Cl2]Cl.6H2O and trans-Na[Co(cyclam)(tios)2].7H2O. The electrochemical analysis, when compared the cathodic potential (Ec) processes of the complexes trans- [Co(cyclam)Cl2]Cl and trans-[Co(en)2Cl2]Cl, indicated a more negative value (-655 mV) for the second complex, suggesting a greater electron donation to the metal center in this complex which can be attributed to a greater proximity of the nitrogen atoms of ethylenediamine in relation to metal-nitrogen cyclam. Due to the effect of setting macrocyclic ring to the metal center, the metal-nitrogen bound in the cyclam are not as close as the ethylenediamine, this fact became these two ligands different. Similar behavior is also observed for complexes in which the chlorides are replaced by thiosulfate ligand, trans-Na[Co(en)2(tios)2] (-640 mV) and trans-Na[Co(cyclam)(tios)2] (-376 mV). In absorption spectroscopy in the UV-visible, there is the band of charge transfer LMCT (ligand p d* the metal) in the trans-Na[Co(cyclam)(tios)2] (350 nm, p tios  d* Co3+) and in the trans-Na[Co(en)2(tios)2] (333 nm, p tios d* Co3+), that present higher wavelength compared to complex precursor trans- [Co(cyclam)Cl2]Cl (318 nm, pCl  d* Co3+), indicating a facility of electron density transfer for the metal in the complex with the thiosulfate ligand. The infrared analysis showed the coordination of the thiosulfate ligand to the metal by bands in the region (620-635 cm-1), features that prove the monodentate coordination via the sulfur atom. The νN-H bands of the complexes with ethylenediamine are (3283 and 3267 cm-1) and the complex with cyclam bands are (3213 and 3133 cm-1). The luminescence spectrum of the trans-Na[Co(cyclam)(tios)2] present charge transfer band at 397 nm and bands dd at 438, 450, 467, 481 and 492 nm.

Estudo das ligas titânio-zircônio resultantes do processo de fundição plasma-skull para aplicações como biomateriais

The aim of this work was to study a series of 11 different compositions of Ti-Zr binary alloys resistance to aggressive environment, i. e., their ability to keep their surface properties and mass when exposed to them as a way to evaluate their performance as biomaterials. The first stage was devoted to the fabrication of tablets from these alloys by Plasma-Skull casting method using a Discovery Plasma machine from EDG Equipamentos, Brazil. In a second stage, the chemical composition of each produced tablet was verified. In a third stage, the specimen were submitted to: as-cast microstructure analysis via optical and scanning electron microscopy (OM and SEM), x-ray dispersive system (EDS) chemical analysis via SEM, Vickers hardness tests for mechanical evaluation and corrosion resistence tests in a 0.9% NaCl solution to simulate exposition to human saliva monitored by open circuit potential and polarization curves. From the obtained results, it was possible to infer that specimens A1 (94,07 wt% Ti and 5,93% wt% Zr), A4 (77,81 wt % Ti and 22,19 wt % Zr) and A8 (27,83 wt% Ti and 72,17 wt% Zr), presented best performance regarding to corrosion resistance, homogeneity and hardness which are necessary issues for biomaterials to be applied as orthopedic and odontological prosthesis

Síntese e Caracterização de Titanatos de Cobalto e Níquel, dopados com Praseodímio, obtidos a partir da decomposição de Nitrilotriacetatos

In recent years, studies about the physicochemical properties of mixed oxides, call attention of the scientific community, properties like as piezoelectricity, photoluminescence, or applications as catalysts, arise in these compounds, when their chemical compositions are modified, in this context some routes are employed in the synthesis of these materials, among which can be cited these methods: ceramic, combustion, co-precipitation, Pechini or polymeric precursor method, hydrothermal, sol-gel; these routes are divided into traditional routes or chemical routes. In this work were synthesized oxides with variable composition, from the thermal decomposition of titanium, cobalt, nickel and praseodymium nitrilotriacetates. The nitrilotriacetates were characterized by IR Spectroscopy (FTIR), Thermogravimetric (TG/ DTG) and Differential Scanning Calorimetry (DSC), while oxides have been characterized by X-ray diffraction (XRD), Spectrofluorimetry and IR Spectroscopy (FTIR). From FTIR data, it was demonstrated that the displacement of the band corresponding to the carboxylate group (νCOOH) at 1712 cm-1, present in nitrilotriacetic acid (H3NTA), for 1680-1545 cm-1, these stretches are characteristics of coordinated nitrilotriacetates, By thermal analysis (TG/DTG /DSC), it was suggested, that in an oxidizing atmosphere (air) oxides are obtained at lower temperatures than in an inert atmosphere N2(g). By results from X-ray Diffraction (XRD), it was determinated that the oxides are crystalline and the predominant phases obtained are summarized titanate phases rutile and ilmenite. By fluorimetry was observed that the intensity of emission bands are directly proportional to the concentration of ions Ni2+, Co2+ and Pr3+, and IR spectroscopy (FTIR) from oxides, demonstrated the disappearance of characteristic bands by nitrilotriacetates, determining the complete decomposition of the nitrilotriacetates in oxides

Complexos metálicos de cobalto, níquel e cobre com a Pirazina-2-carboxamida e 4- hidrazida ácida piridincarboxílica: síntese e caracterização

This work involved the synthesis, characterization and proposing the molecular structure of coordination compounds involving ligands pyrazine-2-carboxamide (PZA) and 4- hydrazide acidic pyridine carboxylic (INH) and metals of the first transition series (M = Co2+, Ni2+ and Cu2+). For the characterization of the compounds used were analytical techniques such as infrared absorption spectroscopy average (FT-IR) molar conductivity measurements, CHN elemental analysis, EDTA Complexometric, measurement of melting point, X-ray diffraction by powder method, Thermogravimetry (TG) and Differential Thermal Analysis (DTA) and Simultaneous Differential Scanning Calorimetry (DSC). The absorption spectra in the infrared region suggested that the ligand coordination to the metal center occurs through the carbonyl oxygen atom and nitrogen alpha pyrazine ring to those complexes formed with PZA. For INH complexes with metal-ligand coordination is through the carbonyl oxygen and nitrogen of the terminal hydrazide grouping. The conductivity measurements of the complexes in aqueous solution they suggest to all behavior of the type 1:2 electrolytes, and conduct of non-electrolytes in acetonitrile. The results obtained by CHN elemental analysis and EDTA Complexometric allowed to infer the stoichiometry of the compounds synthesized. For all of the complexes obtained was possible to record the melting points, neither of which melted near the melting temperature of the free ligands. The X-ray diffraction showed that the complexes of pyrazinamide exhibited diffraction lines, suggesting that these compounds are crystalline, while compounds of isoniazid, with the exception of cobalt, exhibited diffraction lines, indicating that they are crystalline. The results from the TG-DTA and DSC allowed information regarding the dehydration and thermal decomposition of these complexes

Otimização da síntese de nanoferritas de nizn dopada com cobre e cobalto

Different compositions of Ni0,5-xCuxZn0,5Fe2O4 and Ni0,5-xCoxZn0,5Fe2O4 0 ≤ x ≤ 0.3 were synthesized ferrite y the citrate precursor method. The stoichiometric compositions were calcined in air at 350°C and then pressed into pellets and toroids. The pressed samples were sintered at temperatures of 1000, 1050 and 1100°C/3h in air control at the speed of heating and cooling. The calcined powders were characterized by XRD, TGA / DTG, FTIR, SEM and vibrating sample magnetometry (VSM) and the sintered samples by XRD, SEM, MAV, density and measurements of permeability and magnetic losses. There was pure phase formation ferrimagnetism applied at all temperatures except for A-I composition at all sintering temperatures and A-II only at a temperature of 1100°C. Crystallite sizes were obtained by Rietveld analysis, nanometer size from 11 to 20 nm for the calcined powders. For SEM, the sintered samples showed grain size between 1 and 10 micrometers. Bulk density (ρ) of sintered material presented to the Families almost linear behavior with increasing temperature and a tendency to decrease with increasing concentration of copper, different behavior of the B Family, where the increase in temperature decreased the density. The magnetic measurements revealed the powder characteristics of a soft ferrimagnetic material. Two processes of magnetization were considered, the superparamagnetism at low temperatures (350°C) and the formation of magnetic domains at higher temperatures. Obtaining the best parameters for P and B-II magnetic ferrites at high temperatures. The sintered material at 1000°C showed a relative permeability (μ) from 50 to 800 for the A Family and from 10 to 600 for the B Family. The samples sintered at 1100°C, B Family showed a variation from 10 to 1000 and the magnetic loss (tan δ) of A and B Families, around of 1. The frequency response of the toroidal core is in the range of 0.3 kHz. Several factors contribute to the behavior of microstructure considering the quantities μ and tan δ, such as the grain size, inter-and intragranular porosity, amount of grain boundary and the aspects of the dynamics of domain walls at high frequencies.

Síntese e caracterização de ferritas de níquel dopadas com cobalto e efeito da substituição nas suas propriedades magnéticas

The ferrite composition Ni1 - xCoxFe2O4 (0 ≤ x ≤ 0.75) were obtained by the method of microwave assisted synthesis and had their structural and magnetic properties evaluated due to the effect of the substitution of Ni by Co. The compounds were prepared: according to the concept of chemical propellants and heated in the microwave oven with power 7000kw. The synthesized material was characterized by absorption spectroscopy in the infrared (FTIR), Xray diffraction (XRD) using the Rietveld refinement, specific surface area (BET) , scanning electron microscopy (SEM) with aid of energy dispersive analysis (EDS) and magnetic measurements (MAV). The results obtained from these techniques confirmed the feasibility of the method of synthesis employed to obtain the desired spinel structure, the ferrite, nickel ferrite as for nickel doped with cobalt. The results from XRD refinement ally showed the formation of secondary phases concerning stages α - Fe2O3, FeO, (FeCo)O e Ni0. On the other hand, there is an increase in crystallite size with the increase of cobalt in systems, resulting in an increased crystallinity. The results showed that the BET systems showed a reduction in specific surface area with the increase of cobalt and from the SEM, the formation of irregular porous blocks and that the concentration of cobalt decreased the agglomerative state of the system. The magnetic ferrites studied showed different characteristics according to the amount of dopant used, ranging from a very soft magnetic material (easy magnetization and demagnetization ) - for the system without cobalt - a magnetic material with a little stiffer behavior - for systems containing cobalt. The values of the coercive field increased with the increasing growth of cobalt, and the values of saturation magnetization and remanence increased up to x = 0,25 and then reduced. The different magnetic characteristics presented by the systems according to the amount of dopant used, allows the use of these materials as intermediates magnetic

Determinação da temperatura de solubilização da prata em ligas de Cu-Al-Ag por medidas de resistência elétrica

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Nanopartículas magnéticas: o cobalto

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Nodulação e absorção de nitrogênio pelo amendoim em resposta à calagem, cobalto e molibdênio

A resposta do amendoim à calagem tem sido atribuída ao fornecimento de cálcio, mas também tem sido observada maior absorção de nitrogênio. Um experimento foi desenvolvido em casa de vegetação, em vasos de polietileno, utilizando-se um Latossolo Vermelho distrófico textura média, para estudar os efeitos da calagem e da aplicação de cobalto e molibdênio sobre a nodulação e a absorção de nitrogênio pelo amendoim, cultivar Tatu. O delineamento experimental empregado foi o de blocos ao acaso, em esquema fatorial 4x3, com quatro repetições. Os tratamentos do fatorial constituíram-se de quatro aplicações de nutrientes nas sementes (sem aplicação; 0,16 g kg-1 de Co; 0,58 g kg-1 de Mo e 0,16 + 0,58 g kg-1 de Co e Mo, respectivamente) e três doses de calcário (0, 4 e 6 t ha-1). A aplicação de cobalto nas sementes não exerceu efeito sobre a nodulação e a absorção de nitrogênio pelo amendoim. A calagem aumentou a absorção de nitrogênio pelo amendoim, provavelmente por causar melhoria na fixação simbiótica do N2, em decorrência da formação de maior número de nódulos. Apesar do molibdênio ter aumentado a matéria seca de nódulos na planta de amendoim, a sua aplicação não influenciou a absorção de nitrogênio, mostrando que a redução da toxicidade de manganês pela calagem foi mais importante do que o aumento da disponibilidade de molibdênio para a formação de nódulos e a fixação simbiótica do N2.

Síntese e caracterização do sistema ZrO2-SiO2 com adição de cobalto para uso como pigmentos cerâmicos

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Ligas Acadêmicas e formação médica: contribuições e desafios

Nos últimos anos tem havido um considerável aumento do número de ligas acadêmicas atuantes nos cursos de graduação em medicina no Brasil. Esse fenômeno, no entanto, não vem sendo acompanhado de adequada reflexão sobre seus determinantes, o papel das ligas dentro das instituições, ou mesmo sua função pedagógica. A partir destas constatações, os autores analisam a precária literatura sobre o tema, descrevem a experiência das ligas acadêmicas da Faculdade de Medicina de Botucatu - Unesp e refletem a respeito do papel destas na formação médica, na tentativa de suprir um pouco dessa lacuna e contribuir para esta importante discussão.

Influência do escoamento estático (CREEP) na dureza do amálgama. Efeito de ligas e regióes de medida.

The authors studied the CREEP of 5 amalgam alloys (1 conventional and 4 with high cooper) by the application os static load of 36 MPa in 478 mm specimens, 7 days old. After CREEP test, the samples were included in acrylic resin and Vickers hardness determined by three penetrations for each portion (cervical, medium and occlusal). Samples not submitted to the creep test was used with control. They concluded that no statistic difference was found in creep test but in Vickers test all the studied materials showed different hardness averages. The load application to samples increased the hardness of all the studied materials.

Influência de diferentes agentes de fixação na resistência de união, por tração, de ligas metálicas fixadas à dentina.

They were casted pieces using three kinds of alloy (Ni-Cr, Ag-Sn and Cu-Al) with circular and smooth surface. They were cemented to human teeth, on occlusal surface, grounded at dentin level, through three different materials kind (zinc polycarboxylate cement, glassionomer cement and composite). After 24 hours storing, the samples were subjected to the tensile test. The results showed that the samples cemented with composite and the casts made with Ag-Sn alloy had higher bond strength.