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

Síntese, caracterização de ferritas espinélio com propriedades magnéticas e absorvedoras de microondas

Were synthesized spinel-type ferrites with general formula Ni0,8Mg0.2-xMxFe2O4, where M represents the doping Mn, Co or Mn + Co simultaneously, x ranges for the values 0.02, 0.05 and 0.1. The value of x was divided by 2 in cases where M equals Mn and Co conjugates. We used the citrate precursor method and heat treatment to obtain the phases at 1100°C. The materials were characterized by XRD, TGA/ DTGA, SEM, MAV and reflectivity measurements by the method of waveguide. Powders to 350°C/3.5 h were crystalline and nanosized. According to the results this temperature all powders have a percentage of ferrite phase over 90%. The composition had the addition of Mn and Co simultaneously showed a higher percentage of secondary phase NiO, 5.8%. The TGA/DTGA curves indicate that this sample reached phase (s) crystalline (s) at lowest temperatures. The X-ray diffractograms of the samples calcined at 350°C and 1100°C were treated with the Rietveld refinament technique. The powders calcined at 1100 °C/3h in air show to be 100% except spinel phase composition with 0.02 doping. The micrographs show clusters of particles with sizes smaller than 1 μm in calcination temperature of 1100°C which agreed with the result of Rietveld refinement. In the compositions doped with Mn were higher values of magnetization (45.90 and 53.20 Am2/kg), which did not cause high microwave absorption. The theoretical calculation of magnetization (MT) was consistent with the results, considering that there was agreement between the increase of magnetization experimental and theoretical. It was observed that there was the interrelation of the final effect of absorption with the thickness of MARE, the composition of ferrimagnetic materials and in particular the specific values of frequency. The analysis shows that the reflectivity increases in the concentration of cobalt increased the frequency range and also for absorption 10.17 GHz and 84%, respectively. The best result of chemical homogeneity and the value of 2.96 x 10-2 tesla coercive field were crucial for high performance ferrite absorber with 0.1 cobalt. The Cobalt has high magnetocrystalline anisotropy, it is associated with an increased coercive field, Hc. Therefore, this property improves the results of reflectivity of spinel ferrites

Síntese e caracterização de redes metalorgânicas baseadas em zinco e ácidos benzenodicarboxílicos

Metal Organic Frameworks (MOFs) are supramolecular structures consisted of ions or metal clusters coordinated to organic ligands which are repeated in two or three dimensions. These structures have atracted much attention due to their properties such as low density, high specific surface area and large volume of pores. In this work, MOFs consisted of zinc clusters connected by ditopic ligands, terephthalic acid (1,4- H2BDC) or isophthalic acid (1,3-H2BDC) were synthesized. To obtain the proposed materials, different routes and synthetic parameters were tested, such as the molar ratio of the precursors, the addition of template molecules, the type of solvente, the addition of organic base or the type of a counter-ion of Zn salt. It was found that the variation of these parameters led to the formation of different metalorganic structures. The solids obtained were characterized by XRD, SEM and IR. For the samples identified as MOF- 5, it was verified that the structure was composed of both interpenetrated and non interpenetrated structures. These samples showed a low stability, becoming totally transformed into another structure within less than 72 hours. The addition of the nickel and/or cobalt was found to be a promissing method for increasing the stability of MOF- 5, which in this case, still remained unconverted to another structure even after 15 days of exposure to air. The samples prepared from 1,3-H2BDC were probably new, still unknown Metal Organic Frameworks

Síntese e caracterização da ferrita de MnZn obtida pelo método dos citratos precursores

It was synthesized MnZn ferrite with general formulae Mn1-xZnxFe2O4 (mol%), 0,3 ≤ x ≤ 0,7 by using the citrate precursor method. The precursors decomposition was studied by thermogravimetric analysis (TGA), differential thermogravimetric analysis (DTG), differential thermal analysis (DTA) and Fourier transform infrared (FTIR) of powder calcined at 350ºC/3,5h. X-ray diffraction pattern (XRD) of samples was done from 350 to 1200ºC/2h using various atmospheres. The power calcined at 350ºC/3,5h formed spinel phase. It is necessary atmosphere control to avoid secondary phase such as hematite. From 900 to 1200ºC was obtained 90,66 and 100% of MnZn spinel ferrite phase, respectively. Analysis by dispersive energy scanning (EDS) at 350ºC shows high Mn and Zn dispersion, indicating that the diffusion process was homogeneous. Semi-quantitative analysis by EDS verified that despite the atmosphere control during calcinations at high temperatures (< 800ºC) occurred ZnO evaporation causing stoichiometric deviation. Vibrating sample magnetometer (VSM) measures show soft ferrite material characteristics with Hc from 6,5 x 10-3 to 11,1 x 10-2 T. Saturation magnetization (Ms) and initial permeability (µi) of MnZn spinel phase obtained, respectively, from 14,3 to 83,8 Am2/kg and 14,1 to 62,7 (Am2/kg)T

Caracterização estrutural de Perovskitas Lax-1AxCoO3 (x=0 e 0,2) ,dopadas com cálcio e bario, por espectroscopia de absorção de raios X (XAS).

In this work, the structures of LaCoO3, La0,8Ba0,2CoO3 and La0,8Ca0,2CoO3 perovskites were characterized as a function of temperature (LaCoO3 structure being analyzed only at room temperature). The characterization of these materials were made by X-Ray Absorption Spectroscopy (XAS), in the cobalt K-edge, taking into account the correlated Einstein model X-ray absorption fine structure (EXAFS). The first part of the absorption spectrum corresponded the X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS). These materials were prepared by the combustion method. The combustion products were calcinated at 900 0C, for 6 hours in air. Noted that the sample LaCoO3 at room temperature and samples doped with Calcium and Barium in the temperature range of 50 K to 298 K showed greater distortion to monoclinic symmetry with space group I2/a. However, the sample doped with barium at the temperatures 50 K, 220 K, and 260 K showed a slight distortion to rhombohedral symmetry with space group R-3c. The La0,8Ca0, 2CoO3 structure was few sensitive to temperature variation, showing a higher local distortion in the octahedron and a higher local thermal disorder. These interpretations were in agreement with the information electronic structural on the XANES region and geometric in the EXAFS region

Avaliação da remoção catalítica de compostos orgânicos monoaromáticos em água utilizando materiais nanoestruturados de sílica

Statistics of environmental protection agencies show that the soil has been contaminated with problems often resulting from leaks, spills and accidents during exploration, refining, transportation and storage oil operations and its derivatives. These, gasoline noteworthy, verified by releasing, to get in touch with the groundwater, the compounds BTEX (benzene, toluene, ethylbenzene and xylenes), substances which are central nervous system depressants and causing leukemia. Among the processes used in remediation of soil and groundwater contaminated with organic pollutants, we highlight those that use hydrogen peroxide because they are characterized by the rapid generation of chemical species of high oxidation power, especially the hydroxyl radical ( OH), superoxide (O2 -) and peridroxil (HO2 ), among other reactive species that are capable of transforming or decomposing organic chemicals. The pH has a strong effect on the chemistry of hydrogen peroxide because the formation of different radicals directly depends on the pH of the medium. In this work, the materials MCM-41 and Co-MCM-41 were synthesized and used in the reaction of BTEX removal in aqueous media using H2O2. These materials were synthesized by the hydrothermal method and the techniques used to characterize were: XRD, TG/DTG, adsorption/desorption N2, TEM and X-Ray Fluorescence. The catalytic tests were for 5 h of reaction were carried out in reactors of 20 mL, which was accompanied by the decomposition of hydrogen peroxide by molecular absorption spectrophotometry in the UV-Vis, in addition to removal of organic compounds BTEX was performed as gas chromatography with detection photoionization and flame ionization and by static headspace sampler. The characterizations proved that the materials were successfully synthesized. The catalytic tests showed satisfactory results, and the reactions containing BTEX + Co-MCM-41 + H2O2 at pH = 12.0 had the highest percentages of removal for the compounds studied

Estudo de materiais mesoporosos funcionalizados com diferentes aminas para captura do dióxido de carbono através do processo de adsorção

Intensive use of machinery and engines burning fuel dumps into the atmosphere huge amounts of carbon dioxide (CO2), causing the intensification of the greenhouse effect. Climate changes that are occurring in the world are directly related to emissions of greenhouse gases, mainly CO2, gases, mainly due to the excessive use of fossil fuels. The search for new technologies to minimize the environmental impacts of this phenomenon has been investigated. Sequestration of CO2 is one of the alternatives that can help minimize greenhouse gas emissions. The CO2 can be captured by the post-combustion technology, by adsorption using adsorbents selective for this purpose. With this objective, were synthesized by hydrothermal method at 100 °C, the type mesoporous materials MCM - 41 and SBA-15. After the synthesis, the materials were submitted to a calcination step and subsequently functionalized with different amines (APTES, MEA, DEA and PEI) through reflux method. The samples functionalized with amines were tested for adsorption of CO2 in order to evaluate their adsorption capacities as well, were subjected to various analyzes of characterization in order to assess the efficiency of the method used for functionalization with amines. The physic-chemical techniques were used: X- ray diffraction (XRD), nitrogen adsorption and desorption (BET/BJH), scanning electron microscopy (SEM), transmission electron microscopy (TEM), CNH Analysis, Thermogravimetry (TG/DTG) and photoelectron spectroscopy X-ray (XPS). The CO2 adsorption experiments were carried out under the following conditions: 100 mg of adsorbent, at 25 °C under a flow of 100 ml/min of CO2, atmospheric pressure and the adsorption variation in time 10-210 min. The X-ray diffraction with the transmission electron micrographs for the samples synthesized and functionalized, MCM-41 and SBA-15 showed characteristic peaks of hexagonal mesoporous structure formation, showing the structure thereof was obtained. The method used was efficient reflux according to XPS and elemental analysis, which showed the presence of amines in the starting materials. The functionalized SBA -15 samples were those that had potential as best adsorbent for CO2 capture when compared with samples of MCM-41, obtaining the maximum adsorption capacity for SBA-15-P sample

Síntese e caracterização de pós Ba(x)Sr(1-x)Co0,8Fe0,2O3- através do método de coprecipitação via oxalato

Ceramic powders based on oxides of perovskite-type structure is of fundamental interest nowadays, since they have important ionic-electronic conductivity in the use of materials with technological applications such as gas sensors, oxygen permeation membranes, catalysts and electrolytes for solid oxide fuel cells (SOFC). The main objective of the project is to develop nanostructured ceramic compounds quaternary-based oxide Barium (Br), Strontium (Sr), Cobalt (Co) and Iron (Fe). In this project were synthesized compounds BaxSr(1-x)Co0, 8Fe0,2O3- (x = 0.2, 0.5 and 0.8) through the oxalate co-precipitation method. The synthesized powders were characterized by thermogravimetric analysis and differential thermal analysis (TGADTA), X-ray diffraction (XRD) with the Rietveld refinement using the software MAUD and scanning electron microscopy (SEM). The results showed that the synthesis technique used was suitable for production of nanostructured ceramic solid solutions. The powders obtained had a crystalline phase with perovskite-type structure. The TGA-DTA results showed that the homogeneous phase of interest was obtained temperature above 1034°C. It was also observed that the heating rate of the calcination process did not affect the elimination of impurities present in the ceramic powder. The variation in the addition of barium dopant promoted changes in the average crystallite size in the nanometer range, the composition being BSCF(5582) obtained the lowest value (179.0nm). The results obtained by oxalate co-precipitation method were compared with those synthesis methods in solid state and EDTA-citrate method

Obtenção e caracterização de filmes SnO2 depositados em vidro borosilicato por silk-screen modificado: SnCl2.2H2O como precursor

O presente trabalho tem como objetivo investigar as características de filmes de SnO2 depositados em substrato de vidro borosilicato por um processo de silk-screen modificado para obtenção de espessura fina compatível com a aplicação em células solares policristalinas de baixo custo. O filme de SnO2 é um dos mais apropriados para obtenção de vidro TCO (transparent conductive oxide) para uso em células solares devido a sua baixa resistividade elétrica e alta transmitância, sendo quimicamente inerte, mecanicamente duro e tem resistência a altas temperaturas, o que facilita então a calcinação das amostras entre 500º C a 550º C. Os filmes foram obtidos a partir de uma solução precursora básica, preparada pela dissolução de SnCl2.2H2O em Etanol (99,5 %). Foi realizado um planejamento fatorial 2(3-1) para analisar a influência dos parâmetros concentração da solução precursora (CETN), temperatura de calcinação (TC) e taxa de aquecimento (tX) na calcinação, sendo a concentração CETN o parâmetro que apresentou maior efeito sobre os parâmetros de respostas investigados: espessura do filme (ω), resistividade de superfície (ρ) e a transmitância relativa (θ). Foi possível obter com a metodologia utilizada, filmes com espessuras da ordem de 1 Nm com resistividade de superfície de 10 / e transmitância relativa entre 70 e 80 %.

Síntese e caracterização de niobiosilicatos para produção de biocombustível

The mesoporous materials has been an special attention, among them was discovered in the 1990´s the mesoporous molecular sieve of SBA-15 type. The good features of the SBA- 15 makes this material very promising in catalysis, however, due to the absence of native active sites, it has low catalytic activity. In this way, different metals and oxides have been included in this molecular sieve as a means of introducing active sites and increase its catalytic activity. Among the oxides that are being researched, there is the niobium oxide, which presents strong acid sites and exists in abundance. Brazil is the largest producer of the mineral. On the other hand, the production of biofuels has been desired, but it requires the development of new catalysts for this purpose. The aim of this work was to develop silicate of niobium by impregnation and by new synthesis method for application in the cracking of moringa oil. The methodology consisted of inserting the niobium oxide either by postsynthesis process using wet impregnation and direct insertion. For direct insert a new method was developed for pH adjustment, being tested different pH, and the pH 2.2 was used different ratios of Si/Nb. The materials were characterized by different techniques such as: XRD, N2 adsorption, SEM, EDS, UV-visible, TG/DTG, DSC, TEM, acidity by thermodesorption of n-butilamine and FTIR. After this part of the catalysts developed by the two methods were tested in the thermocatalytic cracking of moringa oil, being used a simple distillation. All silicates of Niobium obtained showed a highly ordered structure, having high specific areas, good distribution of pore diameters, beyond present a morphology in the form of fibers. In the catalysts after synthesis was observed that the niobium inserted has so as octahedrally and tetrahedrally coordinated, demonstrating that there were also oxides formed on the external surface of SBA-15. The materials obtained in the direct synthesis are only tetrahedrally coordinated. The new synthesis method of pH adjusting by using the buffer solution for it, proved to be very efficient for the production of such materials, because the materials obtained showed characteristics and structures similar to the molecular sieve of SBA-15 type. Among the pH tested the material that presented better characteristics was synthesized at pH 2.2. The application of these materials in catalytic cracking showed a higher formation of organic liquids when compared to thermal cracking, in addition to significantly reducing the acidity and residues formed, demonstrating that the use of silicates of Niobium increases both the conversion and the selectivity of the products.

Caracterização mecânica, térmica e acústica de um compósito que utiliza rejeitos de mármore, granito e EPS para a fabricação de blocos para a construção civil

The use of composite materials for the construction industry has been the subject of numerous scientific papers in Brazil and in the world. One of the factors that motivate this quest is the housing deficit that countries especially the third world face. In Brazil this deficit reaches more than 6.5 million homes, around 12% of all US households . This paper presents a composite that was obtained from waste generated in processes for the production of granite and marble slabs, cement, gypsum, sand, crushed EPS and water. These wastes cause great damage to the environment and are thrown into landfi lls in bulk. The novelty of the work is in the combined study thermal, mechanical and acoustic composite obtained in real situation of rooms that are part of an experimental housing. Many blocks were made from cement compositions, plaster, foam, sand, marb le and / or granite, preliminary tests of mechanical and thermal resistance were made by choosing the most appropriate proportion. Will be given the manufacturing processes and assembly units 500 units 10 x 80 x 28 cm produced for the construction of an ex perimental home. We studied what kind of block and residue, marble or granite, made it more feasible for the intended purpose. The mechanical strength of the produced blocks were above 3.0 MPa. The thermal resistance of the blocks was confirmed by the maxi mum temperature difference between the inner and outer walls of rooms built around 8.0 ° C. The sound absorption for optimal room was around 31%. Demonstrated the feasibility of using the blocks manufactured with composite material proposed for construction.

Síntese e caracterização de catalisadores baseados em vermiculita modificada com ferro: aplicação em processos do tipo foto-fenton

Clays are materials with specific properties that make them promising for various studies. In this work we used the vermiculite clay as support for iron compounds, in order to obtain promising materials for application in the heterogeneous type photo-Fenton process. In all, the study included six solid, starting from the vermiculite (V0) was obtained calcined vermiculite (V0-C), the mixed material (V0/β-FeOOH) formed by vermiculite more akaganeite, exchanged vermiculite (v0t-C), vermiculite impregnated Wet (V0u-C) and V0u-CL that is the solid obtained by impregnating with a back washing. The solids of the study had their physical and chemical characteristics investigated by the following characterization techniques: X-Ray Diffraction (XRD), Infrared Spectroscopy (IR), Energy Dispersive Spectroscopy (EDS), X-Ray Fluorescence Spectroscopy (XRF), UV-Vis by Diffuse Reflectance (DR UV-Vis), Thermogravimetric Analysis (TGA) and Scanning Electron Microscopy (SEM). The V0 material showed three distinct phases, which are the very vermiculite, hidrobiotite and biotite, the last two phases are part of the geological of formation process vermiculite. The solids obtained after the modification showed an increase in the amount of iron present in the clay, these being quantities important for application in photocatalysis. The micrographs and EDS data, show that after treatment of addition of the metal , the iron was intercalary in structure of vermiculite for solid V0t-C and V0u-C, however, this did not occur with mixed material. In the photoFenton process, was observed a maximum removal of 88.8% of the dye methylene blue coloring for the catalyst V0/β-FeOOH, while for the other solids was obtained values between 76.8 and 62.6%, compared to 37.8% of discoloration without the presence of catalyst. Therefore, it is concluded that the vermiculite clay presents as a good catalyst and iron support for the, beyond of presenting a low cost because of its high abundance.

Síntese e caracterização de PSFC (Pr0,5Sr0,5Fe1-xCuxO3-δ, sendo x=0,2 e x=0,4) para aplicação como catodo de células a combustível de óxido sólido

The PSFC (Pr0.5Sr0.5Fe1-xCuxO3-δ) is a new mixed oxide perovskite and has been studied and evaluated the cathode materials for intermediate temperature solid oxide fuel cells (IT-SOFCs), mainly due to its good compatibility with the electrolyte (CGO) and its high ionic conductivity and electronic in intermediate temperature. In this work, PSFC powders with two different compositions (Pr0,5Sr0,5Fe0,8Cu0,2O3- PSFC5582 and Pr0,5Sr0,5Fe0,6Cu0,4O3-PSFC5564) were synthesized by the citrate method using a new route. The powders obtained were characterized by thermal analysis (Differential Scanning Calorimetry and Thermogravimetry), and the material calcined at 800, 900 and 1000 °C for 5h were analyzed by X-ray diffractometry (XRD), with the Rietveld refinement of the diffraction data and dilatometry. PSFC5582 composite films were obtained by screen printing of powder calcined at 1000 °C. The films were deposited on substrate ceria doped with gadolinia (CGO) and then sintered at 1050 °C for 2h. The electrochemical performance of the electrodes was evaluated by impedance spectroscopy and the interface electrode/electrolyte was observed by scanning electron microscopy (SEM). The specific resistance area (ASR) was 0.44 Ω.cm² at 800 °C, slightly lower than those reported in the literature for cathodes containing cobalt. The thermal expansion coefficients of both the PSFC compositions were obtained and varied between 13 and 15 x 10-6 °C-1 , in a temperature range of 200 to 650 °C, demonstrating the good thermal compatibility of cathodes with Ce0,9Gd0,1O1,95 electrolytes (CET = 12 x 10-6 °C).

Caracterização e separação física de placas de circuito impresso de computadores obsoletos

The unbridled consumption of electronic equipment associated with fast immersion of new technologies on the market leads to the accelerated growth of electronic waste. Such waste mostly contains printed circuit boards in its structure. Printed circuit boards have many metals, including heavy metals, being highly toxic. Electronic waste is discarded improperly and indiscriminately, usually without any previous treatment and with other municipal waste, contaminating the environment and causing serious problems to human health. Beyond these metals, there are also precious metals and high value-added basis, that can be recovered and recycled, reducing the exploration of natural resources. Thus, due to the high growth potential and reuse of these waste treatment processes, characterization and separation were applied to the printed circuit boards. The printed circuit boards were subjected to physical treatments such as dismantling, crushing, sizing separation, magnetic separation and chemical treatments such as pyrolysis and leaching. Through characterization process (pyrolysis and leaching) the proportions of the components of the granulometric range were determined: 46,08% of metals; 23,32% of polymers and 30,60% of ceramics. It was also observed by particle size separation that metal components tend to concentrate in coarse fractions, while polymeric and ceramic components in fine fractions. From the magnetic separation process was obtained 12,08% of magnetic material and 82,33% of non-magnetic material.

Estudo do aproveitamento de resíduos PAE no desenvolvimento de materiais cerâmicos

This work presents a new ceramic material obtained through the incorporation of solid waste from the steel industry and known as dedusting powder PAE - in ceramic formulations based on clay, potassium and sodium feldspars, kaolin and talc. Formulations were prepared with ceramic residue levels of 0% (basic mass - MB), 2%, 4% and 8%, subjected to firing at temperatures of 1000 ° C, 1050ºC, 1100ºC and 1150ºC for periods of 15 min. and 120 min. The physicchemical and mechanical properties of these ceramic formulations were determined based on the firing temperature, residence time in the oven and the percentage of waste. Since the physicochemical and mechanical properties of the sintered materials were evaluated by chemical analysis techniques (fluorescence X-rays - FRX), particle size distribution, specific surface area, apparent density, structural analysis by diffraction of X-rays (DRX) and characterization of surface by scanning electron microscopy (SEM). The magnetic response characteristics and the pattern of magnetic ferrites of the samples were analyzed in the assay conditions, having noticed that the saturation magnetic susceptibility depend on the sintering temperature of the material and it is associated with its crystal structure. From the analysis results, it was concluded that the ceramic material with better physical and mechanical properties is obtained when the 8% from PAE residue is added to standard formulation under the burn time of 15 minutes and temperature of 1150ºC.