Anisotropia magnética (110) em Nanofilmes de Permalloy sobre MgO(100)

The study and fabrication of nanostructured systems composed of magnetic materials has been an area of great scientific and technological interest. Soft magnetic materials, in particular, have had great importance in the development of magnetic devices. Among such materials we highlight the use of alloys of Ni and Fe, known as Permalloy. We present measurement results of structural characterization and magnetic films in Permalloy (Ni81Fe19), known to be a material with high magnetic permeability, low coercivity and small magneto- crystalline anisotropy, deposited on MgO (100) substrates. The Magnetron Sputtering technique was used to obtain the samples with thicknesses varying between 9 150 nm. The techniques of X- ray Diffraction at high and low angle were employed to confirm the crystallographic orientation and thickness of the films. In order to investigate the magnetic properties of the films the techniques of Vibrant Sample Magnetometry (VSM), Ferromagnetic Resonance (FMR) and Magnetoimpedance were used. The magnetization curves revealed the presence of anisotropy for the films of Py/MgO (100), where it was found that there are three distinct axis - an easy-axis for θH = 0°, a hard-axis for θH = 45° and an intermediate for θH = 90°. The results of the FMR and Magnetoimpedance techniques confirm that there are three distinct axes, that is, there is a type C2 symmetry. Then we propose, for these results, the interpretation of the magnetic anisotropy of Py/MgO ( 100 ) is of type simple C2, ie a cubic magnetic anisotropy type ( 110 )

Caracterização magnética e estrutural de filmes depositados por gaiola catódica

Iron nitrite films, with hundred of nanometers thick, were deposited using the Cathodic cage plasma nitriding method, with a N2/H2 plasma, over a common glass substract. The structure, surface morphology and magnetic properties were investigated using X-ray diffractometry (XRD), atomic force microscopy (AFM) and vibrating sample magnetometer (VSM). XRD shows the formation of γ FeN phase and a combination of ζFe2N + ɛFe3N phases. The film s saturation magnetization and coercivity depends on morphology, composition, grain size and treatment temperature. Temperature raising from 250 ºC to 350 ºC were followed by an increase in saturation magnetization and film s surface coercivity on the parallel direction in relative proportion. This fact can be attributed to the grain sizes and to the different phases formed, since iron rich fases, like the ɛFe3N phase, emerges more frequently on more elevated treatment s temperature. Using this new and reasonably low cost method, it was possible to deposit films with both good adhesion and good magnetic properties, with wide application in magnetic devices

Crescimento de filmes nanométricos monocristalinos de Fe/MgO(100) por "SPUTTERING" DC

The research behind this master dissertation started with the installation of a DC sputtering system, from its first stage, the adaptation of a refrigerating system, passing by the introduction of a heating system for the chamber using a thermal belt, until the deposition of a series of Fe/MgO(100) single crystal nanometric film samples. The deposition rates of some materials such as Fe, Py and Cu were investigated through an Atomic Force Microscope (AFM). For the single crystal samples, five of them have the same growth parameters and a thickness of 250Å, except for the temperature, which varies from fifty degrees from one to another, from 100ºC to 300ºC. Three other samples also have the same deposition parameters and a temperature of 300ºC, but with thickness of 62,5Å, 150Å, and 250Å. Magneto-optical Kerr Effect (MOKE) of the magnetic curves measurements and Ferromagnetic Resonance (FMR) were made to in order to study the influence of the temperature and thickness on the sample s magnetic properties. In the present dissertation we discuss such techniques, and the experimental results are interpreted using phenomenological models, by simulation, and discussed from a physical point of view, taking into account the system s free magnetic energy terms. The results show the growth of the cubic anisotropy field (Hac) as the sample s deposition temperature increases, presenting an asymptotic behavior, similar to the characteristic charging curve of a capacitor in a RC circuit. A similar behavior was also observed for the Hac due to the increase in the samples thicknesses. The 250˚A sample, growth at 300°C, presented a Hac field close to the Fe bulk value

Polaritons em materiais magnéticos nanoestruturados

In this work we present a theoretical study about the properties of magnetic polaritons in superlattices arranged in a periodic and quasiperiodic fashíons. In the periodic superlattice, in order to describe the behavior of the bulk and surface modes an effective medium approach, was used that simplify enormously the algebra involved. The quasi-periodic superlattice was described by a suitable theoretical model based on a transfer-matrix treatment, to derive the polariton's dispersion relation, using Maxwell's equations (including effect of retardation). Here, we find a fractal spectra characterized by a power law for the distribution of the energy bandwidths. The localization and scaling behavior of the quasiperiodic structure were studied for a geometry where the wave vector and the external applied magnetic field are in the same plane (Voigt geometry). Numerical results are presented for the ferromagnet Fe and for the metamagnets FeBr2 and FeCl2

Síntese e caracterização de componentes nanoestruturados de células a combustível de óxidos sólidos

Perovskite-like ceramic materials present the general formula ABO3, where A is a rare earth element or an alkaline metal element, and B is a transition metal. These materials are strong candidates to assume the position of cathode in Solid Oxide Fuel Cells (SOFC), because they present thermal stability at elevated temperatures and interesting chemical and physical properties, such as superconductivity, dieletricity, magnetic resistivity, piezoelectricity, catalytic activity and electrocatalytic and optical properties. In this work the cathodes of Solid Oxide Fuel Cells with the perovskite structure of La1-xSrxMnO3 (x = 0.15, 0.22, 0.30) and the electrolyte composed of zirconia-stabilized-yttria were synthesized by the Pechini method. The obtained resins were thermal treatment at 300 ºC for 2h and the obtained precursors were characterized by thermal analysis by DTA and TG / DTG. The powder precursors were calcined at temperatures from 450 to 1350ºC and were analyzed using XRD, FTIR, laser granulometry, XRF, surface area measurement by BET and SEM methods. The pellets were sintered from the powder to the study of bulk density and thermal expansion

Estudo do comportamento térmico e da luminescência de filmes de quitosana com os íons Eu3+ e Tb3+

Films of chitosan with trivalent lanthanides ions Eu3+ and Tb3+ were respectively prepared in the ratio of 3:1 m/m (chitosan: lanthanide) and 6:1 m/m (chitosan: lanthanide). There were no formations of films in a ratio of 1:1 m/m (chitosan: lanthanides). The films of chitosan with the Tb3+ ion have the same transparent appearance than the pure chitosan films. The film of chitosan with Eu3+ ion has a muddy appearance. These films present good resistance to tear. The appearance of the compounds prepared in ratio 1:1m/m is a white powder. The films and compounds of chitosan were characterized by Elementary Analysis (CHN), Thermal Analysis (TG/DTG) and Spectroscopy of Luminescence. The CHN analysis was made only for compounds prepared in ratio 1:1m/m, suggesting that these compounds possess the formula QUILn.6H2O, where QUI = Chitosan and Ln = Lanthanide. The results of the curves TG/DTG indicated that there are strong interactions between Eu3+ or Tb3+ and chitosan, causing a lesser lost of mass in the films. The luminescence analysis showed that the films of chitosan with the ions Eu3+ and Tb3+ present emissions in the region of the visible one, with bands of the chitosan and of the Eu3+ ion. The luminescence analysis of the compounds of chitosan with the Eu3+ and Tb3+ ions suggest that the chitosan does not transfer into energy to the ions lanthanides, however the chemical neighborhood around of the ion lanthanides breaks the selection rules and, conseqüently the 4f-4f transitions of the lanthanide ions are observed

Desenvolvimento de componentes nanométricos para aplicação em células a combustível à base de sólidos estruturados e filmes finos

The present work aims the preparation of filmes of strontium-doped lanthanum manganite (perovskita) yttria-stabilized zirconia (LSM-SDC) films deposited on substrate of YSZ by means of spin coating technique having as principal objective their application to solid oxide fuel cells of intermediate temperature. La0,8Sr0,2MnO3 and Ce0,8Sm0,2O1,9 were obtained by modified Pechini method by use of gelatin which act as polymerization agent. The powders obtained were characterized by Xray fluorescence, X ray diffraction, electronic scanning microscopy and the superficial area by BET method. The results obtained by X-ray fluorescence showed that the route adopted for obtention of powders was effective in the obtention of the compositions with close values to the stoichiometrics. Ethyl cellulose was used as pore-forming agent and mixed with the LSM-SDC powders in weight proportions of 1:24, 2:23 and 1:9. The films were sintered at 1150 °C for 4 h and characterized by X-ray diffraction and scanning electron microscopy technique (SEM) and atomic force. The phases quantification of the precursory powders and of the obtained films was carried through Rietveld method. According with the analysis of SEM, as the content of ethyl cellulose was increased, the pore distribution in films become more uniform and the pore size reduced. The methodology used for the obtention of the films was very efficient, considering a material was obtained with characteristics that were proper to the application as electrolyte/cathode system to solid oxide fuel cells

Deposição de filmes de ZrO2 modificados sobre substratos metálicos

This work makes use of the Pechini process for synthesis of the solutions and the dip-coating process for the addition of zirconium oxide films pure and doped cerium metal substrates. The metals with ceramic substrates were subjected to severe conditions of salinity. The x-ray fluorescence of the substrate showed a great diversity of chemical elements. The x-ray diffraction of the samples showed the phase of iron substrate because the thickness of nano-thin film. Tests using an LPR probe showed that the film presents with zirconia corrosion independent of film thickness. The substrates of ZrO2-doped ceria showed low chemical attack of the salt in films with less than 15 dives. The results imply that ultrathin films are shown in protecting metallic substrates

Construção de um sistema de caracterização das propriedades de transporte de filmes finos pelo efeito Hall

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

Avaliação da remoção de hidrocarbonetos aromáticos (BTEX) em águas utilizando materiais nanoestruturados do tipo Ti-MCM-41

Volatile Organic Compounds are pollutants coming mainly from activities that use fossil fuels. Within this class are the BTEX (benzene, toluene, ethylbenzene and xylenes) compounds that are considered hazardous. Among the various existing techniques for degradation of pollutants, there is advanced oxidation using H2O2 generating hidoxil radical ( OH). In this work, the mesoporous material of MCM-41 was synthesized by hydrothermal method and then was used as support, the impregnation of titanium by the method of synthesis with excess solvent to obtain the catalyst Ti-MCM-41. The catalyst was used in the reaction catalyzed removal of BTEX in water using H2O2 as oxidant. The materials were characterized by: XRD, TG/DTG, FTIR, nitrogen adsorption-desorption and FRX-EDX, in order to verify the method of impregnation of the mesoporous titanium support was effective. Catalytic tests were carried out in reactors of 20 mL containing BTEX (100.0 μg/L), H2O2 (2.0 M) and Ti-MCM-41 (2.0 g/L) in acid medium. The reaction occurred for 5 h at 60 °C and analysis were performed by gas chromatography with photoionization detector and static headspace sampler. The characterizations have proven the effectiveness of the synthesis method used and the incorporation of titanium lt in the support. The catalytic tests showed satisfactory results with conversion of more than 95 % for the studied compounds, where the catalyst 48% Ti-MCM-41 showed a higher removal efficiency of the compounds under study

Estudo de titanatos nanoestruturados obtidos por tratamento hidrotérmico de óxido de titânio em meio alcalino

TiTanate NanoTubes (TTNT) were synthesized by hydrothermal alkali treatment of TiO2 anatase followed by repeated washings with distinct degrees of proton exchange. TTNT samples with different sodium contents were characterized, as synthesized and after heattreatment (200-800ºC), by X-ray diffraction, scanning and transmission electron microscopy, electron diffraction, thermal analysis, nitrogen adsorption and spectroscopic techniques like FTIR and UV-Vis diffuse reflectance. It was demonstrated that TTNTs consist of trititanate structure with general formula NaxH2−xTi3O7·nH2O, retaining interlayer water in its multiwalled structure. The removal of sodium reduces the amount of water and contracts the interlayer space leading, combined with other factors, to increased specific surface area and mesopore volume. TTNTs are mesoporous materials with two main contributions: pores smaller than 10 nm due to the inner volume of nanotubes and larger pores within 5-60 nm attributed to the interparticles space. Chemical composition and crystal structure of TTNTs do not depend on the average crystal size of the precursor TiO2-anatase, but this parameter affects significantly the morphology and textural properties of the nanostructured product. Such dependence has been rationalized using a dissolution-recrystallization mechanism, which takes into account the dissolution rate of the starting anatase and its influence on the relative rates of growth and curving of intermediate nanosheets. The thermal stability of TTNT is defined by the sodium content and in a lower extent by the crystallinity of the starting anatase. It has been demonstrated that after losing interlayer water within the range 100-200ºC, TTNT transforms, at least partially, into an intermediate hexatitanate NaxH2−xTi6O13 still retaining the nanotubular morphology. Further thermal transformation of the nanostructured tri- and hexatitanates occurs at higher or lower temperature and follows different routes depending on the sodium content in the structure. At high sodium load (water washed samples) they sinter and grow towards bigger crystals of Na2Ti3O7 and Na2Ti6O13 in the form of rods and ribbons. In contrast, protonated TTNTs evolve to nanotubes of TiO2(B), which easily convert to anatase nanorods above 400ºC. Besides hydroxyls and Lewis acidity typical of titanium oxides, TTNTs show a small contribution of protonic acidity capable of coordinating with pyridine at 150ºC, which is lost after calcination and conversion into anatase. The isoeletric point of TTNTs was measured within the range 2.5-4.0, indicating behavior of a weak acid. Despite displaying semiconductor characteristics exhibiting typical absorption in the UV-Vis spectrum with estimated bandgap energy slightly higher than that of its TiO2 precursor, TTNTs showed very low performance in the photocatalytic degradation of cationic and anionic dyes. It was concluded that the basic reason resides in its layered titanate structure, which in comparison with the TiO2 form would be more prone to the so undesired electron-hole pair recombination, thus inhibiting the photooxidation reactions. After calcination of the protonated TTNT into anatase nanorods, the photocatalytic activity improved but not to the same level as that exhibited by its precursor anatase

Obtenção de diesel verde por craqueamento termocatalítico de óleo de buriti (Mauritia flexuosa L.) sobre materiais nanoestruturados do tipo LaSBA-15

In order to obtain a biofuel similar to mineral diesel, lanthanum-incorporated SBA- 15 nanostructured materials, LaSBA-15(pH), with different Si/La molar ratios (75, 50, 25), were synthesized in a two-steps hydrothermal procedure, with pH-adjusting of the synthesis gel at 6, and were used like catalytic solids in the buriti oil thermal catalytic cracking. These solids were characterized by X-ray fluorescence (XRF), powder X-ray diffraction (XRD), thermogravimetric analysis (TG/DTG), infrared spectroscopy (FTIR), nitrogen porosimetry and ethanol dehydration, aiming to active sites identify. Taken together, the analyses indicated that the synthesis method has employed to obtain materials highly ordered mesostructures with large average pore sizes and high surface area, besides suggested that the lanthanum was incorporated in the SBA-15 both into the framework as well as within the mesopores. Catalytic dehydration of ethanol over the LaSBA-15(pH) products has shown that they have weak Lewis acid and basic functionalities, indicative of the presence of lanthanum oxide in these samples, especially on the La75SBA-15(pH) sample, which has presented the highest selectivity to ethylene. The buriti oil thermal and thermal catalytic cracking, realized from the room temperature to 450 ºC in a simple distillation system, has allowed obtaining two liquid fractions, each consisting of two phases, one aqueous and another organic, organic liquid (OL). The OL obtained from first fractions has shown high acid index, even in the thermal catalytic process. One the other hand, OL coming from second ones, called green diesel (GD), have presented low acid index, particularly that one obtained from the thermal catalytic process realized over LaSBA-15(pH) samples. The acid sites presence in these samples, associated to their large average pore sizes and high surface areas, have allowed them, especially the La75SBA-15(pH), to present deoxygenating activity in the buriti oil thermal catalytic cracking, providing an oxygenates content reduction, particularly carboxylic acids, in the GD. Furthermore, the GD comes from the second liquid fraction obtained in the buriti oil thermal catalytic cracking over this latest solid sample has shown hydrocarbons composition and physic-chemical properties similar to that mineral diesel, beyond sulfur content low

Confecção e caracterização físico-química de filmes compósitos autossustentáveis NaAlg-TiO2-WO3

A new self-sustainable film was prepared through the sol-gel modified method, previously employed in our research group; sodium alginate was used as the polymer matrix, along with plasticizer glycerol, doped with titanium dioxide (TiO2) and tungsten trioxide (WO3). By varying WO3 concentration (0,8, 1,6, 2,4 and 3,2 μmol) and keeping TiO2 concentration constant (059 mmol), it was possible to study the contribution of these oxides on the obtained films morphological and electrical properties. Self-sustainable films have analyzed by Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XDR), Scanning Electron Microscope (SEM), Energy Dispersive X-ray Spectroscopy (EDS) and Electrochemical Impedance Spectroscopy (EIS). By the IR specters, it was possible identify the TiO2, and posteriorly WO3, addition has provided dislocation of alginate characteristics bands to smaller vibrations frequencies indicating an electrostatic interaction between the oxides and the polymer matrix. Diffractograms show predominance of the amorphous phase in the films. SEM, along with EDX, analysis revealed self-sustainable films showed surface with no cracks and relative dispersion of the oxides throughout the polymer matrix. From Impedance analysis, it was observe increasing WO3 concentration to 2,4 μmol provided a reduction of films resistive properties and consequent improvement of conductive properties

Degradação térmica e catalítica do resíduo atmosférico de petróleo (RAT), utilizando materiais nanoestruturados do tipo SBA-15

In this work were synthesized and characterized the materials mesoporous SBA-15 and Al- SBA-15, Si / Al = 25, 50 and 75, discovered by researchers at the University of California- Santa Barbara, USA, with pore diameters ranging from 2 to 30 nm and wall thickness from 3.1 to 6.4 nm, making these promising materials in the field of catalysis, particularly for petroleum refining (catalytic cracking), as their mesopores facilitate access of the molecules constituting the oil to active sites, thereby increasing the production of hydrocarbons in the range of light and medium. To verify that the materials used as catalysts were successfully synthesized, they were characterized using techniques of X-ray diffraction (XRD), absorption spectroscopy in the infrared Fourier transform (FT-IR) and adsorption nitrogen (BET). Aiming to check the catalytic activity thereof, a sample of atmospheric residue oil (ATR) from the pole Guamaré-RN was performed the process by means of thermogravimetry and thermal degradation of catalytic residue. Upon the curves, it was observed a reduction in the onset temperature of the decomposition process of catalytic ATR. For the kinetic model proposed by Flynn-Wall yielded some parameters to determine the apparent activation energy of decomposition, being shown the efficiency of mesoporous materials, since there was a decrease in the activation energy for the reactions using catalysts. The ATR was also subjected to pyrolysis process using a pyrolyzer with gas chromatography coupled to a mass spectrometer. Through the chromatograms obtained, there was an increase in the yield of the compounds in the range of gasoline and diesel from the catalytic pyrolysis, with emphasis on Al-SBA-15 (Si / Al = 25), which showed a percentage higher than the other catalysts. These results are due to the fact that the synthesized materials exhibit specific properties for application in the process of pyrolysis of complex molecules and high molecular weight as constituents of the ATR

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