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 )

Propriedades fisicas do monocristal fe/mgo(100) e estudo da expansao termica da superficie da ag(100)

In this work we have developed a way to grow Fe/MgO(100) monocrystals by magnetron sputtering DC. We investigated the growing in a temperature range among 100 oC and 300 oC. Structural and magneto-crystalline properties were studied by different experimental techniques. Thickness and surface roughness of the films were investigated by atomic force microscopy, while magneto-crystalline properties were investigated by magneto-optical Kerr effect and ferromagnetic resonance. Our results show that as we increase the deposition temperature, the magneto-crystalline anisotropy of the films also increases, following the equation of Avrami. The best temperature value to make a film is 300 oC. As the main result, we built a base of magnetoresistence devices and as an aplication, we present measurements of Fe/Cr/Fe trilayer coupling. In a second work we investigated the temperature dependence of the first three interlayer spacings of Ag(100) surface using low energy electron diffraction. A linear expansion model of crystal surface was used and the values of Debye temperatures of the first two layers and thermal expansion coefficient were determinated. A relaxation of 1% was found for Ag(100) surface and these results are matched with faces (110) and (111) of the silver. iv

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

Síntese e caracterização de espinélios a base de Cu, Fe e Cr para pigmentos cerâmicos

Inorganic pigment comprises a host lattice, which is part of the chromophore component (usually a transition metal cation) and possible components modifiers, which stabilize, add or restate the properties pigments. Among the materials with spinel, ferrites, and the chromite stand out, because they have broad technological importance in the area of materials, applicability, pigments, catalytic hydrogenation, thin film, ceramic tiles, among others. The present work, pigments containing CuFe2O4, CuCr2O4,e CuFeCrO4, were synthesized by a method that makes use of gelatin as organic precursor using their application to ceramic pigments. The pigments were characterized by X-ray diffraction (XRD), Infrared spectroscopy, scanning electron microscopy (SEM) spectroscopy in the UV-visible and Colorimetry. The results confirmed the feasibility of the synthetic route used, with respect to powders synthesized, there is the formation of spinel phase from 500°C, with an increase in crystallinity and the formation of other phases. The pigments were shown to be crystalline and the desired phases were obtained. The copper chromite have hues ranging from green to black according to the calcination temperature, while the copper chromite doped with iron had brownish. The ferrites showed copper color and darker brown to black, which may indicate an interesting factor because of the importance of black pigment

Adição de nanopartículas de Ti em matriz de Fe através da deposição por magnetron sputtering

Microalloyed steels constitute a specific class of steel with low amount of carbon and microalloying elements such as Vanadium (V), Niobium (Nb) and Titanium (Ti). The development and application of microalloyed steels and steels in general are limited to the handling of powders with particles of submicron or nanometer dimensions. Therefore, this work presents an alternative in order to construction of microalloyed steels utilizing the deposition by magnetron sputtering technique as a microalloying element addiction in which Ti nanoparticles are dispersed in an iron matrix. The advantage of that technique in relation to the conventional metallurgical processes is the possibility of uniformly disperse the microalloying elements in the iron matrix. It was carried out deposition of Ti onto Fe powder in high CH4, H2, Ar plasma atmosphere, with two deposition times. After the deposition, the iron powder with nanoparticles of Ti dispersed distributed, were compacted and sintered at 1120 ° C in resistive furnace. Characterization techniques utilized in the samples of powder before and after deposition of Ti were Granulometry, Scanning Electron Microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and X-ray diffraction (DRX). In the case of sintered samples, it was carried out characterization by SEM and Vickers Microhardness assays. The results show which the deposition technique by magnetron sputtering is practicable in the dispersion of particles in iron matrix. The EDX microanalysis detected higher percentages of Ti when the deposition were carried out with the inert gas and when the deposition process was carried out with reactive gas. The presence of titanium in iron matrix was also evidenced by the results of X-ray diffraction peaks that showed shifts in the network matrix. Given these results it can be said that the technique of magnetron sputtering deposition is feasible in the dispersion of nanoparticles of iron matrix in Ti.

Síntese e impregnação de peneiras moleculares Fe MCM-41 derivada de sílica da casca do arroz

The mesoporous molecular sieves of the MCM-41 and FeMCM-41 type are considered promissory as support for metals used as catalysts in oil-based materials refine processes and as adsorbents for environmental protection proposes. In this work MCM-41 and FeMCM41 were synthesized using rice husk ash - RHA as alternative to the conventional silica source. Hydrothermal synthesis was the method chosen to prepare the materials. Pre-defined synthesis parameters were 100°C for 168 hours, later the precursor was calcinated at 550°C for 2 hours under nitrogen and air flow. The sieves containing different proportions of iron were produced by two routes: introduction of iron salt direct synthesis; and a modification post synthesis consisting in iron salt 1 % and 5% impregnation in the material followed by thermal decomposition. The molecular sieves were characterized by X ray diffraction XRD, Fourier transform infrared spectroscopy FT-IR, X ray fluorescence spectroscopy XFR, scanning electronic microscopy SEM, specific surface area using the BET method, Termogravimetry TG. The kinetic model of Flynn Wall was used with the aim of determining the apparent activation energy of the surfactant remove (CTMABr) in the MCM- 41 porous. The analysis made possible the morphology characterization, identifying the presence of hexagonal structure typical for mesoporous materials, as well as observation of the MCM41 and iron of characteristic bands.

Extração de metais (K, Mg, Ba, Ca, Cr, Mn, Li, Fe) de água produzida utilizando sistema microemulsionado

The produced water is a byproduct formed due to production of petroleum and carries with it a high amount of contaminants such as oil particles in suspension, organic compounds and metals. Thus, these latter pollutants are very difficult to treat because of its high solubility in water. The objective of this work is to use and evaluate a microemulsioned system to remove metals ( K , Mg , Ba , Ca , Cr , Mn , Li , Fe ) of synthetic produced water. For the extraction of metals, it was used a pseudoternary diagram containing the following phases: synthetic produced water as the aqueous phase (AP), hexane as organic phase (OP), and a cosurfactant/surfactant ratio equal to four (C/S = 4) as the third phase, where the OCS (saponified coconut oil) was used as surfactant and n-butanol as cosurfactant. The synthetic produced water was prepared in a bench scale and the region of interest in the diagram for the removal of metals was determined by experimental design called. Ten points located in the phase Winsor II were selected in an area with a large amount of water and small amounts of reagents. The samples were analyzed in atomic absorption spectrometer, and the results were evaluated through a statistical assesment, allowing the efficiency analysis of the effects and their interactions. The results showed percentages of extraction above 90% for the metals manganese, iron, chromium, calcium, barium and magnesium, and around 45% for metals lithium and potassium. The optimal point for the simultaneous removal of metals was calculated using statistical artifact multiple response function (MR). This calculation showed that the point of greatest extraction of metals occurs was the J point, with the composition [72% AP, 9% OP, 19% C/S], obtaining a global extraction percentage about 80%. Considering the aspects analyzed, the microemulsioned system has shown itself to be an effective alternative in the extraction of metals on synthetic produced water remediation

Multicamadas Ferromagnéticas Nanométricas Periódicas e Quasiperiódicas

We present a study of nanostructured magnetic multilayer systems in order to syn- thesize and analyze the properties of periodic and quasiperiodic structures. This work evolved from the deployment and improvement of the sputtering technique in our labora- tories, through development of a methodology to synthesize single crystal ultrathin Fe (100) films, to the final goal of growing periodic and quasiperiodic Fe/Cr multilayers and investi- gating bilinear and biquadratic exchange coupling between ferromagnetic layer dependence for each generation. Initially we systematically studied the related effects between deposition parameters and the magnetic properties of ultrathin Fe films, grown by DC magnetron sput- tering on MgO(100) substrates. We modified deposition temperature and film thickness, in order to improve production and reproduction of nanostructured monocrystalline Fe films. For this set of samples we measured MOKE, FMR, AFM and XPS, with the aim of investi- gating their magnocrystalline and structural properties. From the magnetic viewpoint, the MOKE and FMR results showed an increase in magnetocrystalline anisotropy due to in- creased temperature. AFM measurements provided information about thickness and surface roughness, whereas XPS results were used to analyze film purity. The best set of parame- ters was used in the next stage: investigation of the structural effect on magnetic multilayer properties. In this stage multilayers composed of interspersed Fe and Cr films are deposited, following the Fibonacci periodic and quasiperiodic growth sequence on MgO (100) substrates. The behavior of MOKE and FMR curves exhibit bilinear and biquadratic exchange coupling between the ferromagnetic layers. By computationally adjusting magnetization curves, it was possible to determine the nature and intensity of the interaction between adjacent Fe layers. After finding the global minimum of magnetic energy, we used the equilibrium an- gles to obtain magnetization and magnetoresistance curves. The results observed over the course of this study demonstrate the efficiency and versatility of the sputtering technique in the synthesis of ultrathin films and high-quality multilayers. This allows the deposition of magnetic nanostructures with well-defined magnetization and magnetoresistance parameters and possible technological applications

Efeito Kerr magneto-óptico; Ressonância ferromagnética; Acoplamento bilinear; Acoplamento biquadrático

In this work, we investigated the magnetic properties of a monocrystalline Fe thin film and of Fe(80 Å)/Cr(t)/Fe(80 Å) tri-layers, with the nonmagnetic metallic Cr spacer layer thickness varying between 9 Å < t < 40 Å. The samples were deposited by the DC Sputtering on Magnesium Oxide (MgO) substrates, with (100) crystal orientation. For this investigation, experimental magneto-optical Kerr effect (MOKE) magnetometry and ferromagnetic resonance (FMR) techniques were employeed. In this case, these techniques allowed us to study the static and dynamical magnetization properties of our tri-layers. The experimental results were interpreted based on the phenomenological model that takes into account the relevant energy terms to the magnetic free energy to describe the system behavior. In the case of the monocrystalline Fe film, we performed an analytical discussion on the magnetization curves and developed a numerical simulation based on the Stoner-Wohlfarth model, that enables the numerical adjustment of the experimental magnetization curves and obtainment of the anisotropy field values. On the other hand, for the tri-layers, we analyzed the existence of bilinear and biquadratic couplings between the magnetizations of adjacent ferromagnetic layers from measurements of magnetization curves. With the FMR fields and line width angular dependencies, information on the anisotropy in three layers was obtained and the effects of different magnetic relaxation mechanisms were evidenced. It was also possible to observe the dependence of the epitaxy of the multilayers with growth and sputtering parameters. Additionally it was developed the technique of AC magnetic susceptibility in order to obtain further information during the investigation of magnetic thin films

Ondas de spin em nanofilmes nagnéticos acoplados quasiperiodicamente

We studied the spin waves modes that can propagate in magnetic multilayers composed of ferromagnetic metallic films in the nanometer scale. The ferromagnetic films (iron) are separated and coupled through the nonmagnetic spacer films (chromium). The films that make up the multilayer are stacked in a quasiperiodic pattern, following the Fibonacci and double period sequences. We used a phenomenological theory taking into account: the Zeeman energy (between the ferromagnetic films and the external magnetic field), the energy of the magneto-crystalline anisotropy (present in the ferromagnetic films), the energy of the bilinear and biquadratic couplings (between the ferromagnetic films) and the energy of the dipole-dipole interaction (between the ferromagnetic films), to describe the system. The total magnetic energy of the system is numerically minimized and the equilibrium angles of the magnetization of each ferromagnetic film are determined. We solved the equation of motion of the multilayer to find the dispersion relation for the system and, as a consequence, the spin waves modes frequencies. Our theoretical results show that, in the case of trilayers (Fe/Cr/Fe), our model reproduces with excellent agreement experimental results of Brillouin light scattering, known from the literature, by adjusting the physical parameters of the nanofilms. Furthermore, we generalize the model to N ferromagnetic layers which allowed us to determine how complex these systems become when we increase the number of components. It is worth noting that our theoretical calculations generalize all the results known from the literature

Efeitos da interação dipolar na nucleação de vórtices em nano-cilindros magnéticos

The effect of confinement on the magnetic structure of vortices of dipolar coupled ferromagnetic nanoelements is an issue of current interest, not only for academic reasons, but also for the potential impact in a number of promising applications. Most applications, such as nano-oscillators for wireless data transmission, benefit from the possibility of tailoring the vortex core magnetic pattern. We report a theoretical study of vortex nucleation in pairs of coaxial iron and Permalloy cylinders, with diameters ranging from 21nm to 150nm, and 12nm and 21nm thicknesses, separated by a non-magnetic layer. 12nm thick iron and Permalloy isolated (single) cylinders do not hold a vortex, and 21nm isolated cylinders hold a vortex. Our results indicate that one may tailor the magnetic structure of the vortices, and the relative chirality, by selecting the thickness of the non-magnetic spacer and the values of the cylinders diameters and thicknesses. Also, the dipolar interaction may induce vortex formation in pairs of 12nm thick nanocylinders and inhibit the formation of vortices in pairs of 21nm thick nanocylinders. These new phases are formed according to the value of the distance between the cylinderes. Furthermore, we show that the preparation route may control relative chirality and polarity of the vortex pair. For instance: by saturating a pair of Fe 81nm diameter, 21nm thickness cylinders, along the crystalline anisotropy direction, a pair of 36nm core diameter vortices, with same chirality and polarity is prepared. By saturating along the perpendicular direction, one prepares a 30nm diameter core vortex pair, with opposite chirality and opposite polarity. We also present a theoretical discussion of the impact of vortices on the thermal hysteresis of a pair of interface biased elliptical iron nanoelements, separated by an ultrathin nonmagnetic insulating layer. We have found that iron nanoelements exchange coupled to a noncompensated NiO substrate, display thermal hysteresis at room temperature, well below the iron Curie temperature. The thermal hysteresis consists in different sequences of magnetic states in the heating and cooling branches of a thermal loop, and originates in the thermal reduction of the interface field, and on the rearrangements of the magnetic structure at high temperatures, 5 produce by the strong dipolar coupling. The width of the thermal hysteresis varies from 500 K to 100 K for lateral dimensions of 125 nm x 65 nm and 145 nm x 65 nm. We focus on the thermal effects on two particular states: the antiparallel state, which has, at low temperatures, the interface biased nanoelement with the magnetization aligned with the interface field and the second nanoelement aligned opposite to the interface field; and in the parallel state, which has both nanoelements with the magnetization aligned with the interface field at low temperatures. We show that the dipolar interaction leads to enhanced thermal stability of the antiparallel state, and reduces the thermal stability of the parallel state. These states are the key phases in the application of pairs of ferromagnetic nanoelements, separated by a thin insulating layer, for tunneling magnetic memory cells. We have found that for a pair of 125nm x 65nm nanoelements, separated by 1.1nm, and low temperature interface field strength of 5.88kOe, the low temperature state (T = 100K) consists of a pair of nearly parallel buckle-states. This low temperature phase is kept with minor changes up to T= 249 K when the magnetization is reduced to 50% of the low temperature value due to nucleation of a vortex centered around the middle of the free surface nanoelement. By further increasing the temperature, there is another small change in the magnetization due to vortex motion. Apart from minor changes in the vortex position, the high temperature vortex state remains stable, in the cooling branch, down to low temperatures. We note that wide loop thermal hysteresis may pose limits on the design of tunneling magnetic memory cells

Efeito nernst anômalo em Materiais com anisotropia magnetocristalina (110)

Conselho Nacional de Desenvolvimento Científico e Tecnológico

Propriedades físicas de bicamadas magnéticas

The magnetic order of bylayers composed by a ferromagnetic film (F) coupled with an antiferromagnetic film (AF) is studied. Piles of coupled monolayers describe the films and the interfilm coupling is described by an exchange interaction between the magnetic moments at the interface. The F has a cubic anisotropy while the AF has a uniaxial anisotropy. We analyze the effects of an external do magnetic field applied parallel to the interface. We consider the intralayer coupling is strong enough to keep parallel all moments of the monolayer an then they are described by one vector proportional to the magnetization of the layer. The interlayer coupling is represented by an exchange interaction between these vectors. The magnetic energy of the system is the sum of the exchange. Anisotropy and Zeeman energies and the equilibrium configuration is one that gives the absolute minimum of the total energy. The magnetization of the system is calculated and the influence of the external do field combined with the interfilm coupling and the unidirectional anisotropy is studied. Special attention is given to the region near of the transition fields. The torque equation is used to study dynamical behavior of these systems. We consider small oscillations around the equilibrium position and we negleet nonlinear terms to obtain the natural frequencies of the system. The dependence of the frequencies with the external do field and their behavior in the phase transition region is analized

Síntese, sinterização e caracterização de ferritas à base de Ni-Zn

Were synthesized different ferrites NixZn1-xFe2O4 (0,4 ≤ x ≤ 0,6) compositions by using citrate precursor method. Initially, the precursors citrates of iron, nickel and zinc were mixed and homogenized. The stoichiometric compositions were calcined at 350°C without atmosphere control and the calcined powders were pressed in pellets and toroids. The pressed material was sintered from 1100º up to 1200ºC in argon atmosphere. The calcined powders were characterized by XRD, TGA/DTG, FTIR, SEM and vibrating sample magnetometer (VSM). All sintered samples were characterized using XRD, SEM, VSM and measurements of magnetic permeability and loss factor were obtained. It was formed pure ferromagnetic phase at all used temperatures. The Rietveld analyses allowed to calculate the cations level occupation and the crystallite size. The analyses obtained nanometric crystals (12-20 nm) to the calcined powder. By SEM, the sintered samples shows grains sizes from 1 to 10 μm. Sintered densities (ρ) were measured by the Archimedes method and with increasing Zn content, the bulk density decrease. The better magnetization results (105-110 emu/g) were obtained for x=0,6 at all sintering temperatures. The hysteresis shows characteristics of soft magnetic material. Two magnetization processes were considered, superparamagnetism at low temperature and the magnetic domains formation at high temperatures. The sintered toroids presents relative magnetic permeability (μr) from 7 to 32 and loss factor (tanδ) of about 1. The frequency response of toroids range from 0,3 kHz to 0,2 GHz. The composition x=0,5 presents both greater μr and tanδ values and x=0,6 the most broad range of frequency response. Various microstructural factors show influence on the behavior of μr and tanδ, such as: grain size, porosity across grain boundary and inside the grain, grain boundary content and domain walls movement during the process of magnetization at high frequency studies (0,3kKz 0,2 GHz)

Síntese, caracterização, propriedades e aplicação dos sistemas Mg- Al, Zn-Al e Mg-Fe

The Layered Double Hydroxides has become extremely promising materials due to its range of applications, easily obtained in the laboratory and reusability after calcination, so the knowledge regarding their properties is of utmost importance. In this study were synthesized layered double hydroxides of two systems, Mg-Al and Zn-Al, and such materials were analyzed with X-ray diffraction and, from these data, we determined the volume density, planar atomic density, size crystallite, lattice parameters, interplanar spacing and interlayer space available. Such materials were also subjected to thermogravimetric analysis reasons for heating 5, 10, 20 and 25 ° C / min to determine kinetic parameters for the formation of metaphases HTD and HTB based on theoretical models Ozawa, Flynn-Wall Starink and Model Free Kinetics. In addition, the layered double hydroxides synthesized in this working ratios were calcined heating 2.5 ° C / min and 20 ° C / min, and tested for adsorption of nitrate anion in aqueous solution batch system at time intervals 5 min, 15 min, 30 min, 1h, 2h and 4h. Such calcined materials were also subjected to exposure to the atmosphere and at intervals of 1 week, 2 weeks and 1 month were analyzed by infrared spectroscopy to study the kinetics of regeneration determining structural called "memory effect"