Estudo da viabilidade técnica para obtenção de superfície duplex em aço inoxidável martensítico AISI 410 através do processo de deposição a plasma por gaiola catódica

The technique of plasma nitriding by the cathode cage mainly stands out for its ability to produce uniform layers, even on parts with complex geometries. In this study, it was investigated the efficiency of this technique for obtaining duplex surface, when used, simultaneously, to nitriding treatment and thin film deposition at temperatures below 500°C. For this, were used samples of AISI 41 0 Martensitic Stainless Steel and performed plasma treatment, combining nitriding and deposition of thin films of Ti and/or TiN in a plasma atmosphere containing N2-H2. It was used a cathodic cage of titanium pure grade II, cylindrical with 70 mm diameter and 34 mm height. Samples were treated at temperature 420ºC for 2 and 12 hours in different working pressures. Optical Microscopy (OM), Scanning Electron Microscopy (SEM) with micro-analysis by Energy Dispersive Spectroscopy (EDS), X-Ray Diffraction (XRD), Atomic Force Microscopy (AFM) and analysis of Vickers Microhardness were used to investigate coating properties such as homogeneity and surface topography, chemical composition, layer thickness, crystalline phase, roughness and surface microhardness. The results showed there is a direct proportionality between the presence of H2 in plasma atmosphere and the quantity of titanium in surface chemical composition. It was also observed that the plasma treatment at lowpressure is more effective in formation of TiN thin film

Construção de um aparato experimental para monitoramento in situ da deposição de filmes finos de titânio por magnetron sputtering

The technique of surface coating using magnetron sputtering is one of the most widely used in the surface engineering, for its versatility in obtaining different films as well as in the micro / nanometric thickness control. Among the various process parameters, those related to the active species of the plasma are of the most fundamental importance in the mechanism and kinetics of deposition. In order to identify the active species of the plasma, parameters such as gas flow, pressure and density of electric power were varied during titanium coating on glass substrate. By flowing argon gas of 10, 20, 30, 40 and 50 sccm (cubic centimeters per minute) for each gas flow a sequential scan of the electric current of 0.10, 0.20, 0.30, 0.40 , 0.50 A. The maximum value of 0.50 A was chosen based both on literature data and on limitations of the equipment. The monitoring of plasma species present during the deposition was carried out in situ by the technique of optical emission spectroscopy (OES) through the spectrometer Ocean Optics USB2000 Series. For this purpose, an apparatus was developed to adapt the OES inside the plasma reactor to stay positioned closest to the target. The radiations emitted by the species were detected by an optical fiber placed behind the glass substrate and their intensities as a function of wavelength were, displayed on a monitor screen. The acquisition time for each condition of the plain parameters was related to the minima of spectral lines intensities due to the film formed on the substrate. The intensities of different emission lines of argon and titanium were then analyzed as a function of time, to determine the active species and estimate the thickness of the deposited films. After the deposition, the coated glasses thin films were characterized by optical transmittance through an infrared laser. It was found that the thickness and deposition rate determined by in situ analysis were consistent with the results obtained by laser transmittance

Diagnóstico de plasma de cátodo oco: análise da ação de plasma de argônio e Ar-H2 para a deposição de filmes finos de titânio em pós-descarga

Plasma DC hollow cathode has been used for film deposition by sputtering with release of neutral atoms from the cathode. The DC Plasma Ar-H2 hollow cathode currently used in the industry has proven to be effective in cleaning surfaces and thin film deposition when compared to argon plasma. When we wish to avoid the effects of ion bombardment on the substrate discharge, it uses the post-discharge region. Were generated by discharge plasma of argon and hydrogen hollow cathode deposition of thin films of titanium on glass substrate. The optical emission spectroscopy was used for the post-discharge diagnosis. The films formed were analyzed by mechanical profilometry technique. It was observed that in the spectrum of the excitation lines of argon occurred species. There are variations in the rate of deposition of titanium on the glass substrate for different process parameters such as deposition time, distance and discharge working gases. It was noted an increase in intensity of the lines of argon compared with the lines of titanium. Deposition with argon and hydrogen in glass sample observed a higher rate deposition of titanium as more closer the sample was in the discharge

Viabilidade técnica de uma rota não convencional para a produção de leite de cabra em pó em cooperativas do Rio Grande do Norte

Nowadays, Brazil has both the greatest goat herd and the greatest goat milk production of South America. The state of Rio Grande do Norte, located in northeast of Brazil, has an average year production of three thousand cubic meters of goat milk in natura. Part of this milk production is homemade and it comes from small farms, which unite in rural cooperatives created to encourage the production and implementation of industrial processes for preservation and processing of milk. Results presented by literature and obtained from preliminary essays in this thesis show that non conventional dryer of spouted bed with inert particles is able to produce powder milk from in natura milk (cattle or goat), with the same quality of spray dryer, however, operating at low cost. The method of drying in spouted bed consists of injecting milk emulsion on the bed of inert particles gushed by hot air. This emulsion covers the particles with a thin film, which dries and is reduced to powder during the circulation of inerts inside the bed. The powder is dragged by exhaustion air and separated in the cyclone. The friction among particles resulted from the particles circulation, encourages high taxes of shear in the thin film of emulsion, breaking the cohesive forces and making this process possible. Studying the drying process and the powder goat milk production in one unit of spouted bed with inert particles, seeing the development of a low cost technological route for powder milk production is the aim of this thesis. The powder milk produced by this route must attend the local demand of food industries which need an intermediate product to be used as a food ingredient (ice-cream, milk candy). In order to reach this aim, this thesis approaches the aspects related to physical, thermodynamics and physic-chemicals characteristics of goat milk, whose complete data are still inexistent in the literature. The properties of materials are of great importance to the project of any process which involves the operations of transportation of movement, heat and mass quantity, such as the dryers which operate in fluid dynamically active regime, like the spouted bed. It was obtained new data related to the goat milk properties in function of concentration of solids and temperature. It is also important to mention the study developed about the kinetic of solids retention in the bed of inert particles during the drying of goat milk. It was found more adequate processes conditions to the proposed technological route to be implemented in small and micro-industries, with simplifications in the system of milk injection as well as in the form of operation of the dryer. Important data were obtained for a posterior stage of this research which involves the v modeling, simulation, control and optimization of the process. The results obtained in this thesis, in relation to process performance as well as to the quality of produced powder milk validate the proposal of using the spouted bed dryer in the production of powder goat milk

Effect of ion concentration of ionomer in electron injection layer of polymer light-emitting devices

Polymer light-emitting devices (PLEDs) with poly(2-methoxy-5-hexyloxy)-p-phenylenevinylene (OC1OC6-PPV) as the emissive layer were studied with an electron injection layer of ionomers consisting of copolymers of styrene and methylmethacrylate (PS/PMMA) with 3, 6 and 8 mol% degree of sulfonation. The ionomers were able to form very thin films over the emissive layer, with less than 30 nm. Additionally, the presence of ion pairs of ionomer suppresses the tendency toward dewetting of the thin film of ionomer (similar to 10 nm) which can cause malfunction of the device. The effect of the ionomers was investigated as a function of the ion content. The devices performance, characterized by their current density and luminance intensity versus voltage, showed a remarkable increase with the ionomer layer up to 6 mol% of ionic groups, decreasing after that for the 8 mol% ionomer device. The study of the impedance spectroscopy in the frequency range from 0.1 to 10(6) Hz showed that the injection phenomena dominate over the transport in the electroluminescent polymer bulk. (c) 2006 Elsevier B.V. All rights reserved.

Nanostructured hybrid films containing nanophosphor: Fabrication and electronic spectral properties

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

Filmes nanométricos de FeN e ALN crescidos por sputtering e aplicações do efeito peltier

This study will show the capability of the reactive/nonreactive sputtering (dc/rf) technique at low power for the growth of nanometric thin films from magnetic materials (FeN) and widegap semiconductors (AlN), as well as the technological application of the Peltier effect using commercial modules of bismuth telluride (Bi2Te3). Of great technological interest to the high-density magnetic recording industry, the FeN system represents one of the most important magnetic achievements; however, diversity of the phases formed makes it difficult to control its magnetic properties during production of devices. We investigated the variation in these properties using ferromagnetic resonance, MOKE and atomic force microscopy (AFM), as a function of nitrogen concentration in the reactive gas mixture. Aluminum nitride, a component of widegap semiconductors and of considerable interest to the electronic and optoelectronic industry, was grown on nanometric thin film for the first time, with good structural quality by non-reactive rf sputtering of a pure AlN target at low power (≈ 50W). Another finding in this study is that a long deposition time for this material may lead to film contamination by materials adsorbed into deposition chamber walls. Energy-dispersive X-ray (EDX) analysis shows that the presence of magnetic contaminants from previous depositions results in grown AlN semiconductor films exhibiting magnetoresistance with high resistivity. The Peltier effect applied to commercially available compact refrigeration cells, which are efficient for cooling small volumes, was used to manufacture a technologically innovative refrigerated mini wine cooler, for which a patent was duly registered

Fases magnéticas de sistemas nanoestruturados de terras-raras

There is presently a worldwide interest in artificial magnetic systems which guide research activities in universities and companies. Thin films and multilayers have a central role, revealing new magnetic phases which often lead to breakthroughs and new technology standards, never thought otherwise. Surface and confinement effects cause large impact in the magnetic phases of magnetic materials with bulk spatially periodic patterns. New magnetic phases are expected to form in thin film thicknesses comparable to the length of the intrinsic bulk magnetic unit cell. Helimagnetic materials are prototypes in this respect, since the bulk magnetic phases consist in periodic patterns with the length of the helical pitch. In this thesis we study the magnetic phases of thin rare-earth films, with surfaces oriented along the (002) direction. The thesis includes the investigation of the magnetic phases of thin Dy and Ho films, as well as the thermal hysteresis cycles of Dy thin films. The investigation of the thermal hysteresis cycles of thin Dy films has been done in collaboration with the Laboratory of Magnetic Materials of the University of Texas, at Arlington. The theoretical modeling is based on a self-consistent theory developed by the Group of Magnetism of UFRN. Contributions from the first and second neighbors exchange energy, from the anisotropy energy and the Zeeman energy are calculated in a set of nonequivalent magnetic ions, and the equilibrium magnetic phases, from the Curie temperature up to the Nèel temperature, are determined in a self-consistent manner, resulting in a vanishing torque in the magnetic ions at all planes across the thin film. Our results reproduce the known isothermal and iso-field curves of bulk Dy and Ho, and the known spin-slip phases of Ho, and indicate that: (i) the confinement in thin films leads to a new magnetic phase, with alternate helicity, which leads to the measured thermal hysteresis of Dy ultrathin films, with thicknesses ranging from 4 nm to 16 nm; (ii) thin Dy films have anisotropy dominated surface lock-in phases, with alignment of surface spins along the anisotropy easy axis directions, similar to the known spin-slip phases of Ho ( which form in the bulk and are commensurate to the crystal lattice); and (iii) the confinement in thin films change considerably the spin-slip patterns of Ho.

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

Synthesis and characterization of Fe(III)-doped ceramic membranes of titanium dioxide and its application in photoelectrocatalysis of a textile dye

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

Material processing by plasma shock wave generated in an inverse Z-pinch plasma expander

The applicability of plasma shock wave for material processing was investigated using modified inverse Z-pinch device. Shock wave expanding speed and plasma spectral analysis were studied using an internal magnetic,probe and spatially collimated light spectroscopy. The material processing capability of the device was shown by many different surface analysis techniques such as AES, IRS, EPM and SEM. The interactions between a plasma shock wave of similar to4x10(6) cm/s speed with a Si substrate surface shows some ion implantation capability using a nitrogen plasma and thin film formation using a methane plasma.

Obtaining of Nanoapatite in Ti-7.5Mo Surface After Nanotube Growth

Titanium and their alloys have been used for biomedical applications due their excellent mechanical properties, corrosion resistance and biocompatibility. However, they are considered bioinerts materials because when they are inserted into the human body they are cannot form a chemical bond with bone. In several studies, the authors have attempted to modify their characteristic with treatments that changes the material surface. The purpose of this work was to evaluate obtaining of nanoapatite after growing of the nanotubes in surface of Ti-7.5Mo alloy. Alloy was obtained from c.p. titanium and molibdenium by using an arc-melting furnace. Ingots were submitted to heat treatment and they were cold worked by swaging. Nanotubes were processed using anodic oxidation of alloy in electrolyte solution. Surfaces were investigated using scanning electron microscope (SEM), FEG-SEM and thin-film x-ray diffraction. The results indicate that nanoapatite coating could form on surface of Ti-7.5Mo experimental alloy after nanotubes growth.

Dielectric relaxation of vegetable-based polyurethane

Vegetable-based polyurethane (PU) was prepared in the thin film form by spin coating. This polymer is synthesised from castor oil, which can be extracted from the seeds of a native plant in Brazil called mamona. This polymer is biocompatible and is being used as material for artificial bone. The PU was characterised by dielectric spectroscopy in a wide range of frequency (10(-5) Hz to 10(5) Hz) and by thermally stimulated discharge current (TSDC) measurements. The glass transition temperature (T-g=39degreesC) was determined and using the initial rise method the activation energy was found to be 1.58 eV. (C) 2003 Kluwer Academic Publishers.

Electromechanical properties of 0-3 vegetable based polyurethane and lead zirconate titanate composite.

Composite made of Lead Zirconate Titranate (PZT) ceramic powder and castor oil based polyurethane (PU) were prepared in the thin film form with 0-3 connectivity by spin coating. The composite films were obtained in the thickness range of 100 mum to 300 mum using 33-vol.% of ceramic. The samples mechanical resistance. The material was characterised by dielectric spectroscopy, thermally stimulated discharge current (TSDC), hysteresis measurements and laser-intensity-modulation method (LIMM). The pyroelectric coefficient at 343 K was 7x10(-5) C.m(-2) K-1 for the sample poled with 10 MV/m at 373 K for Ih. The results show that this new composite can be used as suitable piezo and pyroelectric sensors.

Dielectric and pyroelectric properties of a composite of ferroelectric ceramic and polyurethane

Flexible piezo- and pyroelectric composite was made in the thin film form by spin coating. Lead Zirconate Titanate (PZT) ceramic powder was dispersed in a castor oil-based polyurethane (PU) matrix, providing a composite with 0-3 connectivity. The dielectric data, measured over a wide range of frequency (10(-5) Hz to 105 Hz), shows a loss peak around 100 Hz related with impurities in the polymer matrix. There is also an evidence of a peak in the range 10(-4) Hz, possibly originating from the glass transition temperature T of the polymer. The pyroelectric coefficient at 34 K is 7.0x10(-5) C(.)m(-2.)K(-1) which is higher than that of P-PVDF (1X10(-5) C(.)m(-2.)K(-1)).