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

Diagnóstico de descarga de cátodo oco de ar e pós-descarga Ar N2 por espectroscopia de emissão óptica e espectrometria de massa

Many applications require that the plasma discharge is produced apart from the surface to be processed, thus preventing damage caused by bombardment and/or plasma radiation. In the post-discharge regime in various applications thermally sensitive materials can be used. In this work, active species produced by discharge and post-discharge hollow cathode were diagnosed by optical emission spectroscopy and mass spectrometry. The discharge was produced with the gases Ar and Ar - N2 gas flow ranging from 1 to 6 cm3/min and electric current between 150 to 600 mA. It was estimated that the ion density inside the hollow cathode, with 2 mm diameter ranged between 7.71 and 14.1 x 1015 cm-3. It was observed that the gas flow and the electric current changes the emission intensity of Ar and N2 species. The major ionic species detected by quadrupole mass spectrometry were Ar+ and N2+. The ratio of optical emission intensities of N2(1 +)/Ar(811 nm) was related to the partial pressure of N2 after the hollow cathode discharge at low pressure

Comparação entre técnicas de nitretação em cátodo oco e gaiola catódica na deposição de TiN

The plasma nitriding has been used in industrial and technological applications for large-scale show an improvement in the mechanical, tribological, among others. In order to solve problems arising in the conventional nitriding, for example, rings constraint (edge effect) techniques have been developed with different cathodes. In this work, we studied surfaces of commercially pure titanium (Grade II), modified by plasma nitriding treatment through different settings cathodes (hollow cathode, cathodic cage with a cage and cathodic cage with two cages) varying the temperature 350, 400 and 430oC, with the goal of obtaining a surface optimization for technological applications, evaluating which treatment generally showed better results under the substrate. The samples were characterized by the techniques of testing for Atomic Force Microscopy (AFM), Raman spectroscopy, microhardness, X-ray diffraction (XRD), and a macroscopic analysis. Thus, we were able to evaluate the processing properties, such as roughness, topography, the presence of interstitial elements, hardness, homogeneity, uniformity and thickness of the nitrided layer. It was observed that all samples were exposed to nitriding modified relative to the control sample (no treatment) thus having increased surface hardness, the presence of TiN observed by XRD as per both Raman and a significant change in the roughness of the treated samples . It was found that treatment in hollow cathode, despite having the lowest value of microhardness between treated samples, was presented the lowest surface roughness, although this configuration samples suffer greater physical aggressiveness of treatment

Efeito antibacteriano de tecidos têxteis revestidos por prata através da técnica de deposição por plasma

In this study, it has been investigated the influence of silver film deposition onto 100% polyester woven and non-woven, on the survival of Escherichia coli and Staphylococcus aureus in contact with these surfaces. The treatment was performedin a chamber containing the working gas at low pressure (~ 10-2 mbar). Some process parameters such as as voltage: 470 V; pressure: 10-2 mbar; current : 0.40 A and gas flow: 6 and 10 cm3/min were kept constant. For the treatments with purêargon plasma using a flow of 6 and 10 cm3/min, different treatment times were evaluated, such as, 10 , 20, 30, 40, 50 and 60 minutes. Contact angle (sessile drop), measurements were used to determine the surface tension of the treated fabrics and its influence on the bacteria grow as weel as the possibilities of a biofilm formation. The formation of a silver film, as well as the amount of this element was verified byEDX technique. The topography was observed through scanning electron microscopy (SEM) to determine the size of silver grains formed on the surfaces of the fabric and assess homogeneity of treatment. The X-ray diffraction (XRD) was used to analyze the structure of silver film deposition. The woven fabric treatments enabled the formation of silver particulate films with particle size larger than the non-woven fabrics. With respect to bacterial growth, all fabrics were shown to be bactericidal for Staphylococcus aureus (S. aureus), while for the Escherichia coli (E. coli), the best results were found for the non-woven fabric (TNT) treated with a flow of 10 cm3/min to both bacteria

Simulação da transferência de calor em amostras aquecidas por plasma

The processing of materials through plasma has been growing enough in the last times in several technological applications, more specifically in surfaces treatment. That growth is due, mainly, to the great applicability of plasmas as energy source, where it assumes behavior thermal, chemical and/or physical. On the other hand, the multiplicity of simultaneous physical effects (thermal, chemical and physical interactions) present in plasmas increases the complexity for understanding their interaction with solids. In that sense, as an initial step for the development of that subject, the present work treats of the computational simulation of the heating and cooling processes of steel and copper samples immersed in a plasma atmosphere, by considering two experimental geometric configurations: hollow and plane cathode. In order to reach such goal, three computational models were developed in Fortran 90 language: an one-dimensional transient model (1D, t), a two-dimensional transient model (2D, t) and a two-dimensional transient model (2D, t) which take into account the presence of a sample holder in the experimental assembly. The models were developed based on the finite volume method and, for the two-dimensional configurations, the effect of hollow cathode on the sample was considered as a lateral external heat source. The main results obtained with the three computational models, as temperature distribution and thermal gradients in the samples and in the holder, were compared with those developed by the Laboratory of Plasma, LabPlasma/UFRN, and with experiments available in the literature. The behavior showed indicates the validity of the developed codes and illustrate the need of the use of such computational tool in that process type, due to the great easiness of obtaining thermal information of interest

Desenvolvimento de um código computacional para simulação e análise de espectros atômicos

The aim of this work was the development a computer code for simulation and analysis of atomic spectra from databases constructed from the literature. There were created four routines that can be useful for spectroscopic studies in the atomic processes of laser isotope separation. In the first routine, Possible Transitions, the program checks the possible electron transitions from an energy level of the atom present in the database considering the selection rules for an electric dipole transition. The second routine, Locator Transitions, checks the possible electronic transitions within a user-specified spectral region. The routine Spectra Simulator creates simulated spectra using the graphical application gnuplot through lorentzian curve and finally, the routine Electronic Temperature determines the temperature of electronic excitation of the atom, thought the Boltzmann Plot Method. To test the reliability of the program there were obtained experimental emission spectra of a hollow cathode discharge of dysprosium and argon as a buffer gas. The hollow cathode discharge has been subjected to different values of operating currents and pressure of inert gas. The spectra obtained were treated with the assistance of program routines developed (Transition Locator and Spectra Simulator) and temperatures electronic excitation of the atoms of dysprosium in the different discharge conditions were calculated (routine Electronic Temperature). The results showed that the electronic excitation temperature of the neutral dysprosium atoms in the hollow cathode discharge increases with increasing current applied to the cathode and also by increasing the gas pressure buffer. The determination coefficients, R2, obtained by the Electronic Temperature routine using the linear adjust of the Boltzmann Plot Method were greater... (Complete abstract click electronic access below)

Dispositivo de microdescargas em gases na pressão atmosférica

This work describes the development of an electro-mechanical micro-discharges device operating at ambient condition of pressure and temperature, capable to produce plasma jets for surface finishing. The discharges are produced through a needle shape electrode hollow cathode type by which flows the helium gas. The voltage applied on the electrode is provided for an AC/AC switching voltage converter of full-bridge topology. The converter is energized by a power line of 110/220 VAC, 60 Hz and gives a 1000 V peak-to-peak from 5 kHz to 40 kHz square waveform output. The output frequency is defined by a control signal provided by an external signal generator. The equipment setup includes output acquisition of voltage and current and a photo-detector for photo-electrical measurements, which allows an optical characterization of the plasma jet

Dispositivo de microdescargas em gases na pressão atmosférica

This work describes the development of an electro-mechanical micro-discharges device operating at ambient condition of pressure and temperature, capable to produce plasma jets for surface finishing. The discharges are produced through a needle shape electrode hollow cathode type by which flows the helium gas. The voltage applied on the electrode is provided for an AC/AC switching voltage converter of full-bridge topology. The converter is energized by a power line of 110/220 VAC, 60 Hz and gives a 1000 V peak-to-peak from 5 kHz to 40 kHz square waveform output. The output frequency is defined by a control signal provided by an external signal generator. The equipment setup includes output acquisition of voltage and current and a photo-detector for photo-electrical measurements, which allows an optical characterization of the plasma jet

Efeito antibacteriano de tecidos têxteis revestidos por prata através da técnica de deposição por plasma

In this study, it has been investigated the influence of silver film deposition onto 100% polyester woven and non-woven, on the survival of Escherichia coli and Staphylococcus aureus in contact with these surfaces. The treatment was performedin a chamber containing the working gas at low pressure (~ 10-2 mbar). Some process parameters such as as voltage: 470 V; pressure: 10-2 mbar; current : 0.40 A and gas flow: 6 and 10 cm3/min were kept constant. For the treatments with purêargon plasma using a flow of 6 and 10 cm3/min, different treatment times were evaluated, such as, 10 , 20, 30, 40, 50 and 60 minutes. Contact angle (sessile drop), measurements were used to determine the surface tension of the treated fabrics and its influence on the bacteria grow as weel as the possibilities of a biofilm formation. The formation of a silver film, as well as the amount of this element was verified byEDX technique. The topography was observed through scanning electron microscopy (SEM) to determine the size of silver grains formed on the surfaces of the fabric and assess homogeneity of treatment. The X-ray diffraction (XRD) was used to analyze the structure of silver film deposition. The woven fabric treatments enabled the formation of silver particulate films with particle size larger than the non-woven fabrics. With respect to bacterial growth, all fabrics were shown to be bactericidal for Staphylococcus aureus (S. aureus), while for the Escherichia coli (E. coli), the best results were found for the non-woven fabric (TNT) treated with a flow of 10 cm3/min to both bacteria

Análise Completa das Fibras de Bragg de Núcleo Oco.

A evolução nos sistemas digitais de comunicação está intrinsicamente relacionada ao desenvolvimento da tecnologia de fibras ópticas. Desde a sua criação, na década de 60, inúmeras pesquisas vem sendo realizadas com o intuito de aumentar a capacidade de informação transmitida, por meio da redução da atenuação, controle da dispersão cromática e eliminação das não-linearidades. Neste contexto, as Fibras de Bragg surgem como uma estrutura de grande potencialidade para se minimizar tais inconvenientes. As fibras de Bragg possuem um mecanismo de operação diferente em relação às fibras tradicionais de suportar os modos confinados. Nelas, o núcleo possui um baixo índice de refração, e a casca é constituída por anéis dielétricos de diferentes índices de refração, alocados alternadamente. Para uma fibra de Bragg com núcleo oco, como a considerada neste trabalho, há perdas decorrentes dos modos de fuga. Portanto, a análise da dispersão destas estruturas se situa no plano complexo, tornando-a muito difícil. Esta dissertação será fundamentada em uma estratégia imprescindível à análise dos modos transversais TE0m, TM0m e dos híbridos. Os resultados encontrados são validados confrontando-os com os obtidos na literatura. O trabalho discutirá as perdas e dispersões dos modos citados, e os resultados obtidos poderão nortear as pesquisas das fibras de Bragg.

Construção, caracterização e aplicação de eletrodos para descarga por arco de cátodo oco

The system built to characterize electrodes and, consequently, deposited fine films are constituted by a hollow cathode that works to discharges and low pressures (approximately 10-3 to 5 mbar), a source DC (0 to 1200 V), a cylindrical camera of closed borossilicato for flanges of stainless steel with an association of vacuum bombs mechanical and spread. In the upper flange it is connected the system of hollow cathode, which possesses an entrance of gas and two entrances for its refrigeration, the same is electrically isolated of the rest of the equipment and it is polarized negatively. In front of the system of hollow cathode there is a movable sample in stainless steel with possibility of moving in the horizontal and vertical. In the vertical, the sample can vary its distance between 0 and 70 mm and, in the horizontal, can leave completely from the front of the hollow cathode. The sample and also the cathode hollow are equipped with cromel-alumel termopares with simultaneous reading of the temperatures during the time of treatment. In this work copper electrodes, bronze, titanium, iron, stainless steel, powder of titanium, powder of titanium and silício, glass and ceramic were used. The electrodes were investigated relating their geometry change and behavior of the plasma of the cavity of hollow cathode and channel of the gas. As the cavity of hollow cathode, the analyzed aspects were the diameter and depth. With the channel of the gas, we verified the diameter. In the two situations, we investigated parameters as flow of the gas, pressure, current and applied tension in the electrode, temperature, loss of mass of the electrode with relationship at the time of use. The flow of gas investigated in the electrodes it was fastened in a work strip from 15 to 6 sccm, the constant pressure of work was among 2.7 to 8 x 10-2 mbar. The applied current was among a strip of work from 0,8 to 0,4 A, and their respective tensions were in a strip from 400 to 220 V. Fixing the value of the current, it was possible to lift the curve of the behavior of the tension with the time of use. That curves esteem in that time of use of the electrode to its efficiency is maximum. The temperatures of the electrodes were in the dependence of that curves showing a maximum temperature when the tension was maximum, yet the measured temperatures in the samples showed to be sensitive the variation of the temperature in the electrodes. An accompaniment of the loss of mass of the electrode relating to its time of use showed that the electrodes that appeared the spherical cavities lost more mass in comparison with the electrodes in that didn't appear. That phenomenon is only seen for pressures of 10-2 mbar, in these conditions a plasma column is formed inside of the channel of the gas and in certain points it is concentrated in form of spheres. Those spherical cavities develop inside of the channel of the gas spreading during the whole extension of the channel of the gas. The used electrodes were cut after they could not be more used, however among those electrodes, films that were deposited in alternate times and the electrodes that were used to deposit films in same times, those films were deposited in the glass substrata, alumina, stainless steel 420, stainless steel 316, silício and steel M2. As the eletros used to deposit films in alternate time as the ones that they were used to deposit in same times, the behavior of the thickness of the film obeyed the curve of the tension with relationship the time of use of the electrode, that is, when the tension was maximum, the thickness of the film was also maximum and when the tension was minimum, the thickness was minimum and in the case where the value of the tension was constant, the thickness of the film tends to be constant. The fine films that were produced they had applications with nano stick, bio-compatibility, cellular growth, inhibition of bacterias, cut tool, metallic leagues, brasagem, pineapple fiber and ornamental. In those films it was investigated the thickness, the adherence and the uniformity characterized by sweeping electronic microscopy. Another technique developed to assist the production and characterization of the films produced in that work was the caloteste. It uses a sphere and abrasive to mark the sample with a cap impression, with that cap form it is possible to calculate the thickness of the film. Through the time of life of the cathode, it was possible to evaluate the rate of waste of its material for the different work conditions. Values of waste rate up to 3,2 x 10-6 g/s were verified. For a distance of the substratum of 11 mm, the deposited film was limited to a circular area of 22 mm diameter mm for high pressures and a circular area of 75 mm for pressure strip. The obtained films presented thickness around 2,1 µm, showing that the discharge of arch of hollow cathode in argon obeys a curve characteristic of the tension with the time of life of the eletrodo. The deposition rate obtained in this system it is of approximately 0,18 µm/min

Estudo sobre a redução aluminotérmica de Ta2O5 e TiO2 usando descarga de cátodo oco

In this study it was used two metallic oxides, Ta2O5 and TiO2, in order to obtain metallic powders of Ta and Ti through aluminothermic reduction ignited by plasma. Ta2O5 and TiO2 powders were mixed with Al in a planetary mill, using different milling times. A thermal analysis study (DTA and TG) was carried out, in order to know the temperature to react both the mixtures. Then, these mixtures were submitted to a hollow cathode discharge, where they were reacted using aluminothermic reduction ignited by plasma. The product obtained was characterized by XRD and SEM, where it was proven the possibility of producing these metallic particles, different from the conventional process, where metallic ingots are obtained. It was verified that the aluminothermic reduction ignited by plasma is able to produce metallic powders of Ta and Ti, and a higher efficiency was observed to the process with Ta2O5-Al mixtures. Among different microstructural aspects observed, it can be noted the presence of metallic nanoparticles trapped into an Al2O3 matrix, besides acicular structures (titanium) and dendritic structures (tantalum), which are a product characteristic from a fast cooling

Biomecânica e otimização topológica com H-adaptatividade em implantes dentários nitretados a plasma em cátodo oco

In recent years there has been a significant growth in technologies that modify implant surfaces, reducing healing time and allowing their successful use in areas with low bone density. One of the most widely used techniques is plasma nitration, applied with excellent results in titanium and its alloys, with greater frequency in the manufacture of hip, ankle and shoulder implants. However, its use in dental implants is very limited due to high process temperatures (between 700 C o and 800 C o ), resulting in distortions in these geometrically complex and highly precise components. The aim of the present study is to assess osseointegration and mechanical strength of grade II nitrided titanium samples, through configuration of hollow cathode discharge. Moreover, new formulations are proposed to determine the optimum structural topology of the dental implant under study, in order to perfect its shape, make it efficient, competitive and with high definition. In the nitriding process, the samples were treated at a temperature of 450 C o and pressure of 150 Pa , during 1 hour of treatment. This condition was selected because it obtains the best wettability results in previous studies, where different pressure, temperature and time conditions were systematized. The samples were characterized by X-ray diffraction, scanning electron microscope, roughness, microhardness and wettability. Biomechanical fatigue tests were then conducted. Finally, a formulation using the three dimensional structural topology optimization method was proposed, in conjunction with an hadaptive refinement process. The results showed that plasma nitriding, using the hollow cathode discharge technique, caused changes in the surface texture of test specimens, increases surface roughness, wettability and microhardness when compared to the untreated sample. In the biomechanical fatigue test, the treated implant showed no flaws, after five million cycles, at a maximum fatigue load of 84.46 N. The results of the topological optimization process showed well-defined optimized layouts of the dental implant, with a clear distribution of material and a defined edge

Redução carbotérmica de TiO2 por descarga em cátodo oco

In this study we used the plasma as a source of energy in the process of carbothermic reduction of rutile ore (TiO2). The rutile and graphite powders were milled for 15 h and placed in a hollow cathode discharge produced by in order to obtain titanium carbonitride directly from the reaction, was verified the influence of processing parameters of plasma temperature and time in the synthesis of TiCN. The reaction was carried out at 600, 700 and 800˚C for 3 to 4 hours in an atmosphere of nitrogen and argon. During all reactions was monitored by plasma technique of optical emission spectroscopy (EEO) to check the active species present in the process of carbothermal reduction of TiO2. The powder obtained after the reactions were characterized by the techniques of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The technique of EEO were detected in all reactions the spectra CO and NO, and these gas-phase resulting from the reduction of TiO2. The results of X-ray diffraction confirmed the reduction, where for all conditions studied there was evidence of early reduction of TiO2 through the emergence of intermediate oxides. In the samples reduced at 600 and 700˚C, there was only the phase Ti6O11, those reduced to 800˚C appeared Ti5O9 phases, and Ti6O11 Ti7O13, confirming that the carbothermal reduction in plasma, a reduction of the ore rutile (TiO2) in a series of intermediate titanium oxide (TinO2n-1) where n varies between 5 and 10