Aplicação de tecnologias eletroquímicas (oxidação via radicais hidroxila, oxidação mediada via cloro ativo e eletrocoagulação) para o tratamento de efluentes reais ou sintéticos

In this work the degradation of real and synthetic wastewater was studied using electrochemical processes such as oxidation via hydroxyl radicals, mediated oxidation via active chlorine and electrocoagulation. The real effluent used was collected in the decanter tank of the Federal University of Rio Grande do Norte (ETE-UFRN) of Effluent Treatment Plant and the other a textile effluent dye Ácido Blue 113 (AB 113) was synthesized in the laboratory. In the electrochemical process, the effects of anode material, current density, the presence and concentration of chloride as well as the active chlorine species on site generated were evaluated. Electrodes of different compositions, Ti/Pt, Ti/Ru0,3Ti0,7O2, BDD, Pb/PbO2 and Ti/TiO2-nanotubes/PbO2 were used as anodes. These electrodes were subjected to electroanalytical analysis with the goal of checking how happen the anodic and cathodic processes across the concentrations of NaCl and supporting electrolyte used. The potential of oxygen evolution reaction were also checked. The effect of active chlorine species formed under the process efficiency was evaluated by removing the organic matter in the effluent-ETE UFRN. The wastewater treatment ETE-UFRN using Ti/Pt, DDB and Ti/Ru0,3Ti0,7O2 electrodes was evaluated, obtaining good performances. The electrochemical degradation of effluent-UFRN was able to promote the reduction of the concentration of TOC and COD in all tested anodes. However, Ti/Ru0,3Ti0,7O2 showed a considerable degradation due to active chlorine species generated on site. The results obtained from the electrochemical process in the presence of chloride were more satisfactory than those obtained in the absence. The addition of 0.021 M NaCl resulted in a faster removal of organic matter. Secondly, was prepared and characterized the electrode Ti/TiO2-nanotubes/PbO2 according to what the literature reports, however their preparation was to disk (10 cm diameter) with surface area and higher than that described by the same authors, aiming at application to textile effluent AB 113 dye. SEM images were taken to observe the growth of TiO2 nanotubes and confirm the electrodeposition of PbO2. Atomic Force Microscope was also used to confirm the formation of these nanotubes. Furthermore, was tested and found a high electrochemical stability of the electrode Ti/TiO2-nanotubes/PbO2 for applications such as long-term indicating a good electrocatalytic material. The electrochemical oxidation of AB 113 using Ti/Pt, Pb/PbO2 and Ti/TiO2-nanotubes/PbO2 and Al/Al (electrocoagulation) was also studied. However, the best color removal and COD decay were obtained when Ti/TiO2-nanotubes/PbO2 was used as the anode, removing up to 98% of color and 92,5% of COD decay. Analysis of GC/MS were performed in order to identify possible intermediates formed in the degradation of AB 113.

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

Aplicação da técnica eletroanalítica de pulso diferencial usando o eletrodo de carbono vítreo modificado com cisteína para monitorar a degradação eletroquímica de ácido oxálico

In this paper, the technique of differential pulse voltammetry (DPV) has been studied for monitoring the concentration of oxalic acid (OA) during their electrochemical oxidation (EO) in acidic medium using platinum anode supported on titanium (Ti / Pt). The DPV was standardized and optimized using a glassy carbon electrode modified with cysteine. The modification with cysteine was developed electrochemically, forming a polymeric film on the surface of the glassy carbon electrode. The formation of the polymer film was confirmed by analysis of scanning electron microscope and atomic force microscope, confirming the modification of the electrode. The electrochemical degradation was developed using different current densities 10, 20 30 and 40 mA cm -2 electrode with Ti / Pt observing the degradation of oxalic acid, and monitored using the method of KMnO4 titration. However, the analyzes with DPV showed the same behavior elimination of oxalic acid titration. Compared with the titration method classical observed and DPV could be a good fit, confidence limits of detection and confirming the applicability of the technique electroanalytical for monitoring the degradation of oxalic acid

Influência das espécies do plasma de N2 + O2 nas propriedades físicoquímicas das superfícies do pet

This work reports the influence of the poly (ethylene terephthalate) textile and films surface modification by plasmas of O2 and mixtures (N2 + O2), on their physical and chemical properties. The plasma surface polymeric modification has been used for many researchs, because it does not affect the environment with toxic agents, the alterations remains only at nanometric layers and this technique shows expressive results. Then, due to its good acceptance, the treatment was carried out in a vacuum chamber. Some parameters remained constant during all treatment, such as: Voltage 470 V; Pressure 1,250 Mbar; Current: 0, 10 A and gas flow: 10 cm3/min, using oxygen plasma alternating the treatment time 10 to 60 min with an increase of 10 min to each subsequent treatment. Also, the samples were treated with a gas mixture (nitrogen + oxygen) which was varied only the gas composition from 0 to 100% leaving the treatment time remaining constant to all treatment (10 min). The plasma treatment was characterized in-situ with Optics Emission Spectroscopy (OES), and the samples was characterized by contact angle, surface tension, Through Capillary tests, Raman spectroscopy, Infrared attenuated total reflection (IR-ATR) and atomic force microscopy, scanning electronic Microscopy (SEM) and X-ray Photoelectron Spectroscopy (XPS). The results showed that oxygen treated fabrics presented high wettability, due to the hydrophilic groups incorporation onto the surface formed through spputering of carbon atoms. For the nitrogen atmosphere, there is the a film deposition of amine groups. Treatment with small oxygen concentration in the mixture with nitrogen has a higher spputered species of the samples

Desenho e Construção de um protótipo gerador de jato de plasma frio a pressão atmosférica para aplicações biomédicas

Research for better performance materials in biomedical applications are constants. Thus recent studies aimed at the development of new techniques for modification of surfaces. The low pressure plasma has been highlighted for its versatility and for being environmentally friendly, achieving good results in the modification of physic chemical properties of materials. However, it is requires an expensive vacuum system and cannot able to generate superficial changes in specific regions. Furthermore, it is limits their use in polymeric materials and sensitive terms due to high process temperatures. Therefore, new techniques capable of generating cold plasma at atmospheric pressure (APPJ) were created. In order to perform surface treatments on biomaterials in specific regions was built a prototype capable of generating a cold plasma jet. The prototype plasma generator consists of a high voltage source, a support arm, sample port and a nozzle through which the ionized argon. The device was formed to a dielectric tube and two electrodes. This work was varied some parameters such as position between electrodes, voltage and electrical frequency to verify the behavior of glow discharges. The disc of titanium was polished and there was a surface modification. The power consumed, length, intensity and surface modifications of titanium were analyzed. The energy consumed during the discharges was observed by the Lissajous figure method. To check the length of the jets was realized with Image Pro Plus software. The modifications of the titanium surfaces were observed by optical microscopy (OM ) and atomic force microscopy (AFM ). The study showed that variations of the parameters such as voltage, frequency and geometric position between the electrodes influence the formation of the plasma jet. It was concluded that the plasma jet near room temperature and atmospheric pressure was able to cause modifications in titanium surface

Deposição de A/N por sputtering não reativo

In this work we deposit via non-reactive magnetron sputtering of radio-frequency nanofilmes of nitreto of aluminum(AlN). The nanofilms aluminum nitride are semiconductors materials with high thermal conductivity, high melting point, piezoelectricity and wide band gap (6, 2 eV) with hexagonal wurtzite crystal structure, belonging to the group of new materials called III-V nitrides in which together with the gallium nitride and indium nitride have attracted much interest because they have physical and chemical properties relevant to new technological applications, mainly in microelectronic and optoelectronic devices. Three groups were deposited with thicknesses nanofilms time dependent on two substrates (glass and silicon) at a temperature of 25 ° C. The nanofilms AlN were characterized using three techniques, X-ray diffraction, Raman spectroscopy and atomic force microscopy (AFM), examined the morphology of these. Through the analysis of X-rays get the thickness of each sample with its corresponding deposition rate. The analysis of X-rays also revealed that nanofilms are not crystalline, showing the amorphous character of the samples. The results obtained by the technique, atomic force microscopy (AFM) agree with those obtained using the technique of X-rays. Characterization by Raman spectroscopy revealed the existence of active modes characteristic of AlN in the samples

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

Avaliação microscópica dos fragmentos ósseos obtidos por diferentes métodos de osteotomia e de irrigação em aloenxertos irradiados e congelados de coelho

Oral and facial bone defects can undertake appearance, psychosocial well-being and stomathognatic function of its patients. Over the yerars several strategies for bone defect regeneration have arised to treat these pathologies, among them the use of frozen and irradiated bone allograft. Manipulation of bone grafts it s not determined yet, and several osteotomy alternatives can be observed. The present work evaluated with a microscope the bone fragments obtained from different osteotomy methods and irrigation on rings and blocks allografts irradiated and frozen at 80° negative in a rabbit model. The study is experimental in vitro and it sample was an adult male New Zealand rabbit. The animal was sacrificed to obtain long bones, that were submitted to freezing at 80º negative and irradiated with Cobalt- 60. Then the long bones were sectioned into 24 bone pieces, divided into 4 groups: G1 (n=06) osteotomy was performed with bur No. 6 forming rings with 5 mm thickness with high-speed handpiece with manual irrigation; G2 (n=06) osteotomy was performed with bur No. 6 forming rings with 5 mm thick with surgical motor with a manual irrigation rotation 1500 rpm; GA (n=06), osteotomy with trephine using manual irrigation with saline; and GB (n=06), osteotomy with trephine using saline from peristaltic pumps of surgical motor. Five bone pieces of each group were prepared for analysis on light microscopy (LM) and one on electronic scan electronic microscopy (SEM). On the SEM analysis edges surface, presence of microcracks and Smear Layer were evaluated. Analyzing osteotomy technics on SEM was observed: increased presence of microcracks cutting with high speed; increased presence of areas covered by Smear Layer when cutting with motor implant. The irrigation analysis with SEM was observed: that the presence of microcracks does not depend on the type of irrigation; on manual irrigation, there was greater discrepancy between the cutting lines. The descriptive analysis of the osteotomy and irrigation process on LM showed: histological analysis showing the bony margins with clear tissue changed layer, composed of blackened tissue of charred appearance near to the cortical bone; on the edges of the bony part, bone fragments that were displaced during the bone cut and bone irregularities were observed. After analysis of results we can conclude: that there was greater regularity of the bone cut using high-speed handpiece than using motor implant; the cut with trephine using saline irrigated from peristaltic pumps of surgical motor showed greater homogeneity when compared with manual irrigation; charred tissue was found in all obtained bone samples, whit no significant statistically difference on the proportion of carbonization of the two analysed technics

Influência da superfície do titânio nitretado a plasma em diferentes atmosferas na ativação de plaquetas sanguíneas

This study aimed to analyze the biological response of titanium surfaces modified by plasma Ar + N2 + H2. Titanium disks grade II received different surface treatments Ar + N2 + H2 plasma, constituting seven groups including only polished samples used as standard. Before and after treatment the samples were evaluated in terms of topography, crystal structure and wettability, using atomic force microscopy, X-ray diffraction, Raman spectroscopy and testing of the sessile drop, respectively. Rich plasma (PRP) was applied to the surfaces modified in culture plates. Images obtained by scanning electron microscopy of the adhered platelets were analyzed to verify the behavior of platelets in the different experimental conditions. We verified that the adition of H2 on plasma atmosphere resulted in more rough surfaces, with round tops. These surfaces, in contrast to that surfaces treated with high concentration of N2, are less propense to platelet aggregation and, consequently, to the formation of thrombus when applied in biomedical devices.

Estudo da deposição de filmes finos de BaTi(1-X)Zr(X)O3 por meio de planejamento Box-Behnken

Ferroelectric ceramics with perovskite structure (ABO3) are widely used in solid state memories (FeRAM’s and DRAM's) as well as multilayered capacitors, especially as a thin films. When doped with zirconium ions, BaTiO3-based materials form a solid solution known as barium zirconate titanate (BaTi1-xZrxO3). Also called BZT, this material can undergo significant changes in their electrical properties for a small variation of zirconium content in the crystal lattice. The present work is the study of the effects of deposition parameters of BaTi0,75Zr0,25O3 thin films by spin-coating method on their morphology and physical properties, through an experimental design of the Box-Behnken type. The resin used in the process has been synthesized by the polymeric precursor method (Pechini) and subsequently split into three portions each of which has its viscosity adjusted to 10, 20 and 30 mPa∙s by means of a rotary viscometer. The resins were then deposited on Pt/Ti/SiO2/Si substrates by spin-coating method on 15 different combinations of viscosity, spin speed (3000, 5500 and 8000 rpm) and the number of deposited layers (5, 8 and 11 layers) and then calcined at 800 ° C for 1 h. The phase composition of the films was analyzed by X-ray diffraction (XRD) and indexed with the JCPDS 36-0019. Surface morphology and grain size were observed by atomic force microscopy (AFM) indicating uniform films and average grain size around 40 nm. Images of the cross section of the films were obtained by scanning electron microscopy field emission (SEM-FEG), indicating very uniform thicknesses ranging from 140-700 nm between samples. Capacitance measurements were performed at room temperature using an impedance analyzer. The films presented dielectric constant values of 55-305 at 100kHz and low dielectric loss. The design indicated no significant interaction effects between the deposition parameters on the thickness of the films. The response surface methodology enabled better observes the simultaneous effect of variables.

Influência das espécies do plasma de N2 + O2 nas propriedades físicoquímicas das superfícies do pet

This work reports the influence of the poly (ethylene terephthalate) textile and films surface modification by plasmas of O2 and mixtures (N2 + O2), on their physical and chemical properties. The plasma surface polymeric modification has been used for many researchs, because it does not affect the environment with toxic agents, the alterations remains only at nanometric layers and this technique shows expressive results. Then, due to its good acceptance, the treatment was carried out in a vacuum chamber. Some parameters remained constant during all treatment, such as: Voltage 470 V; Pressure 1,250 Mbar; Current: 0, 10 A and gas flow: 10 cm3/min, using oxygen plasma alternating the treatment time 10 to 60 min with an increase of 10 min to each subsequent treatment. Also, the samples were treated with a gas mixture (nitrogen + oxygen) which was varied only the gas composition from 0 to 100% leaving the treatment time remaining constant to all treatment (10 min). The plasma treatment was characterized in-situ with Optics Emission Spectroscopy (OES), and the samples was characterized by contact angle, surface tension, Through Capillary tests, Raman spectroscopy, Infrared attenuated total reflection (IR-ATR) and atomic force microscopy, scanning electronic Microscopy (SEM) and X-ray Photoelectron Spectroscopy (XPS). The results showed that oxygen treated fabrics presented high wettability, due to the hydrophilic groups incorporation onto the surface formed through spputering of carbon atoms. For the nitrogen atmosphere, there is the a film deposition of amine groups. Treatment with small oxygen concentration in the mixture with nitrogen has a higher spputered species of the samples