Efeito da moagem de alta energia na microestrutura e nas propriedades magnéticas do compósito wc-10%p.Co

This work a studied the high energy milling effect in microstructure and magnetic properties of the WC-10wt.%Co composite. The composite powders were prepared by mechanical mixed and milled at 2 hours, 100 hours, 200 hours and 300 hours in planetary milling. After this process the composite were compacted in stainless steel die with cylindrical county of 10 mm of diameter, at pressure 200 Mpa and sintered in a resistive furnace in argon atmosphere at 1400 oC for 5 min. The sintered composite were cutted, inlaid, sandpapered, and polished. The microestrutural parameters of the composite was analyzed by X-ray diffraction, scanning electronic microscopy, optical microscopy, hardness, magnetic propriety and Rietveld method analyze. The results shows, with milling time increase the particle size decrease, it possibility minor temperature of sintering. The increase of milling time caused allotropic transformation in cobalt phase and cold welding between particles. The cold welding caused the formation of the particle composite. The X-ray diffraction pattern of composite powders shows the WC peaks intensity decrease with the milling time increase. The X-ray diffraction pattern of the composite sintered samples shows the other phases. The magnetic measurements detected a significant increase in the coercitive field and a decrease in the saturation magnetization with milling time increase. The increase coercitive field it was also verified with decrease grain size with milling time increase. For the composite powders the increase coercitive field it was verified with particle size reduction and saturation magnetization variation is relate with the variation of free cobalt. The Rietveld method analyze shows at milling time increase the mean crystalline size of WC, and Co-cfc phases in composite sintered sample are higher than in composite powders. The mean crystallite size of Co-hc phase in composite powders is higher than in composite sintered sample. The mean lattice strains of WC, Co-hc and Co-cfc phases in composite powders are higher than in composite sintered samples. The cells parameters of the composite powder decrease at milling time increase this effect came from the particle size reduction at milling time increase. In sintered composite the cells parameters is constant with milling time increase

Síntese e caracterização da ferrita de MnZn obtida pelo método dos citratos precursores

It was synthesized MnZn ferrite with general formulae Mn1-xZnxFe2O4 (mol%), 0,3 ≤ x ≤ 0,7 by using the citrate precursor method. The precursors decomposition was studied by thermogravimetric analysis (TGA), differential thermogravimetric analysis (DTG), differential thermal analysis (DTA) and Fourier transform infrared (FTIR) of powder calcined at 350ºC/3,5h. X-ray diffraction pattern (XRD) of samples was done from 350 to 1200ºC/2h using various atmospheres. The power calcined at 350ºC/3,5h formed spinel phase. It is necessary atmosphere control to avoid secondary phase such as hematite. From 900 to 1200ºC was obtained 90,66 and 100% of MnZn spinel ferrite phase, respectively. Analysis by dispersive energy scanning (EDS) at 350ºC shows high Mn and Zn dispersion, indicating that the diffusion process was homogeneous. Semi-quantitative analysis by EDS verified that despite the atmosphere control during calcinations at high temperatures (< 800ºC) occurred ZnO evaporation causing stoichiometric deviation. Vibrating sample magnetometer (VSM) measures show soft ferrite material characteristics with Hc from 6,5 x 10-3 to 11,1 x 10-2 T. Saturation magnetization (Ms) and initial permeability (µi) of MnZn spinel phase obtained, respectively, from 14,3 to 83,8 Am2/kg and 14,1 to 62,7 (Am2/kg)T

Efeito da moagem de alta energia na microestrutura e nas propriedades magnéticas do compósito wc-10%p.Co

This work a studied the high energy milling effect in microstructure and magnetic properties of the WC-10wt.%Co composite. The composite powders were prepared by mechanical mixed and milled at 2 hours, 100 hours, 200 hours and 300 hours in planetary milling. After this process the composite were compacted in stainless steel die with cylindrical county of 10 mm of diameter, at pressure 200 Mpa and sintered in a resistive furnace in argon atmosphere at 1400 oC for 5 min. The sintered composite were cutted, inlaid, sandpapered, and polished. The microestrutural parameters of the composite was analyzed by X-ray diffraction, scanning electronic microscopy, optical microscopy, hardness, magnetic propriety and Rietveld method analyze. The results shows, with milling time increase the particle size decrease, it possibility minor temperature of sintering. The increase of milling time caused allotropic transformation in cobalt phase and cold welding between particles. The cold welding caused the formation of the particle composite. The X-ray diffraction pattern of composite powders shows the WC peaks intensity decrease with the milling time increase. The X-ray diffraction pattern of the composite sintered samples shows the other phases. The magnetic measurements detected a significant increase in the coercitive field and a decrease in the saturation magnetization with milling time increase. The increase coercitive field it was also verified with decrease grain size with milling time increase. For the composite powders the increase coercitive field it was verified with particle size reduction and saturation magnetization variation is relate with the variation of free cobalt. The Rietveld method analyze shows at milling time increase the mean crystalline size of WC, and Co-cfc phases in composite sintered sample are higher than in composite powders. The mean crystallite size of Co-hc phase in composite powders is higher than in composite sintered sample. The mean lattice strains of WC, Co-hc and Co-cfc phases in composite powders are higher than in composite sintered samples. The cells parameters of the composite powder decrease at milling time increase this effect came from the particle size reduction at milling time increase. In sintered composite the cells parameters is constant with milling time increase

Efeito do tratamento térmico do titânio sobre a proliferação de células pré-osteoblásticas

Titanium is a biomaterial widely employed in biomedical applications (implants, prostheses, valves, stents). Several heat treatments are usually used in order to obtain physical properties required to different applications. This work studied the influence of the heat treatment on microstructure of commercial pure titanium, and their consequences in growth and proliferation of MC3T3-E1 cells. Discs of titanium were treated in different temperatures, and characterized by optical microscopy, image analysis, wettabillity, roughness, hardness and X-ray diffraction. After the heat treatment, significant modifications in these properties were observed. Pattern images of titanium, before and after the cell culture, were compared by overlapping to analyze the influence of microstructure in microstructure and preferences guidance cells. However, in general, titanium discs that showed a higher residual strength also presented an increase of cells numbers on surface

Influência dos parâmetros de processo na deposição de nitreto de titânio por plasma em gaiola catódica

Titanium nitride films were grown on glass using the Cathodic Cage Plasma Deposition technique in order to verify the influence of process parameters in optical and structural properties of the films. The plasma atmosphere used was a mixture of Ar, N2 and H2, setting the Ar and N2 gas flows at 4 and 3 sccm, respectively and H2 gas flow varied from 0, 1 to 2 sccm. The deposition process was monitored by Optical Emission Spectroscopy (OES) to investigate the influence of the active species in plasma. It was observed that increasing the H2 gas flow into the plasma the luminescent intensities associated to the species changed. In this case, the luminescence of N2 (391,4nm) species was not proportional to the increasing of the H2 gas into the reactor. Other parameters investigated were diameter and number of holes in the cage. The analysis by Grazing Incidence X-Ray Diffraction (GIXRD) confirmed that the obtained films are composed by TiN and they may have variations in the nitrogen amount into the crystal and in the crystallite size. The optical microscopy images provided information about the homogeneity of the films. The atomic force microscopy (AFM) results revealed some microstructural characteristics and surface roughness. The thickness was measured by ellipsometry. The optical properties such as transmittance and reflectance (they were measured by spectrophotometry) are very sensitive to changes in the crystal lattice of the material, chemical composition and film thicknesses. Therefore, such properties are appropriate tools for verification of this process control. In general, films obtained at 0 sccm of H2 gas flow present a higher transmittance. It can be attributed to the smaller crystalline size due to a higher amount of nitrogen in the TiN lattice. The films obtained at 1 and 2 sccm of H2 gas flow have a golden appearance and XRD pattern showed peaks characteristics of TiN with higher intensity and smaller FWHM (Full Width at Half Maximum) parameter. It suggests that the hydrogen presence in the plasma makes the films more stoichiometric and becomes it more crystalline. It was observed that with higher number of holes in the lid of the cage, close to the region between the lid and the sample and the smaller diameter of the hole, the deposited film is thicker, which is justified by the most probability of plasma species reach effectively the sample and it promotes the growth of the film

Efetividade do clareamento dentário com peróxido de carbamida a 10% e avaliação dos efeitos adversos sobre o esmalte dentário

The aim of the present study was to assess the effectiveness and adverse effects on dental enamel caused by nightguard vital bleaching with 10% carbamide peroxide. This was accomplished through the interaction of researchers from different areas such as dentistry, materials engineering and physics. Fifty volunteers took part in the doubleblind randomized controlled clinical trial. They were allocated to an experimental group that used Opalescence PF 10% (OPA) and a control group that used a placebo gel (PLA). Fragments of human dental enamel from the vestibular surface of healthy premolars, extracted for orthodontic reasons, were fixed to the vestibular surface of the first upper molars of the volunteers for in situ observation. Bleaching was performed at night for 21 days. The observation periods included Baseline (BL), T0 (21 days), T30 (30 days after treatment) and T180 (180 days after treatment, only for the OPA group). Tooth color was assessed by comparing it with the Vita® scale and by the degree of satisfaction expressed by the volunteer. We also assessed adverse clinical effects, dental sensitivity and gingival bleeding. The study of adverse effects on enamel was conducted in vivo and in situ, using the DIAGNOdent® laser fluorescence device to detect mineral loss. Scanning electron microscopy (SEM) was used to check for superficial morphological alterations, energy dispersive spectrophotometry (EDS) to semiquantitatively assess chemical composition using the Ca/P ratio, and the x-ray diffraction (XRD) technique to observe alterations in enamel microstructure. The results showed that nightguard vital bleaching with 10% carbamide peroxide was effective in 96% of the cases, versus 8% for the PLA group. Dental sensitivity was present in 36% (9/25) of the cases. There was no significant association between gingival bleeding and the type of gel used (p = 1.00). In vivo laser fluorescence analysis showed no difference in values for the control group, whereas in the OPA group there was a statistically significant difference between baseline values in relation to the subsequent periods (p<0.01), with lower mean values for post-bleaching times. There was a significant difference between the groups for times T0 and T30. Micrographic analysis showed no enamel surface alterations related to the treatment performed. No significant alteration in Ca/P ratio was observed in the OPA group (p = 0.624) or in the PLA group (p = 0.462) for each of the observation periods, nor between the groups studied (p=0.102). The XRD pattern for both groups showed the presence of three-phase Hydroxyapatite according to JCPDS files (9-0432[Ca5(PO4)3(OH)], 18-0303[Ca3(PO4)2.xH2O] and 25-0166[Ca5(PO4)3(OH, Cl, F)]). No other peak associated to other phases was found, independent of the group analyzed, which reveals there was no disappearance, nucleation or phase transformation. Neither was there any alteration in peak pattern location. With the methodology and protocol used in this study, nightguard vital bleaching with 10% carbamide peroxide proved to be an effective and safe procedure for dental enamel

Aplicações de Dispositivos de Microondas utilizando Substrato EBG/PBG para Comunicações Móveis

The modern society depends on an efficient communications system able to of transmitting and receiving information with a higher speed and reliability every time. The need for ever more efficient devices raises optimization techniques of microstrip devices, such as techniques to increase bandwidth: thicker substrates and substrate structures with EBG (Electromagnetic Band Gap) and PBG (Photonic Band Gap). This work has how aims the study of the application of PBG materials on substrates of planar structures in microstrip, more precisely in directional quadrature couplers and in rat-race and impedance of transformers. A study of the planar structures in microstrip and substrates EBG is presented. The PBG substrates can be used to optimize the radiation through the air, thus reducing the occurrence of surface waves and the resulting diffraction edge responsible for degradation of radiation pattern. Through specific programs in FORTRAN Power Station obtained the frequencies and couplings for each structure. Are used the program PACMO - Computer Aided Design in Microwave. Results are obtained of the frequency and coupling devices, ranging the frequency band used (cellular communication and Wimax systems) and the permittivity of the substrate, comparing the results of conventional material and PBG materials in the s and p polarizations.

Síntese e caracterização de aluminofosfato impregnado com molibdênio/zinco visando a dessulfurização por adsorção

Discussions about pollution caused by vehicles emission are old and have been developed along the years. The search for cleaner technologies and frequent weather alterations have been inducing industries and government organizations to impose limits much more rigorous to the contaminant content in fuels, which have an direct impact in atmospheric emissions. Nowadays, the quality of fuels, in relation to the sulfur content, is carried out through the process of hydrodesulfurization. Adsorption processes also represent an interesting alternative route to the removal of sulfur content. Both processes are simpler and operate to atmospheric temperatures and pressures. This work studies the synthesis and characterization of aluminophosphate impregnate with zinc, molybdenum or both, and its application in the sulfur removal from the gasoline through the adsorption process, using a pattern gasoline containing isooctane and thiophene. The adsorbents were characterized by x-ray diffraction, differential thermal analysis (DTG), x-ray fluorescence and scanning electron microscopy (SEM). The specific area, volume and pore diameter were determined by BET (Brunauer- Emmet-Teller) and the t-plot method. The sulfur was quantified by elementary analysis using ANTEK 9000 NS. The adsorption process was evaluated as function of the temperature variation and initial sulfur content through the adsorption isotherm and its thermodynamic parameters. The parameters of entropy (ΔS), enthalpy variation (ΔH) and free Gibbs energy (ΔG) were calculated through the graph ln(Kd) versus 1/T. Langmuir, Freundlich and Langmuir-Freundlich models were adjusted to the experimental data, and the last one had presented better results. The thermodynamic tests were accomplished in different temperatures, such as 30, 40 and 50ºC, where it was concluded the adsorption process is spontaneous and exothermic. The kinetic of adsorption was studied by 24 h and it showed that the capability adsorption to the adsorbents studied respect the following order: MoZnPO > MoPO > ZnPO > AlPO. The maximum adsorption capacity was 4.91 mg/g for MoZnPO with an adsorption efficiency of 49%.

Utilização de rejeitos de Caulins na Síntese de Zeólita A

Three studies were performed using tailings kaolin for the synthesis of zeolite A. The first synthesis of zeolite A was performed using a kaolin waste generated from the beneficiation of kaolin for paper production process was studied. The kaolin waste was thermally activated at a temperature range of 550-800°C. For comparison was performed a synthesis pattern of Zeolite A(procedure IZA). The prepared materials were characterized by 27Al MAS NMR, X-ray diffraction and scanning electron microscopy with microprobe rays. The pre-tramento proved to be the most appropriate and suitable temperatures are between 600 and 700°C. Observed the formation of zeolite A in all materials, reaching 52% crystallinity, and the presence of phase sodalite and amorphous material. The second study was the use of a highly reactive metakaolin originating from the Jari region in the synthesis of zeolite A by a new method of hydrothermal synthesis. The zeolite is obtained pure and highly crystalline employing the Jari kaolin calcined at 600 ° C for 2h when the transformation to metakaolin occurs. Get to zeolite phase A at 4pm. The best crystallization time was of 24 h afforded a crystallinity of 67.9%. The third study was the evaluation of the NaOH / metakaolin and crystallization time on the synthesis of zeolite NaA from a sample of kaolin waste, named Kaolin Coverage. The experiments were performed using statistical design (axial points) and rejoinder the center point. The samples were characterized by X-ray diffraction (XRD), scanning microscopic analysis and chemical analysis using an EPMA microprobe. The results showed that a relationship exists between the amount of NaOH added and the crystallization time. The experiment performed using the lowest ratio NaOH / metakaolin (0.5) and shorter (4 h) produced an amorphous material. The increase ratio of NaOH / metakaolin and crystallization time leads to formation of a more crystalline NaA phase, but the presence of phase with sodalite as impurities

Variação espacial e sazonal de elementos maiores e traços no estuários do Rio Curimataú (RN), através de dados geoquímicos e de sensoriamento remoto

The Curimataú estuary is located in the oriental coast of Rio Grande do Norte State in Brazil. Its importance resides in the fact that this region possesses one of the last portions of preserved mangrove in the Rio Grande do Norte State. Nevertheless, it has been severely affected by many anthropogenic activities, as sugarcane monoculture and shrimp farming. Former works demonstrated that an accumulation of heavy metals is occurring in oysters in this estuary, and perhaps it could be explained by the input of metals in this ecosystem deriving from the shrimp farming. To better understanding the origin of these metals, bottom sediment samples, cores and suspended particulate matter were collected for a characterization of metal concentrations (Al, Ba, Cd, Cu, Cr, Fe, Mn, Ni, Pb, Zn) and to determine the potentially bioavailable metals. Additionally, the enrichment ratio for each element analyzed was calculated. The mineralogical composition of sediment samples and cores were obtained by X-ray diffraction. Moreover, data of orbital remote sensing were used in order to detect and quantify suspended matter by applying a logarithmic algorithm. Geochemical data of bottom sediments and cores revealed that, excepting Ba and Pb, the elements analyzed presented concentrations characteristic of an unpolluted ecosystem (Al: 0,25 - 8,76 %; Ba: 3,03 - 870 µg.g-1; Cd: < 0,25 µg.g-1; Cr: 1,72 - 82,4 µg.g-1; Cu: 0,12 -25,3 µg.g-1; Pb: 0,38 - 23,7 µg.g-1; Fe: 0,10 - 5,82 %; Mn: 15,1 - 815 µg.g-1; Ni: 0,14 - 36,1 µg.g-1; Zn: 1,37 - 113 µg.g-1). During the dry season a distribution pattern was observed, with higher metal concentrations in the margins, decreasing toward the central portion of the channel. These metal concentrations were well correlated with mineralogical compositions, with clay minerals prevailing at the margins, and quartz and feldspar in the center. However, this pattern was not observed during the wet season, probably because of the high water flux that disturbed bottom sediments. But, as observed for the dry season, a good correlation between metal concentrations and mineralogical composition was also observed for the wet season, with high metal concentrations where there were high quantities of clay minerals. Low enrichment ratios were obtained for the majority of elements analyzed, excepting for Mn, Ba and Pb. Manganese presented the higher ratios downstream for both seasons, and it can be an evidence of anthropogenic impact by shrimp farming. As barium and lead concentrations in sediment samples presented analytical problems during the total sample digestion, one cannot be sure that the ratios obtained correspond to the reality. The highest metal concentrations in particulate matter were obtained in the portion dominated by fluvial transport for all metals analyzed, excepting for copper. Barium and zinc were the only elements that presented elevated concentrations that are not common of unpolluted ecosystems (Ba: 5730 - 8355 µg.g-1; Zn: 3899 - 4348 µg.g-1). However, these high concentrations could not be related to the shrimp farming and waste waters from the town of Canguaretama, once they were obtained from the fluvial particulate matter, that is upstream from the activities above mentioned. The application of the logarithmic algorithm to the processed LANDSAT image was well succeeded, although the acquired image does not correspond exactly to the field campaigns. The IKONOS image provided very detailed views of the suspended sediment concentration at the estuary, as the mixture of distinct water flows at the confluence of Cunhaú and Curimataú rivers, with more turbid waters from Cunhaú river, that is directly affected by effluents from shrimp farming and urban waste waters deriving from the town of Canguaretama