Produção de estrutura com gradiente de porosidade a partir da sinterização por plasma da mistura de pós Ti-Nb-Sn

Porous structures are being widely investigated for use in biomedical implants, aiming to mechanically integrate and functionally the implant inside the bone tissue. Moreover, this structure is also important for drugs that can be stored and can induce and accelerate the process of osseointegration. With the purpose to investigate this effect, Ti, Nb and Sn metal powders, were sintered by plasma using a hollow cathode discharge. Sintering was performed in argon plasma set at 4 mbar pressure and temperatures of 500 ° C, 600 ° C and 700 ° C. Samples were also sintered in the electrical resistance furnace at 1200 ° C in order to compare plasma sintering with the conventional method. It was observed that plasma samples sintered with the hollow cathode configuration showed a gradient in porosity, while the samples sintered in the resistive furnace did not. Furthermore, differences in the microstructure of the samples were found, were a surface with higher porosity and ales porous core were obtained at different temperatures. The percolation profile of distilled water and the chemical compositions of the porous layers of the plasma treated samples were the main results obtained. Based on these results, we can conclude that this structure is particularly important for application in the biomedical field such as scaffolds for drug delivery and implants

Estudo de um compósito Nb-15%pCu obtidos por moagem de alta energia e sinterizados por fase líquida

There is great difficulty in forming a composite refractory metal niobium with copper. This is due to the fact that Nb-Cu system is almost mutually immiscible and may be neglected solubility between them. These properties hinder or prevent obtaining homogeneous and high-density structures, conventionally prepared. This study aims to analyze the use of high-energy milling process (MAE) to implement these natural difficulties, with regard to the densification of the sintered bodies. The MAE and the press were used in the preparation of powders, to obtain a fine and homogeneous distribution of the grain size. Four loads Nb and Cu powders containing 15% by weight of Cu were then milled for MAE in a planetary type ball mill under various milling times and speeds. The results obtained by MAE were analyzed by scanning electron microscopy (SEM), according to the parameters of time and grinding speed. The samples were compacted under pressure of 200 MPa, were then sintered in liquid phase in a vacuum furnace at temperatures of 1100 ° C / 60 min and 1200 ° C / 60 min. Then it was used to characterize diffraction of X-rays to identify the phases. The microstructures of the sintered samples were observed and evaluated using scanning electron microscopy (SEM). Vickers Microhardness tests were performed, obtaining higher values for the sintered bodies in the largest of the post milling times and the larger grinding speeds. It was found that the liquid phase sintering of the samples that were processed by MAE produced at the end of a homogeneous and densified structure in 77,4% relative to the value of the theoretical density of the composite

Efeito da moagem de alta energia na densificação e microestrutura do compósito AI2O3-Cu

The Cu-Al2O3 composite ceramic combines the phase of alumina, which is extremely hard and durable, yet very brittle, to metallic copper phase high ductility and high fracture toughness. These characteristics make this material a strong candidate for use as a cutting tool. Al2O3-Cu composite powders nanocrystalline and high homogeneity can be produced by high energy milling, as well as dense and better mechanical structures can be obtained by liquid phase sintering. This work investigates the effect of high-energy milling the dispersion phase Al2O3, Cu, and the influence of the content of Cu in the formation of Cu-Al2O3 composite particles. A planetary mill Pulverisatte 7 high energy was used to perform the experiments grinding. Al2O3 powder and Cu in the proportion of 5, 10 and 15% by weight of Cu were placed in a container for grinding with balls of hard metal and ethyl alcohol. A mass ratio of balls to powder of 1:5 was used. All powders were milled to 100 hours, and powder samples were collected after 2, 10, 20, 50 and 70 hours of grinding. Composite powders with compact cylindrical shape of 8 mm diameter were pressed and sintered in uniaxial matrix resistive furnace to 1200, 1300 to 1350 °C for 60 minutes under an atmosphere of argon and hydrogen. The heating rate used was 10°C/min. The powders and structures of the sintered bodies were characterized by XRD, SEM and EDS. Analysis TG, DSC and particle size were also used to characterize the milled powders, as well as dilatometry was used to observe the contraction of the sintered bodies. The density of the green and sintered bodies was measured using the geometric method (mass / volume). Vickers microhardness with a load of 500 g for 10 s were performed on sintered structures. The Cu-Al2O3 composite with 5% copper density reached 61% of theoretical density and a hardness of 129 HV when sintered at 1300 ° C for 1h. In contrast, lower densities (59 and 51% of the theoretical density) and hardness (110 HV and 105) were achieved when the copper content increases to 10 and 15%.

Determinação de CD, PB, e TL em água produzida por HR-CS GF AAS após extração em ponto nuvem

Produced water is a major problem associated with the crude oil extraction activity. The monitoring of the levels of metals in the waste is constant and requires the use of sensitive analytical techniques. However, the determination of trace elements can often require a pre-concentration step. The objective of this study was to develop a simple and rapid analytical method for the extraction and pre-concentration based on extraction phenomenon cloud point for the determination of Cd, Pb and Tl in produced water samples by spectrometry of high resolution Absorption source continues and atomization graphite furnace. The Box Behnken design was used to obtain the optimal condition of extraction of analytes. The factors were evaluated: concentration of complexing agent (o,o-dietilditilfosfato ammonium, DDTP), the concentration of hydrochloric acid and concentration of surfactant (Triton X -114). The optimal condition obtained through extraction was: 0,6% m v-1 DDTP, HCl 0,3 mol L-1 and 0,2% m v-1 of Triton X - 114 for Pb; 0,7% m v-1 DDTP, HCl 0,8 mol L-1 and 0,2% m v-1 Triton X-114 for Cd. For Tl was evidenced that best extraction condition occurs with no DDTP, the extraction conditions were HCl 1,0 mol L-1 e 1,0% m v-1 de Triton X - 114. The limits of detection for the proposed method were 0,005 µg L-1 , 0,03 µg L-1 and 0,09 µg L-1 to Cd, Pb and Tl, Respectively. Enrichment factors Were greater than 10 times. The method was applied to the water produced in the Potiguar basin, and addition and recovery tests were performed, and values were between 81% and 120%. The precision was expressed with relative standard deviation (RSD) is less than 5%

Desenvolvimento de metodologia de extração e pré-concentração utilizando sistema microemulsionado para determinação de Cd, Co, Cu, Ni, Pb e Tl em águas naturais e produzidas por HR-CS AAS

The determination and monitoring of metallic contaminants in water is a task that must be continuous, leading to the importance of the development, modification and optimization of analytical methodologies capab le of determining the various metal contaminants in natural environments, because, in many cases, the ava ilable instrumentation does not provide enough sensibility for the determination of trace values . In this study, a method of extraction and pre- concentration using a microemulsion system with in the Winsor II equilibrium was tested and optimized for the determination of Co, Cd, P b, Tl, Cu and Ni through the technique of high- resolution atomic absorption spectrometry using a continuum source (HR-CS AAS). The optimization of the temperature program for the graphite furnace (HR-CS AAS GF) was performed through the pyrolysis and atomization curves for the analytes Cd, Pb, Co and Tl with and without the use of different chemical modifiers. Cu and Ni we re analyzed by flame atomization (HR-CS F AAS) after pre-concentr ation, having the sample introduction system optimized for the realization of discrete sampling. Salinity and pH levels were also analyzed as influencing factors in the efficiency of the extraction. As final numbers, 6 g L -1 of Na (as NaCl) and 1% of HNO 3 (v/v) were defined. For the determination of the optimum extraction point, a centroid-simplex statistical plan was a pplied, having chosen as the optimum points of extraction for all of the analytes, the follo wing proportions: 70% aqueous phase, 10% oil phase and 20% co-surfactant/surfactant (C/S = 4). After extraction, the metals were determined and the merit figures obtained for the proposed method were: LOD 0,09, 0,01, 0,06, 0,05, 0,6 and 1,5 μg L -1 for Pb, Cd, Tl, Co, Cu and Ni, re spectively. Line ar ranges of ,1- 2,0 μg L -1 for Pb, 0,01-2,0 μg L -1 for Cd, 1,0 - 20 μg L -1 for Tl, 0,1-5,0 μg L -1 for Co, 2-200 μg L -1 and for Cu e Ni 5-200 μg L -1 were obtained. The enrichment factors obtained ranged between 6 and 19. Recovery testing with the certified sample show ed recovery values (n = 3, certified values) after extraction of 105 and 101, 100 and 104% for Pb, Cd, Cu and Ni respectively. Samples of sweet waters of lake Jiqui, saline water from Potengi river and water produced from the oil industry (PETROBRAS) were spiked and the recovery (n = 3) for the analytes were between 80 and 112% confirming th at the proposed method can be used in the extraction. The proposed method enabled the sepa ration of metals from complex matrices, and with good pre-concentration factor, consistent with the MPV (allowed limits) compared to CONAMA Resolution No. 357/2005 which regulat es the quality of fresh surface water, brackish and saline water in Brazil.

Fabricação e estudo de um forno solar com dispositivo de transporte

It presents a solar oven manufactured from MDF boards intended for the baking of foods such as pizza, cakes, breads, hamburgers and the like. They will be given the manufacturing processes and assembly of such an oven which has features of low cost manufacturing. The main feature of the proposed furnace and can be transported to any locations because it is seated on a device for carrying case / backpack. Tests will be conducted for the baking of various foods and their results will be compared with the various types of existing solar ovens shown by the literature. They will analyze the thermal and economic feasibility of such an oven that can provide socialization of the use of solar energy for poor communities and can become a source of generation of employment and income. The proposed solar oven baking has capacity for two foods and can be manufactured to allow multiple simultaneous baking of food.

Efeito da adição de WC e Co na sinterização e propriedades mecânicas da alumina

Composites based on alumina (Al2O3), tungsten carbide (WC) and cobalt (Co) exhibit specific properties such as low density, high oxidation resistance, high melting point and high chemical inertia. That composite shows to be a promising material for application in various fields of engineering. In this work, the mechanical properties of the composite (Al2O3 – WC – Co), particularly density and hardness, were evaluated according to the effects of the variables of powder processing parameters, green compact and sintered. Powder composites with the composition of 80 wt% Al2O3, 18 wt% WC and 2 wt% Co were processed by high energy ball milling in a planetary mill for 50 hours as well as mixed by manual mixing in a glass vessel with the same proportion. Samples were collected (2, 10, 20, 30, 40 and 50 hours) during the milling process. Then, the powders were compacted in a cylindrical die with 5 mm in diameter in a uniaxial press with pressures of 200 and 400 MPa. The sintering was in two stages: first, the solid phase sintering was performed at 1126 and 1300 °C for 1 hour with a heating rate of 10 °C/min in a resistive furnace under argon atmosphere for green samples compacted in 200 and 400 MPa; the second sintering was performed on dilatometer in solid phase at 1300 °C for green sample compacted in 200 MPa, another sintering also was performed on dilatometer, this time in liquid phase at 1550 °C for green samples compacted in 200 and 400 MPa, with the same parameters used in resistive furnace. The raw materials were characterized by X – ray diffraction (XRD), X – ray fluorescence (XRF), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and laser particlemeter. The sintered samples were subjected to microhardness testing. The results showed that high energy milling achieved to the objectives regarding the particle size and the dispersion of composite phases. However, the hardness did not achieve to significant results, this is an indication that the composite has low fracture toughness.

Efeito da adição de WC e Co na sinterização e propriedades mecânicas da alumina

Composites based on alumina (Al2O3), tungsten carbide (WC) and cobalt (Co) exhibit specific properties such as low density, high oxidation resistance, high melting point and high chemical inertia. That composite shows to be a promising material for application in various fields of engineering. In this work, the mechanical properties of the composite (Al2O3 – WC – Co), particularly density and hardness, were evaluated according to the effects of the variables of powder processing parameters, green compact and sintered. Powder composites with the composition of 80 wt% Al2O3, 18 wt% WC and 2 wt% Co were processed by high energy ball milling in a planetary mill for 50 hours as well as mixed by manual mixing in a glass vessel with the same proportion. Samples were collected (2, 10, 20, 30, 40 and 50 hours) during the milling process. Then, the powders were compacted in a cylindrical die with 5 mm in diameter in a uniaxial press with pressures of 200 and 400 MPa. The sintering was in two stages: first, the solid phase sintering was performed at 1126 and 1300 °C for 1 hour with a heating rate of 10 °C/min in a resistive furnace under argon atmosphere for green samples compacted in 200 and 400 MPa; the second sintering was performed on dilatometer in solid phase at 1300 °C for green sample compacted in 200 MPa, another sintering also was performed on dilatometer, this time in liquid phase at 1550 °C for green samples compacted in 200 and 400 MPa, with the same parameters used in resistive furnace. The raw materials were characterized by X – ray diffraction (XRD), X – ray fluorescence (XRF), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and laser particlemeter. The sintered samples were subjected to microhardness testing. The results showed that high energy milling achieved to the objectives regarding the particle size and the dispersion of composite phases. However, the hardness did not achieve to significant results, this is an indication that the composite has low fracture toughness.

Estudo da incorporação de cinza e chamote gerado pela cerâmica vermelha ao próprio processo industrial

The ceramics industry generates waste at various stages of that process, defective products, waste from burning solid fuels, among others. This waste is dumped in landfills, garbage dumps or directly on roads, which has a negative environmental impact. This paper presents a study to incorporate the waste of algaroba wood and chamote (scrap pieces of ceramic already sintered), in to the ceramic material for making sealing blocks. The methodological procedures consist in the characterization of chemical and mineralogical residues, raw materials, and physical-mechanical of the formulations of mixes with clay, silt and waste. By pressing test pieces were produced using a pressure of 200 kgf/cm², varying compositions in the range of 0%, 5%, 10% and 15% by weight of residue. The sintering was performed in a muffle furnace, with the temperature levels of 850 ° C, 900 ° C, 950 ° C, 1000 ° C and 1050 ° C. The evaluated physical and mechanical properties were: Water Absorption, Linear Shrinkage Burning, Apparent Porosity, Apparent Density and Mechanical Resistance to Flexion. Analysis was carried out by Scanning Electron Microscopy on fracture surfaces of the specimens. Evaluation of linear shrinkage property drying and firing , water absorption and mechanical resistance to compression of the sealing blocks 5% wood ash residue, sintered at 900 °C hold temperature in the laboratory the products manufactured on an industrial scale. The main results, it was found on the viability of using the residues of algaroba wood and to confer refractory properties of the ceramic product. The main results, it was concluded feasibility of using the ash residues algaroba wood to impart refractory properties to the ceramic product and the residue of chamote, being derived from the own ceramic product not interfere with the properties, when used in a percentage of up to 5%.Since the residue of chamote being derived from the ceramic product itself had no effect on the properties. Studies in the laboratory have shown that the incorporation of up to 5% of these residues may be adopted as an alternative technology to reduce the environmental impact caused by the industrial sector, without compromising the final properties of the material, since the results on an industrial scale showed absorption values 11.66 and 11.74 of water and waste products respectively, within the parameters of NBR - 15,270, since the mechanical strength was 1.25 MPa and 0.94 MPa respectively for products with and without residue, lower than the minimum required by the technical standard that is 1.5 MPa.

Estudo da incorporação de cinza e chamote gerado pela cerâmica vermelha ao próprio processo industrial

The ceramics industry generates waste at various stages of that process, defective products, waste from burning solid fuels, among others. This waste is dumped in landfills, garbage dumps or directly on roads, which has a negative environmental impact. This paper presents a study to incorporate the waste of algaroba wood and chamote (scrap pieces of ceramic already sintered), in to the ceramic material for making sealing blocks. The methodological procedures consist in the characterization of chemical and mineralogical residues, raw materials, and physical-mechanical of the formulations of mixes with clay, silt and waste. By pressing test pieces were produced using a pressure of 200 kgf/cm², varying compositions in the range of 0%, 5%, 10% and 15% by weight of residue. The sintering was performed in a muffle furnace, with the temperature levels of 850 ° C, 900 ° C, 950 ° C, 1000 ° C and 1050 ° C. The evaluated physical and mechanical properties were: Water Absorption, Linear Shrinkage Burning, Apparent Porosity, Apparent Density and Mechanical Resistance to Flexion. Analysis was carried out by Scanning Electron Microscopy on fracture surfaces of the specimens. Evaluation of linear shrinkage property drying and firing , water absorption and mechanical resistance to compression of the sealing blocks 5% wood ash residue, sintered at 900 °C hold temperature in the laboratory the products manufactured on an industrial scale. The main results, it was found on the viability of using the residues of algaroba wood and to confer refractory properties of the ceramic product. The main results, it was concluded feasibility of using the ash residues algaroba wood to impart refractory properties to the ceramic product and the residue of chamote, being derived from the own ceramic product not interfere with the properties, when used in a percentage of up to 5%.Since the residue of chamote being derived from the ceramic product itself had no effect on the properties. Studies in the laboratory have shown that the incorporation of up to 5% of these residues may be adopted as an alternative technology to reduce the environmental impact caused by the industrial sector, without compromising the final properties of the material, since the results on an industrial scale showed absorption values 11.66 and 11.74 of water and waste products respectively, within the parameters of NBR - 15,270, since the mechanical strength was 1.25 MPa and 0.94 MPa respectively for products with and without residue, lower than the minimum required by the technical standard that is 1.5 MPa.

Dissolved Zinc in the Southern Ocean measured on water bottle samples during POLARSTERN cruise ANT-XXIV/3

The distribution of dissolved zinc (Zn) was investigated in the Atlantic sector of the Southern Ocean in the austral autumn of 2008 as part of the IPY GEOTRACES expedition ZERO & DRAKE. Research focused on transects across the major frontal systems along the Zero Meridian and across the Drake Passage. There was a strong gradient in surface zinc concentrations observed across the Antarctic Polar Front along both transects and high zinc levels were found in surface waters throughout the Southern Ocean. Vertical profiles for dissolved Zinc showed the presence of local minima and maxima in the upper 200 m consistent with significant uptake by phytoplankton and release by zooplankton grazing, respectively. Highest deep water zinc concentrations were found in the centre of the Weddell Gyre associated with Central Intermediate Water (CIW), a water mass which is depleted in O2, elevated in CO2 and is regionally a CFC minimum. Our data suggests that the remineralization of sinking particles is a key control on the distribution of Zn in the Southern Ocean. Disappearance ratios of zinc to phosphate (Zn:P) in the upper water column increased southwards along both transects and based on laboratory studies they suggest slower growth rates of phytoplankton due to iron or light limitation. Zinc and silicate were strongly correlated throughout the study region but the disappearance ratio (Zn:Si) was relatively uniform overall except for the region close to the ice edge on the Zero Meridian.

Beryllium isotopes of sediments from the Portuguese margin

A high resolution study of authigenic Be isotopes (10Be and 9Be) combined with continuous relative paleointensity records has been performed along the same marine sedimentary sequences from the Portuguese margin (NE Atlantic) covering the past 300 kyr in order to assess relationships between geomagnetic moment variations and 10Be production rate variations. A careful examination of the various ways of taking into account environmental disturbing effects on the authigenic 10Be concentration leads to the conclusion that the most reliable proxy of cosmonuclide production rates is presently the authigenic 10Be/9Be ratio. Eight intervals of significant authigenic 10Be/9Be enhancement evidence geomagnetic moment drops related to global paleomagnetic excursions, some being already admitted, others being proposed as new geomagnetic features. Since, unlike sedimentary magnetic remanence, the authigenic 10Be/9Be records dipole moment variations without significant acquisition delay, it provides better constraints on their timing. Comparison of 10Be/9Be and benthic delta18O records from the same cores suggests that dipole moment lows preferentially occurred during or at the end of interglacial episodes, with a quasi-period of 100 kyr.

Paleomagnetic and beryllium isotope record of West Equatorial Pacific sediments

The reliability of paleomagnetic records as proxies of the geomagnetic field intensity is still a matter of controversy since volcanic materials hardly provide continuous records, and marine sediments are suspected to carry a remanence biased by post-depositional realignments and/or by overprints. Such long standing debate emphasizes the need for the development of methods independent from paleomagnetism to decipher geomagnetic intensity variations. High resolution measurements of authigenic 10Be/9Be along with a detailed sedimentary record of directional and relative paleointensity variations evidence, over the 0.6-1.3 Ma time interval, frequent and recurrent excursions or short events in the late Matuyama and the early Brunhes epochs, among which two Brunhes-Matuyama reversal precursors and an intra-Jaramillo excursion. The results of this study confirm the idea of a highly unstable geomagnetic field as suggested by paleomagnetic evidences.

(Table 2) Concentration of heavy metals and organic carbon, and 210Pb activity of sediments near Büsum, eastern Wadden Sea

A 3.38 m long sediment core raised from the tidal flat sediments of the 'Blauortsand' in the Wadden Sea northwest of Büsum (Schleswig-Holstein, Germany) was analysed in order to investigate long term changes in sediment pollution with Pb, Cu, Zn and Cd. Comparison with the topographic maps since 1952 and 210Pb activity allowed a general dating of the sediment succession in the core. The heavy metal concentrations including 210Pb of the < 20 µm grain-size fraction in thick sediment slices below 1.30 m indicated background niveaus. Their values increased and reached modern levels in the upper sediment layers of the core above 1 m. The increments for Pb, Cu, Zn was 1 to 3 fold and Cd up to 11 fold since the second half of the 19th century. More investigations are needed to quantify the geographical extent and history of the contaminations shown in this pilot study.