Estudo da síntese e sinterização de pós compósitos do sistema Ta-Cu

Ta-Cu bulk composites combine high mechanical resistance of the Ta with high electrical and thermal conductivity of the Cu. These are important characteristics to electrical contacts, microwave absorber and heat skinks. However, the low wettability of Ta under Cu liquid and insolubility mutual these elements come hard sintering this composite. High-energy milling (HEM) produces composite powders with high homogeneity and refines the grain size. This work focus to study Ta-20wt%Cu composite powders prepared by mechanical mixture and HEM with two different conditions of milling in a planetary ball mill and then their sintering using hydrogen plasma furnace and a resistive vacuum furnace. After milling, the powders were pressed in a steel dye at a pressure of 200 MPa. The cylindrical samples pressed were sintered by resistive vacuum furnace at 10-4torr with a sintering temperature at 1100ºC / 60 minutes and with heat rate at 10ºC/min and were sintered by plasma furnace with sintering temperatures at 550, 660 and 800ºC without isotherm under hydrogen atmosphere with heat rate at 80ºC/min. The characterizations of the powders produced were analyzed by scanning electron microscopy (SEM), x-ray diffraction (XRD) and laser granulometry. After the sintering the samples were analyzed by SEM, XRD and density and mass loss tests. The results had shown that to high intense milling condition produced composite particles with shorter milling time and amorphization of both phases after 50 hours of milling. The composite particles can produce denser structure than mixed powders, if heated above the Cu melting point. After the Cu to arrive in the melting point, liquid copper leaves the composite particles and fills the pores

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

Nanopartíulas de magnetita com oxacilina obtida por moagem de alta energia para aplicações biomédicas

The drug targeting has been the subject of extensive studies in order to develop site-specific treatments that minimize side effects and become more effective anticancer therapy. Despite considerable interest in this class, drugs like antibiotics also have limitations, and have been neglected. Using new pharmaceutical technologies, the use of magnetic vectors appear as promising candidate for drug delivery systems in several studies. Small magnetic particles bound to the drug of interest can be modulated according to the orientation of a magnet outside the body, locating and holding in a specific site. In this work, we propose the use of High Energy Milling (HEM) for synthesis of a magnetic vector with characteristics suitable for biomedical applications by intravenous administration, and for the formation of an oxacillin-carrier complex to obtain a system for treating infections caused by Staphylococcus aureus. The results of the variation of milling time showed that the size and structural properties of the formed material change with increasing milling time, and in 60 hours we found the sample closest to the ideal conditions of the material. The vector-drug system was studied in terms of structural stability and antimicrobial activity after the milling process, which revealed the integrity of the oxacillin molecule and its bactericidal action on cultures of Staphylococcus aureus ATCC

Análise do efeito do tempo da moagem de alta energia no tamanho de cristalito e microdeformação da rede cristalina do WC-Co

Hard metals are the composite developed in 1923 by Karl Schröter, with wide application because high hardness, wear resistance and toughness. It is compound by a brittle phase WC and a ductile phase Co. Mechanical properties of hardmetals are strongly dependent on the microstructure of the WC Co, and additionally affected by the microstructure of WC powders before sintering. An important feature is that the toughness and the hardness increase simultaneously with the refining of WC. Therefore, development of nanostructured WC Co hardmetal has been extensively studied. There are many methods to manufacture WC-Co hard metals, including spraying conversion process, co-precipitation, displacement reaction process, mechanochemical synthesis and high energy ball milling. High energy ball milling is a simple and efficient way of manufacturing the fine powder with nanostructure. In this process, the continuous impacts on the powders promote pronounced changes and the brittle phase is refined until nanometric scale, bring into ductile matrix, and this ductile phase is deformed, re-welded and hardened. The goal of this work was investigate the effects of highenergy milling time in the micro structural changes in the WC-Co particulate composite, particularly in the refinement of the crystallite size and lattice strain. The starting powders were WC (average particle size D50 0.87 μm) supplied by Wolfram, Berglau-u. Hutten - GMBH and Co (average particle size D50 0.93 μm) supplied by H.C.Starck. Mixing 90% WC and 10% Co in planetary ball milling at 2, 10, 20, 50, 70, 100 and 150 hours, BPR 15:1, 400 rpm. The starting powders and the milled particulate composite samples were characterized by X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) to identify phases and morphology. The crystallite size and lattice strain were measured by Rietveld s method. This procedure allowed obtaining more precise information about the influence of each one in the microstructure. The results show that high energy milling is efficient manufacturing process of WC-Co composite, and the milling time have great influence in the microstructure of the final particles, crushing and dispersing the finely WC nanometric order in the Co particles

Structure study of Bi4Ti3O12 produced via mechanochemically assisted synthesis

Nanosized bismuth titanate was prepared via high-energy ball milling process through mechanically assisted synthesis directly from their oxide mixture of Bi2O3 and TiO2. Only Bi4Ti3O12 phase was formed after 3 h of milling time. The excess of 3 wt% Bi2O3 added in the initial mixture before milling does not improve significantly the formation of Bi4Ti3O12 phase comparing to stoichiometric mixture. The formed phase was amorphized independently of the milling time, The Rietveld analysis was adopted to determine the crystal structure symmetry, amount of amorphous phase, crystallite size and microstrains. With increasing the milling time from 3 to 12 h, the particle size of formed Bi4Ti3O12 did not reduced significantly. That was confirmed by SEM and TEM analysis. The particle size was less than 20 nm and show strong tendency to agglomeration. The electron diffraction pattern indicates that Bi4Ti3O12 crystalline powder is embedded in an amorphous phase of bismuth titanate. Phase composition and atom ratio in BIT ceramics were determined by X-ray diffraction and EDS analysis. (c) 2007 Elsevier Ltd. All rights reserved.

Bulk and high-energy ball-milled Gd5Si2Ge2: Comparative study of magnetic and magnetocaloric properties

High-energy ball milling was employed to produce small particles of Gd5Si2Ge2. Magnetic and magnetocaloric properties of the ball-milled and bulk Gd5Si2Ge2 samples were investigated through the magnetization measurements. When compared to the bulk material, a significant decrease in saturation magnetization and magnetocaloric effect (-Delta S-max = 4 vs. 20 J/kgK for Delta H = 0-5 T) is observed even after the relatively short ball milling time of 4 h which produced particles with an average size of ca. 0.5 mu m. The ball-milled samples appear to loose a first-order structural transition, present in bulk Gd5Si2Ge2, and display a superparamagnetic behaviour below the corresponding Curie temperatures. (C) 2010 Elsevier Masson SAS. All rights reserved.

Study of Structure and Properties of Bi4Ti3O12 Prepared by Mechanochemical Syntheses

Bi4Ti3O12 powder was synthesized from bismuth oxide and titanium oxide. Mixture of oxides was milled in zirconium oxide jar in the planetary ball-mill during 1, 3 and 6 h. Extended time of milling directed to formation of higher amount of titanates perovskite phase. Bi4Ti3O12 was formed between 1 and 3 h of milling time. The phase formation of Bi4Ti3O12, crystal structure and powder particle size were followed by XRD, Raman spectroscopy and SEM analysis. After milling for various times the powders were compacted by pressing and isothermal sintering. Sample milled for 3 h and subsequently sintered at 1000C for 24 h exhibit a hysteresis loop, confirming that the synthesized material possesses ferroelectric properties. All results affect that the structure Bi4Ti3O12 is strongly dependent on the milling time.

Mechanochemical synthesis of yttrium manganite

Yttrium manganite (YMnO3) is a multiferroic material, which means that it exhibits both ferromagnetic and ferroelectric properties, so making it interesting for a variety of technological applications. In this work, single-phase YMnO3 was prepared for the first time by mechanochemical synthesis in a planetary ball mill. The YMnO3 was formed directly from the highly activated constituent oxides, Y 2O3 and Mn2O3, after 60 min of milling time. During prolonged milling, the growth of the particles occurred. The cumulative energy introduced into the system during milling for 60 min was 86 kJ/g. The X-ray powder-diffraction analysis indicates that the as-prepared samples crystallize with an orthorhombic (Pnma) YMnO3 structure. The morphology and chemical composition of the powder were investigated by SEM and FESEM. The magnetic properties of the obtained YMnO3 powders were found to change as a function of the milling time in a manner consistent with the variation in the nanocomposite microstructure. © 2012 Elsevier B.V. All rights reserved.

Obtenção de materiais magnéticos para o estudo da propriedade magnetocalórica

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Properties of nanoparticles prepared from NdFeB-based compound for magnetic hyperthermia application

Nanoparticles were prepared from a NdFeB-based alloy using the hydrogen decrepitation process together with high-energy ball milling and tested as heating agent for magnetic hyperthermia. In the milling time range evaluated (up to 10 h), the magnetic moment per mass at H = 1.59 MA m(-1) is superior than 70 A m(2) kg(-1); however, the intrinsic coercivity might be inferior than 20 kA m(-1). The material presents both ferromagnetic and superparamagnetic particles constituted by a mixture of phases due to the incomplete disproportionation reaction of Nd2Fe14BHx during milling. Solutions prepared with deionized water and magnetic particles exposed to an AC magnetic field (H-max similar to 3.7 kA m(-1) and f = 228 kHz) exhibited 26 K <= Delta T-max <= 44 K with a maximum estimated specific absorption rate (SAR) of 225 W kg(-1). For the pure magnetic material milled for the longest period of time (10 h), the SAR was estimated as similar to 2500 W kg(-1). In vitro tests indicated that the powders have acceptable cytotoxicity over a wide range of concentration (0.1-100 mu g ml(-1)) due to the coating applied during milling.

Recycling of end of life concrete fines (0 - 4 mm) into silica and cement

The purpose of this work is to find a methodology in order to make possible the recycling of fines (0 - 4 mm) in the Construction and Demolition Waste (CDW) process. At the moment this fraction is a not desired by-product: it has high contaminant content, it has to be separated from the coarse fraction, because of its high water absorption which can affect the properties of the concrete. In fact, in some countries the use of fines recycled aggregates is highly restricted or even banned. This work is placed inside the European project C2CA (from Concrete to Cement and Clean Aggregates) and it has been held in the Faculty of Civil Engineering and Geosciences of the Technical University of Delft, in particular, in the laboratory of Resources And Recycling. This research proposes some procedures in order to close the loop of the entire recycling process. After the classification done by ADR (Advanced Dry Recovery) the two fractions "airknife" and "rotor" (that together constitute the fraction 0 - 4 mm) are inserted in a new machine that works at high temperatures. The temperatures analysed in this research are 600 °C and 750 °C, cause at that temperature it is supposed that the cement bounds become very weak. The final goal is "to clean" the coarse fraction (0,250 - 4 mm) from the cement still attached to the sand and try to concentrate the cement paste in the fraction 0 - 0,250 mm. This new set-up is able to dry the material in very few seconds, divide it into two fractions (the coarse one and the fine one) thanks to the air and increase the amount of fines (0 - 0,250 mm) promoting the attrition between the particles through a vibration device. The coarse fraction is then processed in a ball mill in order to improve the result and reach the final goal. Thanks to the high temperature it is possible to markedly reduce the milling time. The sand 0 - 2 mm, after being heated and milled is used to replace 100% of norm sand in mortar production. The results are very promising: the mortar made with recycled sand reaches an early strength, in fact the increment with respect to the mortar made with norm sand is 20% after three days and 7% after seven days. With this research it has been demonstrated that once the temperature is increased it is possible to obtain a clean coarse fraction (0,250 - 4 mm), free from cement paste that is concentrated in the fine fraction 0 - 0,250 mm. The milling time and the drying time can be largely reduced. The recycled sand shows better performance in terms of mechanical properties with respect to the natural one.

Magnetic disorder in TbAl2 nanoparticles

The magnetic and thermal properties of TbAl2 nanosized alloys (diameters, 12 nm $\leqslant D\leqslant $ 20 nm) obtained by high-energy milling are characterised by specific heat, magnetisation and neutron scattering. The specific heat shows that the λ-anomaly at Curie temperature vanishes when the milling time reaches 300 h and its field variation shows a broad peak around 70 K disclosing a disordered magnetic state. The thermal variation of magnetization follows a Bloch process with a decrease of the stiffness constant and a faster demagnetisation with a quadratic exponent instead of the bulk ordinary ${T}^{3/2}$-dependence. The magnetic moment reduction in the nanosized alloys follows a 1/D dependence, remarking the role of disordered moment surface. The Rietveld analysis of the neutron diffraction patterns indicates a collinear ferromagnetic structure, with a reduction of the Tb-magnetic moment when decreasing the particle size. The temperature dependent overall magnetic signal of nanoparticles is derived from small-angle neutron scattering. A magnetic nanoparticle structure with an ordered ferromagnetic core and a disordered surface layer is proposed.

Estudo da influência da adição de níquel em alumina pela rota da metalurgia do pó

Ceramic materials alumina basis have been widely used in structural components, mainly because owning properties such as high hardness, chemical inertness and good wear resistance, however, the low toughness is a factor that compromises its use in many other applications, featuring the addition of nickel as a possible solution to this problem, in this context, this work aims to study the addition of nickel alumina using the route of powder metallurgy processing of the material. The percentage of nickel were added 2, 4 and 6 wt%; and each composition to high energy milling in a planetary mill was performed for 2, 4, 9 and 16h. Subsequently, the samples were compacted at 300 MPa and sintered in a vacuum oven at 1400⁰C for 2h. The samples were characterized as the physical and mechanical properties, observing, in general, an improvement in sinterability of the material with increasing grinding time and nickel content, and mixing with a decrease of porosity and increase of hardness, density values above 80% of theoretical were obtained. The milling time of 4 hours and addition of 2% nickel, particularly if achieved higher hardness (HV 1068.7 +/- 32.6) and density of about 99% theoretical density.

Estudo da influência da adição de níquel em alumina pela rota da metalurgia do pó

Ceramic materials alumina basis have been widely used in structural components, mainly because owning properties such as high hardness, chemical inertness and good wear resistance, however, the low toughness is a factor that compromises its use in many other applications, featuring the addition of nickel as a possible solution to this problem, in this context, this work aims to study the addition of nickel alumina using the route of powder metallurgy processing of the material. The percentage of nickel were added 2, 4 and 6 wt%; and each composition to high energy milling in a planetary mill was performed for 2, 4, 9 and 16h. Subsequently, the samples were compacted at 300 MPa and sintered in a vacuum oven at 1400⁰C for 2h. The samples were characterized as the physical and mechanical properties, observing, in general, an improvement in sinterability of the material with increasing grinding time and nickel content, and mixing with a decrease of porosity and increase of hardness, density values above 80% of theoretical were obtained. The milling time of 4 hours and addition of 2% nickel, particularly if achieved higher hardness (HV 1068.7 +/- 32.6) and density of about 99% theoretical density.

Mechanochemical synthesis of TiO2/NiFe2O4 magnetic catalysts for operation under RF field

Composite NiFe2O4–TiO2 magnetic catalysts were prepared by mechanochemical synthesis from a mixture of titania supported nickel ferrite nanoparticles and P25 titania (Evonic). The former provides fast and efficient heating under radiofrequency field, while the latter serves as an active catalyst or catalyst support. The highest heating rate was observed over a catalyst prepared for a milling time of 30 min. The catalytic activity was measured over the sulfated composite catalysts in the condensation of aniline and 3-phenylbutyric acid in a stirred tank reactor and in a continuous RF heated flow reactor in the 140–170 °C range. The product yield of 47% was obtained over the sulfated P25 titania catalyst in the flow reactor.