Resumo em Inglês:

This study presents the results of microstructural examinations, mechanical tests and service performance tests carried out on thin TiN/(Ti,Al,Si)N/TiN wear resistance coatings obtained by the CAE process on cermet and cemented carbide substrates. Microstructural examinations of the applied coatings and the substrate were made with an OPTON DSM 940 SEM and a LEICA MEF4A light microscope. Adhesion of the coatings on cemented carbides and cermets was measured using the scratch test. The cutting properties of the materials were determined from service tests in which continuous machining of C45E steel was carried out. The hardness of the substrate and the microhardness of the coatings were determined with a DUH 202 SHIMADZU ultra microhardness tester with a load of 70 mN. Roughness tests were also carried out before applying the coatings and after the PVD process. Cutting tests confirmed the advantages of the TiN/(Ti,Al,Si)N/TiN type coatings obtained using the PVD method in the CAE mode on cemented carbides and cermets, as a material that undergoes very low abrasive, thermal and adhesion wear. These coatings extend tool life compared to commercially available uncoated tools with single and multi-layer coatings deposited using PVD/CVD methods.

Resumo em Inglês:

The purpose of this investigation was to compare catalysts produced by the Bönnemann - colloidal method (PtRu (B1) and PtRu (B2)), and those produced by the spontaneous deposition method (PtRu (SD)). The catalysts produced by both methods had good electrochemical behavior for methanol oxidation for proton exchange membrane fuel cell applications. The structure of the catalyst was examined by transmission electron microscopy (TEM). Energy dispersive spectroscopic analysis (EDS) was used to determine the semi-quantitative composition of the catalysts, and the electrochemical behavior was determined by cyclic voltammetry (CV). The diffractograms of the binary catalysts revealed platinum and ruthenium as the only crystalline phases, as per ICDD data base. The PtRu (B1) catalyst, treated in a reducing atmosphere, has the same structure as PtRu (B2), treated in an oxidising/reducing atmosphere, except that the crystallite size was around 1.7 nm for PtRu (B1) instead of 9.9 nm for PtRu (B2). The catalysts PtRu (B2) and PtRu (SD) showed similar cyclic voltammetric behavior, which was better than that of PtRu (B1). Both methods are suitable for the production of electrocatalysts for fuel cell applications. The colloidal method is more expensive than the deposition method, but the former permits the production of ternary and quaternary catalyst systems with enhanced CO tolerance.

Resumo em Inglês:

Many methods are currently used to measure the fracture toughness of ceramic materials. Methods based on crack-length measurements of cracks introduced into the sample surface by the Vicker's indentor have the advantage that they are easy to use, but are very unreliable due to subcritical crack growth and the difficulty in determining the exact length of the cracks. Furthermore, depending on the crack shape there are many equations to calculate K Ic. Other methods like the Chevron Notch or Single Edge Pre-cracked Beam (SEPB) are often difficult to execute or expensive. The simple and inexpensive Single-Edge-V-Notched Beam (SEVNB) on the other hand gives reliable values of fracture toughness of ceramic materials. In this method a saw cut is tapered to a sharp V-notch using a razor blade sprinkled with diamond paste. Thus, it is possible to introduce a sharp crack with a notch width of less than 20 micrometers, necessary to conduct valid tests. In this investigation, fracture toughness measurements on LPS-SiC materials carried out by the indentation technique and the SEVNB method have been compared.

Resumo em Inglês:

An apparatus to conduct high temperature erosion-oxidation studies up to 850 °C and with particle impact velocities up to 15 m.s-1 was designed and constructed in the Corrosion Laboratories of IPEN. The erosion-oxidation behavior of high velocity oxy fuel (HVOF) sprayed alloy and cermet coatings of Ni20Cr, WC 20Cr7Ni and Cr3C2 Ni20Cr on a steel substrate has been studied. Details of this apparatus and the erosion-oxidation behavior of these coatings are presented and discussed. The erosion-oxidation behavior of HVOF coated Cr3C2 25(Ni20Cr) was better than that of WC 20Cr7Ni, and the erosion-oxidation regimes have been identified for these coatings at particle impact velocity of 3.5 m.s-1, impact angle of 90° and temperatures in the range 500 to 850 °C.

Resumo em Inglês:

Computer simulation of the hard phase of WC-based hard metals is not common in scientific literature. This phase is formed by carbide grains embedded in a metallic matrix. In the equilibrium state, the grain has an equilateral prismatic form with beveled edges. It is nevertheless possible to model stereological aspects of this phase, using a Monte Carlo simulation assuming a prism structure without beveled edges. From the grain's height to width ratio, physical parameters such as grain area and intercept lengths can be calculated. The goal of this work is to present a simple method to obtain this ratio for metallographic samples. One of the results is to establish a relationship between the intercept length and the true size of the grain, which facilitates better understanding of this material's structure.

Resumo em Inglês:

Durability of surfaces has been reported as the main factor affecting tribological behavior of steam oxidised sintered iron. The presence of surface pores and their negative influence on load bearing capacity, suggest that surface topography might play an important role on the durability of the oxide layer. In this paper, the influence of compaction pressure and powder grade on surface topography, and as a consequence, its effect on the tribological behavior of steam oxidised sintered iron has been analysed. Specimens prepared from atomised iron powders with different sizes were compacted using 4 different pressures, sintered, and then subjected to steam treatment. Tribological characterisation was carried out in a reciprocating sliding wear test. Although the processing parameters affected the surface topography to a considerable extent, the main influence may be attributed to powder grade. A strong influence of surface topography on the durability distance, evaluated in terms of the evolution of contact resistance with total sliding distance, has been highlighted. Surfaces which were smoother and had high load-carrying capacity were always associated with a higher durability distance.

Resumo em Inglês:

Sintered Pr-based magnets were produced using a new laboratory technique for powder handling. Unlike the conventional procedure for preparing sintered permanent magnets in the laboratory, the powder technique used in this investigation does not require a glove box. The effects of processing parameters on the magnetic properties of Pr-based sintered magnets prepared using the hydrogen decrepitation process have been studied. Specifically, the effects of sintering temperature and milling time for processing Pr16Fe76B8 magnets have been investigated. Pr16Fe76B8 magnets with the best magnetic properties were sintered between 1015 °C to 1075 °C.

Resumo em Inglês:

Nd-Fe-B magnets are highly susceptible to corrosion and need protection against environment attack. The use of organic coatings is one of the main methods of corrosion protection of these materials. Data related to the effect of conversion coatings, such as phosphating, on corrosion performance of these magnets is still scarce. Studies about the effect of phosphating on the corrosion resistance of a commercial Nd-Fe-B sintered magnet indicated that it increases the corrosion resistance of these magnets, compared to non-phosphated magnets. In this study, the solution chemistry of a phosphating bath was altered with the addition of molybdate and its effect on the corrosion resistance of magnets investigated. Sintered magnet specimens were phosphated in solutions of 10 g/L NaH2PO4 (pH 3.8), either with or without molybdate [10-3 M MoO4(2-)], to improve their corrosion resistance. The effect of phosphating time was also evaluated, and specimens were phosphated for 4 and 18 hours. To evaluate the corrosion performance of phosphated and unphosphated specimens, a corrosion test based on monitoring hydrogen evolution on the surface of the magnets was used. This technique revealed that the addition of molybdate to the phosphating solution improved the corrosion resistance of the magnets phosphated by immersion for short periods but had no beneficial effect if phosphated by immersion for longer periods.

Resumo em Inglês:

The electrocatalytic properties of steel-FeNbC composites were evaluated after potentiostatic ageing with the purpose of establishing the potential use of such materials as electrodes for the industrial production of oxygen. The effect of processing parameters, involved in the production of the composites by powder metallurgy, such as milling conditions and compaction pressure, on the performance of the electrodes was also studied. The electrodes were characterized according to their electrical resistance in NaOH 1M solution, considering that the purpose of the application requires this value to be ~ 0.5 omega.cm². This parameter was evaluated from repetitive electrochemical measurements carried out from 0.7 V to 1.5 V (vs. Ag/AgCl) by electrode anodization. Changes in the electrochemical behavior of the electrodes, especially concerning the O2 evolution in alkaline medium, were studied as a function of the applied potential. The results revealed that the electrocatalytic activity of the electrodes increased upon ageing, probably as a consequence of the growth of oxide layers and/or increase in the conductivity of the material, resulting in current gain and corresponding decrease in the polarization resistance to 0.75 omega cm².

Resumo em Inglês:

In this investigation the corrosion resistance of four Al-Si hypereutectic alloys in a solution typical of condensate from automotive fuel combustion products, and referred to here as synthetic condensed automotive solution, has been studied. Three commercial alloys that are used for cylinder liners, and a laboratory made alloy, were studied by electrochemical impedance spectroscopy and measurements were taken after increasing times of immersion in this solution. Comparison of the electrochemical response of the four alloys in the corrosive solution was carried out. Although the mechanisms by which the four alloys corroded were similar, the results indicated differences in corrosion resistances of these alloys, and these differences could be related to their microstructures. The laboratory prepared alloy showed increased susceptibility to pitting corrosion compared to the commercial alloys. The surfaces of the alloys were examined, before and after the corrosion test, by scanning electron microscopy and analyzed by energy dispersive spectroscopy. The results indicated preferential attack of the aluminium matrix phase in all the alloys. The alloy with higher copper content and prepared by spray forming was more susceptible to pitting compared to the other alloys. The EIS response at low frequencies indicated a diffusion-controlled process, probably that of oxygen to the alloy interface.

Resumo em Inglês:

The effect of heat treatment on crystallization behavior of Fe73.5B15Si10Nb1.5 alloy powder prepared by mechanical alloying was studied. The powder samples were prepared by mechanical alloying (MA) and for different milling times (1, 5, 25, 70 and 100 hours). Crystalline powders of iron, boron, silicon and niobium were sealed with tungsten carbide balls in a cylindrical vial under nitrogen atmosphere. The ball-to-powder weight ratio was 20 to 1. A Fritsch Pulverizette 5 planetary ball mill was used for MA the powders at room temperature and at 250 rpm. To study the microstructural evolution, a small amount of powder was collected after different milling times and examined by X-ray diffraction, using CuKalpha radiation (lambda = 0.15418 nm). The crystallization behavior was studied by differential thermal analysis, from 25 up to 1000 °C at a heating rate of 25 °C min-1.

Resumo em Inglês:

In this investigation, the corrosion resistance of AISI 316 SS filters prepared with powders in the size ranges 74-44 µm and 210-105 µm and compacted with pressures of 300 MPa and 400 MPa has been evaluated in naturally aerated 0.5 M H2SO4 solution at 25 °C. Weight loss of filters manufactured with compacting pressure of 400 MPa were significantly higher than that of filters compacted at 300 MPa. The filter compacted at 400 MPa had higher carbon and nitrogen contents compared to those compacted at 300 MPa. The former also had chromium rich precipitates and oxides in the grain boundaries. The pores in filters compacted at 400 MPa were smaller than in filters compacted at 300 MPa. Smaller pores favor the formation of concentration cells and consequently, increased crevice corrosion.

Resumo em Inglês:

The technical viability of preparing a Cu-Al-Nb shape memory alloy by high energy ball milling in a planetary mill has been evaluated. The alloy Cu-13Al-2Nb (wt. (%)) was prepared by mixing pure elemental powders. A ball-to-powder weight ratio of 6:1 and rotation rate of 150 rpm in argon atmosphere were the main processing parameters. The milling time ranged from 1 to 65 hours. Changes in microstructure as a function of milling time were investigated, using X-ray diffraction analysis and scanning electron microscopy. To investigate the viability of producing sintered parts from milled powders, the conventional powder metallurgy route was used. The milled powders were compacted in a cylindrical die at 900 MPa. Sintering was carried out in argon atmosphere at 850 °C for 6 hours. This study has shown that high energy ball milling, combined with pressing and sintering, can be used to promote the formation of a copper-aluminum solid solution and achieve final sintered densities of 91% of the theoretical density.

Resumo em Inglês:

Powder Metallurgy has been reported as a suitable alternate processing route for the manufacture of tool steels. The advantage of this technique is in being able to obtain a refined and more uniform microstructure that improves properties such high wear resistance and toughness. A molybdenum containing AISI M3:2 tool steel, (trade name Sinter 23), manufactured from spherical gas-atomized powders by hot isostatic pressing followed by hot working was tested in three-point bending tests after various heat treatments. Transverse rupture strength (TRS) samples were cut and heat treated at four distinct austenitizing temperatures. Each austenitizing temperature was combined with three tempering temperatures, giving a total of twelve different hardening conditions. Hardness tests were carried out to establish correlations among the effectiveness of heat treatment, the hardness values and the TRS results. At least five parallel samples were tested in each heat treatment condition.

Resumo em Inglês:

Experimental results on the performance of a laboratory scale rectangular Venturi scrubber in the removal of fine mineral particles from a confined air stream are presented, and a new correlation is proposed and evaluated. The scrubber was operated with air velocities in the throat varying from 58 m/s to 75 m/s and liquid flow rates varying from 280 ml/min to 900 ml/min. Liquid was injected as a jet emerging from a 1.0 mm orifice at the throat. Results for dust collection grade efficiency varied from 87% to 98% for particles from 0.1 µm to 2.0 µm.

Resumo em Inglês:

Aluminium-silicon alloys have been wide accepted in the automotive, electric and aerospace industries. Preferred orientation is a very common condition for metals and alloys. Particularly, aluminium induces texture during the forming process. The preparation of an aggregate with completely random crystal orientation is a difficult task. The present work was undertaken to analyse the texture by X-ray diffraction techniques, of three spray formed hypereutectic Al-Si alloys. Samples were taken from a billet of an experimental alloy (alloy 1) and were subsequently hot-rolled and cold-rolled (height reduction), 72% and 70%, respectively. The other used samples, alloys 2 and 3, were taken from cylinders liners. The results from the Laue camera showed texture just in the axial direction of alloy 3. The pole figures also indicated the presence of a typical low intensity deformation texture, especially for alloy 3. The spray formed microstructure, which is very fine, hinders the Al-Si texture formation during mechanical work.

Resumo em Inglês:

The rheological behavior of alumina molding feedstocks containing polyethylene glycol (PEG), polyvinylbutyral (PVB) and stearic acid (SA) and having different powder loads were analyzed using a capillary rheometer. Some of the feedstocks showed a pseudoplastic behavior of n < 0, which can lead to the appearance of weld lines on molded parts. Their viscosity also displayed a strong dependence on the shear rate. The slip phenomenon, which can cause an unsteady front flow, was also observed. The results indicate that the feedstock containing a lower powder load displayed the best rheological behavior. The 55 vol. % powder loaded feedstock presented the best rheological behavior, thus appearing to be more suitable than the formulation containing a vol. 59% powder load, which attained viscosities exceeding 10³ Pa.s at low shear rates, indicating its unsuitability for injection molding.

Resumo em Inglês:

Research in the preparation of ceramics from polymeric precursors is giving rise to increased interest in ceramic technology because it allows the use of several promising polymer forming techniques. In this work ceramic composite pieces were obtained by pyrolysis of a compacted mixture of a polysiloxane resin and alumina/silicon powder. The mixture consists of 60 vol% of the polymer phase and 40 vol% of the filler in a 1:1 ratio for alumina/silicon, which was hot pressed to crosslink the polymer, thus forming a compact body. This green body was trimmed into different geometries and pyrolised in nitrogen atmosphere at temperatures up to 1600 °C. X-ray diffraction analysis indicated the formation of phases such as mullite and Si2ON2 during pyrolysis, that result from reactions between fillers, polymer decomposition products and nitrogen atmosphere. The porosity was found to be less than 20% and the mass loss around 10%. The complex geometry was maintained after pyrolysis and shrinkage was approximately 8%, proving pyrolisis to be a suitable process to form near-net-shaped bulk ceramic components.

Resumo em Inglês:

In ceramic wall tile processing, fast single-firing cycles have been widely used. In this investigation a fast single-firing porous wall tile mixture was prepared using raw materials from the North Fluminense region.Specimens were obtained by uniaxial pressing and sintered in air at various temperatures (1080 - 1200 °C) using a fast-firing cycle (60 minutes). Evolution of the microstructure was followed by XRD and SEM. The results revealed that the main phases formed during the sintering step are anorthite, gehlenite and hematite. It appears that the sintering process is characterized by the presence of a small amount of a liquid phase below 1140 °C. As a result, the microstructure of the ceramic bodies showed a network of small dense zones interconnected with a porous phase. In addition, the strength of the material below 1140 °C appeared to be related to the type and quantity of crystalline phases in the sintered bodies.

Resumo em Inglês:

Silicon carbide is an important structural ceramic and finds applications as abrasives, as a refractory and in automotive engine components. This material can attain high densities during liquid phase sintering if suitable additives are used. Silicon carbides containing silica, alumina and rare earth oxides have suitable characteristics to promote liquid phase sintering. In this paper, the sintering behavior of silicon carbide ceramics with additives based on the (SiO2-RE2O3-Al2O3) system (RE = Y, Dy) has been studied. Samples with different compositions and containing 90 vol.% SiC were sintered in a dilatometer at 1950 °C/1h and in a graphite resistance furnace from 1500 °C/1h up to 1950 °C/1h. The shrinkage behavior as a function of rare earth oxide used and additive composition was also studied. The sintered materials were characterized by density and weight loss measurements. The crystalline phases were identified by X-ray diffraction analysis. The sintering kinetics of these materials can be related to the formation of secondary crystalline phases.

Resumo em Inglês:

Commercial purity titanium (cp-Ti), and some of its alloys are important materials in the medical field because of their excellent biocompatibility and mechanical properties. Recently a simple chemical method to induce bioactivity in these inert metallic materials was reported. In this work, the biomimetic chemical process has been used to modify the surface of cp-Ti with the formation of a deposit layer of apatite (a calcium phosphate compound). The main purpose was to study the influence of heat treatment on changes in crystallinity in the deposited phases. X-ray diffraction analysis and scanning electron microscopy showed that the apatite coatings heat treated between 400 and 600 °C were less crystalline, similar to biological apatites. Upon heat treatment at temperatures above 700 °C, the apatite coatings appeared more crystalline, and were a mixture of hydroxyapatite, octacalcium phosphate and magnesium phosphate.

Resumo em Inglês:

Oxides with spinel structures have been studied for many decades as they have been used in a variety of applications like pigments and refractories. They have also been used as a model structure to evaluate the relative stability of ions in octahedral and tetrahedral sites. Zinc- antimony spinels (Zn7Sb2O12) were synthesized by the Pechini method and the cation Zn2+ was substituted by Co2+, taking into consideration the stoichiometry of Co xZn7-xSb2O12 (x = 0 - 7). Characterization of the thermal properties of pyrolyzed powders was carried out with a TG/DTA analyzer, and mass losses were determined as a function of the cobalt content in the resin. The powders were calcined at temperatures in the range 600 to 1000 °C and characterized by XRD, BET and IR spectroscopy. Maximum cristalinity was obtained in powders calcined at 1000 °C. Materials with x = 5 - 7 revealed the presence of a secondary phase (Co, Zn)Sb2O6. Infrared analysis facilitated in the determination of the possible sites of Zn2+, Co2+ and Sb2+ ions in the lattice.

Resumo em Inglês:

Spinel-type solid solutions were synthesized by the Pechini method and calcined between 500 and 900 °C for 4 hours and at 900 °C for 8 hours to produce ceramic pigments. The resulting powders were characterized by thermogravimetric analysis, Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), particle size analysis and BET surface area measurements. The formation of spinel took place upon calcination at 700 °C. IR spectroscopy revealed the presence of n1 and n2 bands, typical of spinel structures, broadened by the presence of more than one cationic species in the structure. The specific area of the resulting powder decreased from 24.7 to 1.4 m² g-1 as the calcination temperature increased from 700 to 900 °C. Microstructural analyses revealed the presence of crystalline spinel as the only phase present in powders calcined at 900 °C. Colorimetric analyses using L*a*b* coordinates and UV-visible spectroscopy revealed that the pigment was predominantly black.