Resumo em Inglês:

In the field of biomedical applications a special interest exists regarding the study of the physicochemical and mechanical behaviour of materials, with special focus on the electrochemical degradation of metal/ceramic interfaces. In fact, metal/ceramic interfaces may be present in several biomedical devices, ranging from external or implantable sensors, to dental implants. Diffusion bonding represents an important technique since, in opposition to other production technologies, such as active metal brazing, avoid the possible liberation of certain chemical components harmful to health. The aim of this work is to study the electrochemical degradation of the interface formed between commercially pure Ti and Al2O3 produced by diffusion bonding, in contact with a physiological solution. The present approach included the evaluation of the contribution of individual and pairs of interfacial layers on the global degradation processes. For this propose d.c. electrochemical techniques were used to monitor the open-circuit potential, and to perform potentiodynamic polarization and galvanic corrosion evaluation. Also, electrochemical impedance spectroscopy was used as a complementary technique of the corrosion behaviour of the interface. Chemical composition and morphology of samples and corrosion products were evaluated by SEM and EDS analysis. According to experimental results, two principal reaction layers were formed in the interface: TiAl and Ti3Al. The TiAl layer appears to be the responsible for the strong increase in corrosion rate of the interface.

Resumo em Inglês:

Er-doped SnO2 thin films and xerogels are obtained by sol-gel technique. In order to understand the Er³+ rare-earth ion activity in SnO2 matrix, a characterization of Er incorporation is done through emission and excitation spectra of xerogels, besides thin film electrical characterization. Effects to grain dimensions are also analyzed based on X-ray diffraction data showing the particle growth with annealing temperature and inhibition of this growth by Er doping. Electrical characterization results suggest that Er³+ has an acceptor-like character in SnO2, and that codoping with Yb³+ allows an energy transfer process Yb³+ -> Er³+.

Resumo em Inglês:

Transparent electrically conducting antimony-doped SnO2 thin films have been prepared by sol-gel dip-coating process from colloidal aqueous suspension. The effect of doping content on the structural, optical and electrical properties is analyzed. Results from infrared optical transmission and reflection have shown that the higher the Sb concentration the lower the transmission intensity and the higher the reflection signal. Absorption intensity increases as well. Results of X-ray reflectometry and electron microscopy have shown that the density of films fired at 400 °C after each dip is higher than that of multi-dipped films prepared with a single annealing. Both the electrical characteristics in the dark and the increase in conductivity as function of illumination through different filters, at 190 K, evidence that the transport properties of these films are dominated by the presence of defects, including the trapping at grain boundary due to excess of oxygen.

Resumo em Inglês:

This paper reports a study of the influence of Cr concentration and preparation method in the electrical conductivity and microstructure of SnO2-based powders doped with Mn and Nb, prepared by an organic route (Pechini method) and a mixture of oxides. All the samples were compacted into discs and sintered at 1300 °C for 3h, resulting in ceramics with relative density varying between 81 and 99%. The powders were morphologically characterized by X-ray diffraction and their specific surface area was determined by N2 adsorption/desorption isotherms. Electrical conductivity characterization indicated that the conductivity decreases as Cr concentration increases, probably due to Cr segregation at grain boundaries, which reduces grain size, increasing the number of resistive boundaries, thus limiting the passage of current.

Resumo em Inglês:

The objective of this work has been to compare the reliability of two Si3N4 ceramics, with Y2O3/Al2O3 or CTR2O3/Al2O3 mixtures as additives, in regard to their 4-point bending strength and to confirm the potential of the rare earth oxide mixture, CTR2O3, produced at FAENQUIL, as an alternative, low cost sinter additive for pure Y2O3 in the sintering of Si3N4 ceramics. The oxide mixture CTR2O3 is a solid solution formed mainly by Y2O3, Er2O3, Yb2O3 and Dy2O3 with other minor constituents and is obtained at a cost of only 20% of pure Y2O3. Samples were sintered by a gas pressure sintering process at 1900 °C under a nitrogen pressure of 1.5 MPa and an isothermal holding time of 2 h. The obtained materials were characterized by their relative density, phase composition and bending strength. The Weibull analysis was used to describe the reliability of these materials. Both materials produced presented relative densities higher than 99.5%t.d., b-Si3N4 and Y3Al5O12 (YAG) as cristalline phases and bending strengths higher than 650 MPa, thus demonstrating similar behaviors regarding their physical, chemical and mechanical characteristics. The statistical analysis of their strength also showed similar results for both materials, with Weibull moduli m of about 15 and characteristic stress values s o of about 700 MPa. These results confirmed the possibility of using the rare earth oxide mixture, CTR2O3, as sinter additive for high performance Si3N4 ceramics, without prejudice of the mechanical properties when compared to Si3N4 ceramics sintered with pure Y2O3.

Resumo em Inglês:

Flexible, free-standing piezo and pyroelectric composite with 0 to 3 connectivity was made up from Lead Zirconate Titanate (PZT) powder and poly(vinylidene fluoride-hexafluoropropylene) (PVDF-HFP) copolymer. The pyroelectric and the piezoelectric longitudinal (d33) coefficients were measured. A 50/50 vol.% PZT/PVDF-HFP composite resulted in piezo and pyroelectric coefficients of d33 = 25.0 pC/N and p = 4.5 × 10-4 C/m²K at 70 °C, respectively. Analysis of the complex permittivity in a wide range of frequency was carried out indicating lower permittivity of the composite in comparison with a permittivity of the PZT ceramic. The low value of the permittivity gives a high pyroelectric figure of merit indicating that this material can be used to build a temperature sensor in spite of the lower pyroelectric coefficient compared with PZT.

Resumo em Inglês:

HCx powder metallurgy steel contains in its composition high contents of Cr and C, and significant quantities of alloy elements typical of tool steels (Mo, V, W), to provide the corrosion resistance of stainless steel with wear resistance of tool steels. HCx appears to be a suitable material for applications in aggressive environments, as valve seat inserts in automotive engines. However, this steel presents a low compressibility leading to high production costs. In this work, some results carried out to improve the compressibility of HCx are presented. The way to attempt this improvement is the dilution of base material with two stainless steels, the ferritic 430LHC and the austenitic 316L. The powder mixes prepared were uniaxially pressed to study the compressibility. The sinterability was study by determining of density, hardness, transverse rupture strength (TRS) and microstructural evolution after vacuum sintering at different temperatures. As a result, better compressibility is observed in the mixes although not all of them present the properties required.

Resumo em Inglês:

Sintered metallic porous structures have an application as capillary structures in two-phase heat transfer loops. In this work the manufacturing procedure of tubular porous structures for capillary pump application is discussed. The application of porous structures on capillary pumping systems requires porosity higher than 40% and pore size diameter lower than 20 µm. Carbonyl nickel powder with particle diameter between 3 and 7 µm and stainless steel AISI316L powder with particle diameter between 1 and 22 µm were used as raw material. Sintering under hydrogen atmosphere was performed both in a resistive furnace and in a plasma reactor. Temperature and time were the modified parameters to obtain suitable porosity and roundness on the samples. The porosity was measured using the Arquimedes Principle (MPIF-42), the roundness was evaluated using a simplified measurement technique of the sample diameter and the pore size distribution was determined by image analysis techniques. Images obtained by Scanning Electronic Microscopy were employed on the image analysis. The sintering parameters selected to manufacture nickel samples were 700 °C and 30 min resulting in a porosity of about 44%. The sintering parameters selected to manufacture stainless steel samples were 1000 °C and 30 min resulting in a porosity of about 40%.

Resumo em Inglês:

The present work discusses some principles of materials selection and examines a few selection criteria and contexts in which this technical activity takes place. Emphasis is given to the concept of Merit Indices, and to the methodology employed for its deduction. The Materials Properties Charts and their integration with the Merit Indices are introduced and illustrated by the former of the two case studies here presented whilst the second associates the methodology of materials selection to process selection.

Resumo em Inglês:

Potassium dihydrogen phosphate presents a ferroelectric phase below 122 K and a paraelectric phase for T > 122 K. X-ray scattering measurements were performed in order to verify the mechanism of the phase transition from point group C2v19 to C2v¹19 at 119 K induced by DC electric field; in other words, a change of the local site symmetries of the phosphate group occurs from C2 site in the C2v19 point group to Cs in the C2v¹19 point group. This phenomenon was shown by analyzing the behavior of the integrated intensity of the (800), (080), (1600), (0160), (400) and (040) reflections. The curve fitting of these reflections showed the occurrence of a rotation of the phosphate group around the [010] crystallographic direction during the phase transition. This study confirms the observation of this metastable phase obtained by Raman spectroscopy.

Resumo em Inglês:

Poly (vinyl chloride), PVC, is a rigid polymer and for several of its applications must be compounded with plasticizing agents. The plasticizers minimize the dipolar interactions, which exist between the polymer's chains, promoting their mobility. In this work we studied the properties of PVC/plasticizer systems submitted to different doses of gamma radiation. We have used four commercial plasticizers amongt them di(2-ethylhexyl) phthalate, DEHP, which is present in a great number of commercial applications. The PVC/plasticizer systems have been studied as films made by the solvent evaporation technique. Irradiated and non-irradiated films have been characterized by viscosimetric analysis, mechanical essays and infrared spectroscopy. The results have shown that the rigid, non plasticized, PVC film presented the greatest degradation index, while among the plasticized films the one which presented the larger degradation index due to chain scission was the DEHP plasticized PVC.

Resumo em Inglês:

The polyquaternium 7® polymer is widely used in cosmetic formulations. Morphologic alterations in hair fibers were observed after the application of the polyquaternium 7® polymer, using SEM and AFM. Continuous applications of this product indicated that it accumulates on the fibers, improving the aspect of the hair surface. Quantitative analysis of the images obtained by AFM was undertaken. The data obtained for the hair surface roughness indicates that the fibers treated with the polymer presented higher roughness than the untreated hair fibers.

Resumo em Inglês:

The texturing process and the characterization of textured Sr xBa1-xNb2O6 (x = 0.5; x = 0.6) ferroelectric ceramics were investigated. The ceramic bodies were fabricated through two stage sintering. The first and second stage consisted in conventional firing and hot forging of the ceramic bodies, respectively, both at oxygen atmosphere. The forged ceramics achieved high densification level although showing abnormal grain growth. X-ray diffraction, dielectric and pyroelectric analysis showed that is possible to obtain preferential orientation of the [00l] crystallographic planes due to grain arrangement during hot forging. Consequently, the investigated properties for this textured material were strongly dependent on the measurement direction. On the other hand, high room temperature pyroelectric coefficients, of the same order of that obtained for single crystals of same composition, were observed.

Resumo em Inglês:

Gas sensors based in semiconductor oxides show a change in the resistance when they are exposed to certain gaseous atmospheres. In this paper, the influence on the sensor electrical resistance with the film thickness in vacuum and air are studied. The conduction process is analyzed considering the existence of Schottky potential barriers at the grain boundaries. These barriers are affected by the intergranular gas diffusion. This process increases the barrier height and width, altering the electrical resistance. Also, the influence of the diffusion process on the stabilization time is analized.

Resumo em Português:

Átomos de oxigênio, presentes em metais com estrutura cristalina cúbica de corpo centrado, são localizados preferencialmente em sítios octaedrais. Na ausência de uma tensão mecânica externa, estes átomos são distribuídos aleatoriamente. Na presença de oscilações mecânicas, a redistribuição dos átomos nos diferentes sítios deve ocorrer pela interação com esta tensão, levando a perdas na energia elástica. Este trabalho mostra o estudo da interação de átomos de oxigênio presentes em amostras da liga Nb-16% p. Ti, utilizando um pêndulo de torção. Os resultados mostram espectros bastante complexos, que foram decompostos em seus picos constituintes, representando os processos de relaxação devido à reorientação induzida por tensão de átomos e pares de átomos de oxigênio em torno de átomos de nióbio da matriz metálica e átomos de oxigênio em torno de átomos de titânio (interação substitucional-intersticial).

Resumo em Inglês:

In the last years the possibility of creating new conducting polymers exploring the concept of copolymerization (different structural monomeric units) has attracted much attention from experimental and theoretical points of view. Due to the rich carbon reactivity an almost infinite number of new structures is possible and the procedure of trial and error has been the rule. In this work we have used a methodology able of generating new structures with pre-specified properties. It combines the use of negative factor counting (NFC) technique with artificial intelligence methods (genetic algorithms - GAs). We present the results for a case study for poly(phenylenesulfide phenyleneamine) (PPSA), a copolymer formed by combination of homopolymers: polyaniline (PANI) and polyphenylenesulfide (PPS). The methodology was successfully applied to the problem of obtaining binary up to quinternary disordered polymeric alloys with a pre-specific gap value or exhibiting metallic properties. It is completely general and can be in principle adapted to the design of new classes of materials with pre-specified properties.

Resumo em Inglês:

In this study, the MAXIM technique was used in an attempt to clarify the phase transformation sequence that occurs during in situ annealing of galvanized samples. A diffractometer equipped with a novel imaging system comprising a Micro-Channel Plate in front of a CCD camera was used. The galvanized samples were produced under typical industrial conditions, with effective aluminum content at 0.147wt.%. In situ experiments were performed and the phase evolution was recorded in real time. It can be concluded that, coupled to in situ thermal treatment, MAXIM is an efficient method to observe the evolution of the phases present in galvannealed samples. This technique has enough sensitivity to detect the evolution of the involved phases with good spatial resolution.

Resumo em Inglês:

The effect of silver addition as a promoter in alumina supported cobalt oxide catalysts is investigated in this study. The Co/Al2O3 and Ag/Co/Al2O3 catalysts were prepared by incipient wetness impregnation. The catalysts were characterized by inductively-coupled plasma spectrometry, X-ray diffraction (XRD), temperature programmed reduction with hydrogen (TPR-H2), Raman spectroscopy and nitrogen adsorption at 77 K. XDR and Raman Spectroscopy results indicated the presence of Co3O4 species. The peaks observed in the TPR-H2 patterns were attributed to the reduction of Ag2O, Co3O4 crystallites and Co+3, Co+2 species interacting with alumina. It is suggested that silver used as a promoter favors the reduction of cobalt, facilitating the formation of active Co0 sites.

Resumo em Inglês:

Measurements of internal friction as a function of temperature were performed in samples of Nb containing different amounts of substitutional (Zr) and interstitial (O, N) solutes. These data were resolved using the method of successive subtraction, into a series of constituent Debye peaks corresponding to different interactions. For each relaxation process we obtained the height (Q-1max) and temperature (Tp) of the peak, the activation energy (E) and the relaxation time (t0). The height, shape and temperature of the peaks depend on the concentration of interstitial and substitutional elements. With the addition of substitutional solute one can observed interactions between the two types of solutes (substitutional and interstitial), showing that the random distribution of the interstitial atoms was affected by presence of substitutional atoms. The peaks observed were associated with matrix-interstitial (Nb-O, Nb-N) and substitutional-interstitial (Zr-O) interaction processes.

Resumo em Inglês:

This work investigated the influence of the aggregate's aspect ratio on the fracture behavior of a low cement aluminum silicate refractory castable treated at two different temperatures (110 °C and 1000 °C). The aggregates were cylindrical pellets with an aspect ratio of 1, 2, 3 and 4, produced by extruding a mixture of clay and calcined alumina fired at 1600 °C for 4 h to yield mullite (3Al2O3.2SiO2). The behavior of the R-Curve and other relevant fracture parameters were evaluated based on the "Two Parameter Fracture Model" in a three-point flexure test of single-edge straight through notched specimens. The two temperature treatments produced different degrees of matrix-aggregate adhesion. The larger aspect ratio aggregates were found to promote toughening only in the dried condition, at 110 °C, while the specimens fired at 1000 °C for 4 h, regardless of their aggregate aspect ratio, displayed no significant toughening. The best results for fired samples, however, were obtained from specimens containing conventional angular aggregates.

Resumo em Inglês:

Crystalline, electric and fracture properties of Pb(Zr0.52Ti0.48)O3 (PZT) thin films are strongly affected by annealing temperatures in rapid treatment annealing (RTA) of metal organic decomposition (MOD). X-ray diffraction (XRD), RT66A standard ferroelectric analyzer and Vickers indentation method were used to investigate the crystalline, ferroelectric and mechanical properties, respectively. PZT thin film with complete perovskite structure and best ferroelectric property can be obtained at 750 °C, however the fracture toughness was weaker than the thin films annealed at 600 °C and 650 °C. With the increase of annealing temperature from 600 °C to 750 °C, the remanent polarization and coercive field increased in the ranges 13.8~25.2 (µC/cm²) and 7.2~8.3 (kV/cm) respectively, while the fracture toughness of PZT thin films decreased from 0.49 MPam½ to 0.47 MPam½.

Resumo em Inglês:

In this work we report some aspects of the chemistry involved in the preparation of modified silicon oxide by the sol-gel process. Europium III compounds were used as luminescent probe. An organic-inorganic hybrid was obtained by hydrolysis of tetraethylorthosilicate (TEOS) and 3-aminopropyltriethoxysilane (APTS). The Eu III compounds were added in different ways. In the first, silica was prepared in the presence of Eu III, and in the second, Eu III was added on the silica surface. These materials were studied by luminescence, infrared spectroscopy and termogravimetric analysis. The results obtained for the hybrid material show different behavior for Eu III emission, which could be excited by the antenna effect and the influence of the surrounding in the luminescence quenching. The thermogravimetric data present different mass loss in samples to range temperature 50 - 150 °C. Thermogravimetric and infrared spectra showed that inorganic polymers incorporated the organic part.

Resumo em Inglês:

The physico-chemical properties of a series of Ni,Mg,Al-HTLC with Al/(Al+Mg+Ni) = 0.25 and low Ni/Mg ratios were studied by means of X-ray diffraction (XRD), thermogravimetric (TGA) and thermodifferential (DTA) analysis, N2 physissorption and temperature programmed reduction (TPR). The as-synthesized materials were well-crystallized, with XRD patterns typical of the HTLCs in carbonate form. Upon calcination and dehydration the dehydroxilation of the layers with concurrent decomposition of carbonate anions produced mixed oxides with high surface area. XRD analysis indicated that the different nickel and aluminum oxides species are well-dispersed in a poor-crystallized MgO periclase-type phase. As observed by TPR, the different Ni species showed distinct interactions with Mg(Al)O phase, which were influenced by both nickel content and calcination temperature. Regardless of the the nickel content, the reduction of nickel species was not complete as indicated by the presence of metallic dispersions.

Resumo em Inglês:

An investigation was made into the synthesis and magnetic properties of Sm(3-x)Ho xFe5O12 (samarium-holmium-iron) garnet ferrite, as yet absent from the literature. The material in question was synthesized by co-precipitation, starting from hydrated chlorides of rare-earth elements and ferrous sulfate, and the mixed hydroxide co-precipitate was calcined at 1000 °C. Using PVA as a binder, rectangular cross section-shaped compacts were produced by means of steel-die pressing, drying and sintering from 1200 to 1450 °C. The main conclusions of this study were that the coercive force decreases as the sintering temperature increases, and that the effect of substituting holmium for samarium in SmIG is entirely different from that provided by replacing yttrium by gadolinium in YIG, which is the most important result of this work. An in-depth investigation will be necessary to determine the correlation between microstructure/magnetic properties and ceramic processing variables.

Resumo em Inglês:

Bi4Ge3O12 (bismuth germanate - BGO) single crystals were produced by the Czochralski technique and their electrical and dielectric properties were investigated by impedance spectroscopy. The isothermal ac measurements were performed for temperatures from room temperature up to 750 °C, but only the data taken above 500 °C presented a complete semicircle in the complex impedance diagrams. Experimental data were fitted to a parallel RC equivalent circuit, and the electrical conductivity was obtained from the resistivity values. Conductivity values from 5.4 × 10(9) to 4.3 × 10-7 S/cm were found in the temperature range of 500 to 750 °C. This electrical conductivity is thermally activated, following the Arrhenius law with an apparent activation energy of (1.41 ± 0.04) eV. The dielectric properties of BGO single crystal were also studied for the same temperature interval. Permittivity values of 20 ± 2 for frequencies higher than 10³ Hz and a low-frequency dispersion were observed. Both electric and dielectric behavior of BGO are typical of systems in which the conduction mechanism dominates the dielectric response.

Resumo em Inglês:

A mathematical pultrusion model of a thermosetting matrix composite is presented. The energy balance was solved by Finite Elements techniques using a program developed for this purpose. This model is applied to describe the temperature and resin conversion profiles along the die. This study was developed considering different pulling velocity, die temperature, different composite and different sections die. The model outcomes are verified through comparison with the experimental results reported in the literature.

Resumo em Inglês:

This paper shows friction results obtained through compression ring tests for two commercially-available lubricants (i.e., Oildag and Deltaforge) applied in the hot forging of aluminum alloys. The experiments were performed with AA 6061 F aluminum alloy samples with the goal of observing the behavior of each lubricant in several conditions of temperature (200, 300, and 450 °C), strain rates (1, 10 and 50 s-1), and strain (25, 50 and 75%). The friction coefficients for each lubrication condition were established by means of calibration curves determined from finite element calculations with the use of the PEP/Larstran software package. An Analysis-of-Variance approach for the ring's internal diameter was followed in order to evaluate the performance of the lubricants. The results indicated that the Oildag lubricant presents a better stability as well as lower friction coefficients than the Deltaforge lubricant for the range of conditions tested, which translates into a better friction condition at die-part interface.

Resumo em Inglês:

The purpose of this investigation was to evaluate the microhardness of two laboratory-processed composites (Artglass; belleGlass) and two direct placement composites (Filtek Z250; Alert), after aging in distilled water. Twenty cylinders (8 mm diameter; 2 mm height) per tested material were prepared and stored in 10 ml of distilled water. Five Knoop hardness measurements were made on the surface of the specimens with a Miniload Hardness Tester under a load of 50 g for 30 s at 10 min, 24 h, 30 and 90 days. Statistical analysis was perfomed using two-way ANOVA, followed by a SNK multiple comparison test (p < 0.05). The analysis showed statistically significant difference among hardness means recorded at the different aging time and the tested materials. It may be concluded that all materials presented hydrolytic degradation due to aging in aqueous environment.

Resumo em Inglês:

The phenomenological analysis of recrystallization data is described. The concept of microstructural path is briefly introduced as well as some of its relevant equations. The correct equation for the impingement compensated chord length is introduced and used here for the first time. The theory is then applied to data from the recrystallization of a commercial Al-Mn-Fe-Si (AA3003) alloy. It is concluded that nucleation is site saturated and that the grain boundary velocity decreases with time. The analysis also shows that the shape of the recrystallized regions significantly deviates from spherical as the reaction progresses, probably because of the boundary/precipitates interaction.