Scielo RSS <![CDATA[Materials Research]]> http://www.scielo.br/rss.php?pid=1516-143920170004&lang=pt vol. 20 num. 4 lang. pt <![CDATA[SciELO Logo]]> http://www.scielo.br/img/en/fbpelogp.gif http://www.scielo.br <![CDATA[Editorial]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400861&lng=pt&nrm=iso&tlng=pt <![CDATA[Effects of Aging on Chlorinated Plasma Polymers]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400862&lng=pt&nrm=iso&tlng=pt Thin films deposited from propanol-chloroform-argon mixtures by plasma enhanced chemical vapor deposition at different partial pressures of chloroform in the feed, CCl, were characterized after two years of aging and their characteristics compared with their as-deposited properties. Film thickness decreased and surface roughness increased with aging. Surface contact angles also increased with aging for the chlorinated films. For the film deposited with 40% chloroform in the feed the contact angle increased about 14°. Transmission infrared and Energy dispersive X-ray spectroscopy revealed that the films gain carbonyl and hydroxyl groups and lose chlorine and hydrogen on aging. Chlorination appears to make the films more durable. Delamination was observed for the unchlorinated films. <![CDATA[Emission Properties Related to Distinct Phases of Sol-Gel Dip-Coating Titanium Dioxide, and Carrier Photo-Excitation in Different Energy Ranges]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400866&lng=pt&nrm=iso&tlng=pt Titanium dioxide (TiO2) in the form of pellets (pressed powder) and thin films are investigated, revealing the presence of distinct phases: mainly anatase and rutile. Characterization of optical, structural and electrical properties were carried out on samples submitted to different sort of thermal annealing (TA), at distinct temperatures, 500 and 1000ºC, due to their influence on the obtained phases. TA temperature along with pressure application for sample conformation, determine the bands present in the photoluminescence (PL) spectra, being about 550nm, characteristic of anatase phase and 800nm, related to the presence of rutile phase. The bandgap of thin films is determined from optical absorbance data, yielding 3.4eV for anatase phase (indirect transition), and 2.9eV for rutile phase (direct transition). Besides, irradiation with monochromatic light strongly affects the thin film conductivity, but the energy range (above or below the bandgap energy) does not seem to affect the behavior, which is associated with the excitation of intrabandgap states or crystallites belonging to phases with distinct bandgaps. <![CDATA[Study of the Nanostructure Effect on Polyalkylthiophene Derivatives Films Using Impedance Spectroscopy]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400874&lng=pt&nrm=iso&tlng=pt In this paper, devices fabricated with a diode-like structure (electrode/polymer/electrode) from spin-coated and nanostructured (Langmuir-Schaefer) films of polythiophene derivatives were characterized by impedance spectroscopy and studied by theoretical fitting to reach a better understanding of the physical processes in the devices. The materials used for this research were the polyalkylthiophene (P3AT) derivatives poly(3-butylthiophene) (P3BT), poly(3-hexylthiophene) (P3HT), poly(3-octylthiophene) (P3OT) and poly(3-decylthiophene) (P3DT). Electrical measurements were performed from 1 Hz to 1 MHz (100 mV ac) while increasing the dc bias in the range from 0 to 2.5 V. The fittings of the experimental results were performed using equivalent circuits. By plotting the theoretical and experimental spectra on a single graph, it was possible to obtain information related to the film morphology, interfacial effects, resistance, capacitance and conductivity of the polymer, thereby enhancing the understanding of this particular type of device. Among the P3AT films, those grown by the Langmuir-Schaefer technique showed higher electrical conductivity, with the only exception being that of P3BT. <![CDATA[Physical Vapor Deposited Films of a Perylene Derivative: Supramolecular Arrangement and Thermal Stability]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400882&lng=pt&nrm=iso&tlng=pt The analysis of supramolecular arrangement is essential to understand the role of this key factor on the optical and electrical properties of organic thin films. In this work, thin solid films of bis(phenethylimido) perylene (PhPTCD) fabricated using physical vapor deposition (PVD) technique (thermal evaporation), deposited simultaneously onto different substrates (Ag mirror, Ge, and quartz plates) contingent on the characterization technique. The main objective is to study the PhPTCD supramolecular arrangement and the thermal stability of this arrangement in PVD films. The ultraviolet-visible absorption reveals a controlled growth of the PVD films, and the micro-Raman scattering data show that the PhPTCD molecule is not thermally degraded in the conditions of these experiments. The microscopy also shows a homogeneous morphological surface of the PVD film at macro and micro scales, with molecular aggregates at nanoscale. Besides, the PVD film roughness does not follow substrate roughness. The X-ray diffraction indicates a crystalline structure for PhPTCD powder and an amorphous form for PhPTCD PVD film. The infrared absorption spectroscopy points to a preferential flat-on organization of the molecules in the PVD films. In addition, the annealing process (200 ºC for 20 minutes) does not affect the supramolecular arrangement of the PhPTCD PVD films. <![CDATA[Mg-Containing Hydroxyapatite Coatings Produced by Plasma Electrolytic Oxidation of Titanium]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400891&lng=pt&nrm=iso&tlng=pt Plasma Electrolytic Oxidation (PEO) is promising for the processing of biomaterials because it enables the production of surfaces with adjustable composition and structure. In this work, aimed at the improvement of the bioactivity of titanium, PEO has been used to grow calcium phosphide coatings on titanium substrates. The effects of the addition of magnesium acetate to the electrolytes on the composition of the coatings produced during 120 s on Ti disks using bipolar voltage pulses and solutions of calcium and magnesium acetates and sodium glycerophosphate as electrolytes have been studied. Scanning electron microscopy, X-ray energy dispersive spectroscopy, Rutherford backscattering spectroscopy, X-ray diffractometry with Rietveld refinement and profilometry were used to characterize the modified samples. Coatings composed of nearly 50 % of Mg-doped hydroxyapatite have been produced. In certain conditions up to 4% Mg can be incorporated into the coating without any observable significant structural modifications of the hydroxyapatite. <![CDATA[Critical Forces at Fractional Matching Fields in Superconducting Thin Films with Triangular Pinning Lattice]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400899&lng=pt&nrm=iso&tlng=pt We numerically study the commensurability effects in the critical forces in a type II superconducting thin film with vortices under the influence of a triangular pinning lattice at sub matching fields and zero temperature. The analysis is made applying a transport force in two mutually perpendicular directions and magnetic field perpendicular to the film surface. The results show critical force peaks at fractional matching fields, as a direct consequence of the commensurability effects. For the first time, we simulate the sequence of force peaks detected in recent experiments. Anisotropic effects in the critical forces are also reported, in analogy with that found at higher fields. <![CDATA[Structural, Atomic and Electrostatic Force Microscopy Analyses on YBCO/PBCO/LCMO Superlattices]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400904&lng=pt&nrm=iso&tlng=pt In order to study the influence of the insulator layer thickness in heterojunctions, (YBa2Cu3O7-δ[20nm]/ PrBa2Cu3Oy/La1/3Ca2/3MnO3[20nm])x20 superlattices were prepared by pulsed laser deposition using three PrBa2Cu3Oy layer thicknesses and two different sequences of deposition. Sample characterization showed primitive orthorhombic crystalline arrangement for YBCO and LCMO, however, a slightly disordered crystalline structure was observed for the sample having thicker PBCO layer. Microscopy analyses indicated influence of both parameters (PBCO thickness and sequence of deposition) on the texture of the upper layer. Electrostatic Force Microscopy analyses showed evident contrast on the phase images, what suggests that samples are conductive. Distinct surface aspect and highest contrast (highest shift in the electric mode phase image) were observed for the surface of the sample in which the sequence of deposition was inverted, with the YBCO ceramic as upper layer of the superlattice. <![CDATA[Easy and Fast Preparation of TiO<sub>2</sub> - based Nanostructures Using Microwave Assisted Hydrothermal Synthesis]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400912&lng=pt&nrm=iso&tlng=pt TiO2 derivatives with distinct morphologies have been successfully obtained by microwave assisted hydrothermal synthesis in acidic and alkaline medium using mild conditions. Titanium tetraisopropoxide (TTIP) was used as precursor in different environmental conditions under low temperatures, inferior to 150 °C, and short synthesis times, from 2 to 60 min. X ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and N2 adsorption at 77 K (BET) were used to characterize the microstructural properties of the oxides. In the acidic synthesis the reaction time and temperature are not accompanied by significant changes in the structure of the material. However, in the basic conditions, the concentration of Na+ ions strongly influences the particle morphology and growth. The morphology of the nanoparticles shows irregular spheres in acidic conditions, while in alkaline medium, needle like structures are formed as well as aggregated nanotube-like structures synthesized in only 30 min. Besides the difference in the morphology and structure, in both systems, high surface area was obtained. <![CDATA[Computational Simulations of Morphological Transformations by Surface Structures: The Case of Rutile TiO<sub>2</sub> phase]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400920&lng=pt&nrm=iso&tlng=pt Computational simulations based on periodic density functional theory have been carried out to investigate the control of crystal morphology by accurate values of surface energies by Wulff theorem. This method can be used as a very useful tool for the design and knowledge of synthesis of new materials. In a special case, rutile TiO2 phase, exhibits great variety of morphologies and properties making this system an interesting target for this approach. The low index, (100), (001), (101), (110), (111) surfaces were modeled and the respective surface energies produces the follows stability order: (110) &lt; (010) &lt; (101) &lt; (001) &lt; (111). The map of some morphologies routes was constructed from the calculated energies as a starting point without environmental influence and can be used to elucidate the influence of chemical routes. This method has helped in the knowledge of morphological modifications as a function of synthesis environment besides the connection between system characteristics and the exposed surfaces. <![CDATA[Films Deposited from Reactive Sputtering of Aluminum Acetylacetonate Under Low Energy Ion Bombardment]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400926&lng=pt&nrm=iso&tlng=pt Films were deposited from aluminum acetylacetonate (Al(acac)3) using a methodology involving reactive sputtering and low energy ion bombardment. The plasma was generated by the application of radiofrequency power to the powder containing electrode and simultaneously, negative pulses were supplied to the electrode where the substrates were attached. It was investigated the effect of the duty cycle of the pulses (Δ) on the properties of the coatings. Association of ion bombardment to the deposition process increased film thickness, structure reticulation and organic content. Ions from the deposition environment were implanted at the film-air interface or underneath it. Morphology and topography were altered depending on Δ. Considering the enhancement of Δ, it affected the flux of ions reaching the depositing interface and then the deposition rate, H content, crosslinking degree and surface microstructure. Alumina groups were detected in the infrared spectra, whereas the precipitation of amorphous alumina was confirmed by X-ray diffraction. <![CDATA[Thermoanalytical, Spectroscopic and DFT Studies of Heavy Trivalent Lanthanides and Yttrium(III) with Oxamate as Ligand]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400937&lng=pt&nrm=iso&tlng=pt Solid-state LnL3∙nH2O complexes, where Ln stands for trivalent lanthanides (Tb to Lu) or yttrium(III) and L is oxamate (NH2COCO2-), have been synthesized. The characterization of the complexes was performed by using elemental analysis (EA), complexometric titration with EDTA, thermoanalytical techniques such as simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC), evolved gas analysis (TG-FTIR), infrared spectroscopy (IR) and powder X-ray diffraction (XRPD). The results provided information about thermal behavior, crystallinity, stoichiometry, coordination sites, as well as the products released during thermal degradation of the complexes studied. Theoretical calculation of yttrium oxamate, as representative of all complexes was performed using density functional theory (DFT) for studying the molecular structure and vibrational spectrum of the investigated molecule in the ground state. The optimized geometrical parameters and theoretical vibrational spectrum obtained by DFT calculations are in good agreement with the experimental results. <![CDATA[The distribution of Lignin and Xylan in the Inner and Surface Layers of the Fiber from Eucalyptus Kraft Pulp and its Effects on Oxygen Delignification]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400945&lng=pt&nrm=iso&tlng=pt The chemical structure and composition of lignin and hemicellulose, as well as the distribution between inner and outer layers of fiber, can adversely affect bleaching operations or fiber-fiber bond on pulp and, consequently the papermaking process. Herein, we have implemented the fractionation and mechanical peeling techniques in order to identify the fines composition from eucalyptus cellulose as well as to verify the effect over xylan and lignin contents and the impact on oxygen delignification. Lignin and xylans in the material removed from the fiber surface (fines) were measured around to 7.6% and 12% of the composition, respectively. The lignin value is three times higher than the percentage measured to original fiber composition (without treatment). The residual xylans content on the pulp, after treatment of fines removal and peeling, was slightly reduced, around 3% for both treatments as well as fractionation and peeling methods decrease the oxygen delignification efficiency. <![CDATA[Carbon Fiber Reinforced Polymer and Epoxy Adhesive Tensile Test Failure Analysis Using Scanning Electron Microscopy]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400951&lng=pt&nrm=iso&tlng=pt Morphological characteristics analysis before and after tensile tests were studied using scanning electron microscopy (SEM) technique to follow the failure evolution on carbon fiber reinforced polymer (CFRP) and epoxy resins. Micrograph analysis of CFRP plate before tensile test shows some intrinsic manufacturing defects, which can influence the mechanical properties of the material. Micrograph analysis after tensile test shows that cracks propagation start in manufacturing defects, which lead the carbon fiber to be pulled out instead of breaking. Thus, cracks propagate through interfacial zones affecting the sharing force between matrix and carbon fiber. For the epoxies materials, the microscopy analysis showed that although epoxies adhesive have different phase distribution before tensile test, failure surfaces are described by fine granular particles covalent bonded with matrix, and the material fails in a brittle manner when the strength outstripped these bonds. Failure process for each material correlating the mechanical properties with the morphological characteristics of materials was discussed. <![CDATA[Evolution of TiO<sub>2</sub> Nanotubular Morphology Obtained in Ethylene Glycol/Glycerol Mixture and its Photoelectrochemical Performance]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400962&lng=pt&nrm=iso&tlng=pt The evolution of TiO2 nanotubular morphology, synthesized in a mixture of fluorinated ethylene glycol and glycerol electrolyte, was studied as a function of the anodization time. The samples were characterized by FEG-SEM, XRD, XPS, UV-Vis and EIS. The formation of single-or double-walled TiO2 nanotube structure can be efficiently controlled by the anodization time. For anodization times less than 30 minutes, a compact oxide layer is formed, followed by double-walled nanotube formation up to 120 minutes and single-walled nanotubes up to 240 minutes. XPS analyses show that the samples obtained with short anodization time have a high carbon content and oxygenated surface species compared to the longer-time anodized sample; however, binding energy peaks for Ti 2p remained invariant. The performances of TiO2 nanotubular photoelectrodes were evaluated in photoelectrochemical water splitting where TiO2 nanotubes anodized for 120 minutes presented the best performance that was related to their optimal morphology and charge transportation. <![CDATA[Preparation, Characterization and Biological Studies of Β-TCP and Β-TCP/Al<sub>2</sub>O<sub>3</sub> Scaffolds Obtained by Gel-Casting of Foams]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400973&lng=pt&nrm=iso&tlng=pt Replacement tissues for tissue engineering can be produced by seeding human cells onto scaffolds. In order to guarantee adequate bio-compatibility, porosity and mechanical resistance for promoting cellular growth, proliferation and differentiation within scaffold structures, it is necessary to investigate and improve materials and processing routes. β-tricalcium phosphate can be considered a very suitable bio-ceramic material for bone therapy because of its biocompatibility, osteo-conductivity and neo-vascularization potential. Alumina is commonly used as a sintering additive. In this study, β-TCP and β-TCP/Al2O3 scaffolds were obtained by gel-casting method. The scaffolds showed high porosity (86-88%) and pore sizes ranging from 200 to 500 µm. Even though alumina did not promote improvement in β-TCP/Al2O3 scaffolds in terms of mechanical performance, they showed great cytocompatibility as there was no cytotoxic and genotoxic effect. Therefore, β-TCP and β-TCP/Al2O3 scaffolds are good candidates for application in tissue engineering. <![CDATA[Effect of Chitosan on the Properties of Electrospun Fibers From Mixed Poly(Vinyl Alcohol)/Chitosan Solutions]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400984&lng=pt&nrm=iso&tlng=pt Electrospun nanofibers were prepared from mixed solutions of partially hydrolyzed poly(vinyl alcohol) (PVA) and medium molar mass chitosan (CS) at different solution compositions, at 15 and 20 kV. The mats were visualized by scanning electron microscopy (SEM), and the average diameters of nanofibers were determined. Three of these solutions were chosen for further studies, to elucidate the influence of CS on the mats properties. Electrospinning at 15 kV had a higher tendency to produce nanofibers free of defects, in which the diameters (157 to 189 nm) were not affected significantly by the total concentration and solution composition. Polymer interactions between the components were supported by infrared spectroscopy, thermogravimetry and dynamic mechanical analysis (DMA). The effect of CS composition was evidenced by DMA and tensile tests techniques. Immersion in water led to the breakage of nanofibers and flower-like morphologies. <![CDATA[High Temperature Erosion-oxidation Resistance of Thermally Sprayed Nanostructured Cr<sub>3</sub>C<sub>2</sub>-25(Ni-20Cr) Coatings]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000400994&lng=pt&nrm=iso&tlng=pt This study reports the high temperature erosion-oxidation (E-O) behavior of conventional and nanostructured Cr3C2-25(Ni-20Cr) coatings prepared by high velocity oxygen fuel (HVOF) spraying. As-received and nanostructured Cr3C2-25(Ni-20Cr) powders with mean crystallite sizes of 145 nm and 50 nm respectively, were used to prepare 120 - 200 µm thick coatings on AISI 310 samples. The E-O behavior of the coatings prepared with the as-received (AR) and nanostructured (NS) powders was determined as weight change in a custom designed rig at room temperature, 450, 700 and 800 ºC. The Vickers microhardness, Young's Modulus and fracture toughness of the AR and NS coatings were determined, and the NS coatings exhibited higher values compared with the AR coatings. The E-O resistance of the NS coating was higher than that of AR coating at all temperatures, and particularly at 800 ºC. The increase in E-O resistance of the NS coatings is due to its superior mechanical properties as well as to the presence of some heterogeneities in the AR coatings. The E-O mechanisms of both types of the coatings are discussed, with special attention to that at high temperatures. The results suggest that at 800 ºC the E-O process is controlled by erosion of the oxide. <![CDATA[Effects of Pre-Strain on the Evolution of Microstructure and Strain Hardening of Extruded Az31 Magnesium Alloy]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401003&lng=pt&nrm=iso&tlng=pt Pre-compression 3% and pre-stretch 3% subsequent annealing at 200ºC for 2h are conducted on AZ31 magnesium alloys, then inverse tensile and compressive deformation are carried out at room temperature, respectively. During inverse tension 3% deformation on 1st pre-compression samples, detwinning behavior happens; after 2nd pre-compression 3%, the volume fraction of {10-12} extension twins decreases comparing with 1st pre-compression. Due to the interaction of dislocation and induced twinning lamellas, strain hardening rate (θ) increases on 1st and 2nd pre-compression samples. {10-12} tensile twinning is restrained during inverse compressive deformation by pre-stretch process. Owing to the decreasing amount of twins, the texture strengthening in compressive deformation weakens. So the slop of stage III in strain hardening rate sustaining reduces after 1st pre-stretch 3% and 2nd pre-stretch 3% deformation during inverse compression deformation. <![CDATA[A Model for the Formation of Niobium Structures by anodization]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401010&lng=pt&nrm=iso&tlng=pt The fluoride use for anodizing electrolytes has been primarily responsible for the formation of nanoporous oxides at valve metals, except aluminum, since it causes a dissolution process. This study presents the formation of an oxide model according to the following anodizing parameters: 100 V, 12.73 mA/cm2, room temperature and the niobium samples anodized in niobium oxalate and oxalic acid electrolytes without and with the addition of HF for 5, 30 and 60 min. The anodized samples were analyzed morphologically by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), atomic force microscopy (AFM) and the hydrophobicity of the samples was assessed by the sessile drop method. The presence of fluor in the niobium oxalate electrolyte formed oxides with lower a dissolution and a low hydrophobicity compared to the one formed in oxalic acid was attributed to the incorporation of niobium and oxalate ions. Thereby, the model proposed in this paper showed that during anodization the migration of the fluoride ion into the oxide occurs at high speed, which results in the formation of microcones, leading to the formation of discrete layers of porous oxide. <![CDATA[Effect of LZSA Glass-Ceramic Addition on Pressureless Sintered Alumina. Part I: Grain Growth]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401024&lng=pt&nrm=iso&tlng=pt The aim of this study was to evaluate the effect of an 11.6Li2O-16.8ZrO2-68.2SiO2-3.4Al2O3 (LZSA) glass ceramic on the grain growth of alumina obtained by pressureless sintering. Three contents of the LZSA glass ceramic (7, 15, and 21 vol%; mean particle size of 1.52 µm) and three types of alumina (mean particle sizes of 0.5, 1.7, and 2.8 µm) were used. The powder compositions were formed by cold pressing. The samples (5 mm × 5 mm × 13 mm) were sintered in an optical dilatometer. The grain size and morphology were evaluated by scanning electron microscopy. The results show that elongated alumina particles were obtained for the investigated composites compared with pure alumina because of the LZSA addition. The grain growth of alumina was less pronounced at higher LZSA contents. High relative densities were obtained for higher LZSA contents at lower temperatures and holding times compared with pure alumina. <![CDATA[Influence of Niobium and Molybdenum on Mechanical Strength and Wear Resistance of Microalloyed Steels]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401029&lng=pt&nrm=iso&tlng=pt The HSLA (High-Strength Low Alloy) steels are used in the production of pipes, flanges and connectors to build ducts for ore, oil and gas transport. The conventional processes are the rolling or forging. In the transport of ore and heavy oil, the abrasive particles impair the surfaces and reduce the pipelines lifetime. Therefore, besides the mechanical properties as API 5L, it is important to verify the wear resistance of these steels. In this context, two microalloyed steels were forged in the form of square bars. Thereafter, specimens of these bars were annealed at 930 ºC, quenched at 900 ºC and tempered at 600 ºC. Tensile and wear tests were performed. The results show that molybdenum and niobium present similar effects on phase transformation of steels, promoting a desired acicular ferrite/bainite microstructure and fulfill the mechanical strength of API 5L-X70 standard. The molybdenum has dominating effect in the hardenability when in solid solution, however, after tempering, thermodynamic simulation by FactSage software indicates that niobium probably promotes secondary hardening. <![CDATA[Phase Diagram Study for the PbO-ZnO-CaO-SiO<sub>2</sub>-"Fe<sub>2</sub>O<sub>3</sub>" System in Air with CaO/SiO<sub>2</sub> in 1.1 and PbO/(CaO+SiO<sub>2</sub>) in 2.4 Weight Ratios]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401035&lng=pt&nrm=iso&tlng=pt An experimental study on the phase equilibrium and the liquidus isotherms for the PbO-ZnO-CaO-SiO2-"Fe2O3" system with CaO/SiO2 in 1.1 and PbO/(CaO+SiO2) in 2.4 weight ratios, respectively, was carried out in the temperature range 1100-1300ºC (1373-1573 K). High temperature phases were determined by the equilibrium-quenching method. Results are presented in the form of pseudo-ternary sections "Fe2O3"-ZnO-(PbO+CaO+SiO2). X-Ray diffraction (XRD) and SEM-EDS results showed that the phase equilibria in this system are dominated by the high melting temperature spinel and zincite phases. It was observed that if the system is at a temperature below 1300ºC and the total (Fe2O3 + ZnO) is greater than 20 wt%, spinel and/or zincite will be present in the slag system. As an application of the phase diagram, the liquid phase compositions below the liquidus surface were estimated, then their viscosities were calculated using FACTSage software. <![CDATA[Nanoparticles of ZnO Doped With Mn: Structural and Morphological Characteristics]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401044&lng=pt&nrm=iso&tlng=pt In this study, the effects of dopant concentrations on the structural and morphological characteristics of Zn1-xMnxO powders (x= 0.025, 0.05, 0.075, and 0.1 mole) synthesized by the Pechini method has been investigated. The powder was characterized by X-ray diffraction (XRD), Brunauer-Emmet-Teller (BET) specific surface, energy dispersive X-ray (EDX), scanning electron microscopy (SEM) and Spectroscopy with Fourier transform (FTIR). An XRD analysis of the powder showed the formation of ZnO phase with a typical single phase wurtzite structure. The EDX analysis revealed Mn incorporated in the ZnO structure. The particle size calculated by BET ranged from 24 to 63 nm, confirming the nanometric size of the powder particles. The SEM analysis revealed irregular shaped particle agglomerates and the presence of nanosheets. From FTIR it was confirmed the wurtzite structure in ZnO and ZnO nanoparticles doped with Mn. <![CDATA[Influence of Tungsten on Dry Sliding Wear Behaviour of Sintered/Hot Extruded P/M Alloy Steels (Fe-C-W-Ti)]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401050&lng=pt&nrm=iso&tlng=pt In the present scenario, Powder Metallurgy (P/M) is an established manufacturing process used to make components of complex geometries with high strength and tolerances by using incredible materials which are difficult to melt or form by other processes. The mechanical properties and microstructures will determine the component characteristic dependent on the final obtained density of sintered P/M alloy steels. An attempt has been made to investigate the dry sliding wear behaviour of sintered/hot extruded P/M alloy steels with Fe-1C as base material, W (Tungsten) and Ti (Titanium) as an alloying element. The wear test was carried out by using a pin-on-disc tribometer (ASTM G99) against EN 38 steel disc (HRC 60) with a constant sliding speed of 2m/s at normal loads of 30, 50 and 70N respectively. The microstructure of the as-sintered P/M alloy steels reveals the ferritic-pearlite structure whereas for hot extruded alloy steels the microstructure shows a combination of Widmanstatten type ferrite, pearlite and bainite. From the microstructure the presence of WC (tungsten carbide) embedded with Ti in the grain boundaries offers greater wear resistance of the hot extruded P/M alloy steels. The common wear mechanism observed for hot extruded alloy steels is Delamination wear. <![CDATA[Phase Equilibria in the Tl<sub>5</sub>Te<sub>3</sub>-Tl<sub>9</sub>BiTe<sub>6</sub>-Tl<sub>9</sub>TmTe<sub>6</sub> Section of the Tl-Bi-Tm-Te Quaternary System]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401057&lng=pt&nrm=iso&tlng=pt Phase relations in the Tl5Te3-Tl9BiTe6-Tl9TmTe6 section of the Tl-Bi-Tm-Te quaternary system were studied by differential thermal analysis, powder X-ray diffraction technique and microhardness measurements applied to equilibria alloys. Some isopleth sections and isothermal section at 760 K, as well as projections of the liquidus and solidus surfaces, were constructed. The system is characterized by formation of continuous series of solid solutions at the solidus temperatures and below. Solid solutions are crystallized in the tetragonal Tl5Te3 structure type. <![CDATA[Microstructure Evolution of the Mg-5.8 Zn-0.5 Zr-1.0 Yb Alloy During Homogenization]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401063&lng=pt&nrm=iso&tlng=pt The influence of homogenization treatment on microstructure evolution of Mg-5.8Zn-0.5Zr-1.0Yb (mass fraction, %) alloy was investigated under different annealing temperatures and holding times. Results indicated a severe dendritic segregation in the as-cast ingot. Zn and Yb segregate remarkably at the grain boundary and Zr appears in the form of precipitates. The Mg-Zn binary eutectic phases and a new ternary phase Mg-Zn-Yb are mainly distributed at dendrite boundaries. After homogenization, most of the eutectic phases dissolve into the matrix, except for a small amount of Mg-Zn-Yb phase. The area fractions of residual secondary phase decrease from 5.54% in the as-cast alloy to 0.59% in the well-homogenized sample. Microhardness test indicates that with the increasing temperature and holding time, microhardness value decreased sharply within the first stage of homogenization and then increased steadily to the local maximum value at 380 ºC and 12 h, followed by a slight reduction. Basing on the comprehensive analysis on microstructure and mechanical properties, the homogenization treatment at 380 ºC for 12 h is preferable. <![CDATA[Structural and Photoacoustic Study of Cr<sub>11</sub>Ge<sub>19</sub> Prepared by Mechanical Alloying]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401072&lng=pt&nrm=iso&tlng=pt A nanostructured Cr11Ge19 phase was produced by mechanical alloying for 15 h. Decomposition occurred for larger milling times, yielding Cr, Ge, Cr2O3 and GeO2. According to the Cr-Ge phase diagram, the Cr11Ge19 phase is stable up to ≈ 928 oC, but, when submitted to milling, a structural instability causes its decomposition. We studied this structural instability using the coordination numbers and interatomic distances of bulk Cr11Ge19 to simulate the structure factors SCrCr(K), SCrGe(K), and SGeGe(K). The radial distribution functions RDFCrCr(R), RDFCrGe(R) and RDFGeGe(R) were obtained by Fourier transforming the Sij(K) factors, and an important chemical disorder up to ≈7 Å was observed in the RDFCrGe(R) and RDFGeGe(R) functions. This chemical disorder was quantified using Cowley-Warren α ij CW parameter. The thermoelectric properties of the Cr11Ge19 phase were also studied. <![CDATA[Influence of ZnO and TiO<sub>2</sub> Particle Sizes in the Mechanical and Dielectric Properties of Vulcanized Rubber]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401082&lng=pt&nrm=iso&tlng=pt The novelty of the present study relies on the straightforward sonication of ZnO and TiO2 and incorporation to a complex formulation of latex, with other several organic-inorganic additives that influences the cross-linking reactions. The new elastomer with particles carefully sonicated exhibit improved electrical and mechanical properties. Strong interaction among the nanoparticles and the polymer amorphous phase has been proved by means of FTIR, SEM and XRD analyses. The synergistic effect of hybrid fillers with nanometric dimensions can be used to design high-performance natural rubber nanocomposites with enhanced electrical resistance and good cross-linking degree. <![CDATA[Micro-Scale Abrasive Wear Testing of CrN Duplex PVD Coating on Pre-Nitrided Tool Steel]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401092&lng=pt&nrm=iso&tlng=pt Specific wear rates were calculated from a series of micro-scale abrasive tests by means of the calotte-grinding method. The tested material was a CrN coating deposited by arc evaporation on ion-nitrided AISI H13 steel. Characterizations included: phase analysis, chemical composition, metallography, microhardness, micro-scratch resistance and nano-indentation hardness. On wear testing, the counter body was a 30 mm diameter steel ball rotating at a tangential speed of 9.42 m/min and normal load of 0.54 N. The abrasive was a mono-crystalline diamond micro abrasive paste, 1 micrometer grit. Wear volumes were calculated by measuring the wear scars at various test intervals. In non-perforating tests, Archard's wear equation was directly employed for calculating coating wear rate as the slope of the linear least square data fit. In perforating tests, Allsopp's method was employed for the simultaneous determination of coating and substrate wear rates, from the slope and intercept values of the linear least square data fit. Coating specific wear rate values obtained from both non-perforating and perforating tests were very consistent, with a relative difference within 6%. Relative errors in specific wear rate values were estimated to be of the order of 0.05 for the coating and 0.2 for the substrate. <![CDATA[The Effect of TiO<sub>2</sub>-SiO<sub>2</sub> Nanocomposite on the Performance Characteristics of Leather]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401103&lng=pt&nrm=iso&tlng=pt In this study the effect of TiO2-SiO2 nanocomposite on various performance characteristics of finished leather was investigated. For this purpose, TiO2-SiO2 nanocomposite was prepared via the sol-gel method from tetraethoxysilane (TEOS) and titanium n-butoxide (TBO) catalyzed with acid at ambient temperature. The prepared composite was applied by spraying on to the top coat of finished leathers. Scanning electron microscopy (SEM) and Fourier transform infrared (FTIR) were employed to characterize the surface properties and the chemical structure of the nanocomposite films. Inductively coupled plasma optic emission spectrometer (ICP-OES) was used to evaluate elemental analysis of the nanocomposite on leather. The physical-mechanical and fastness properties of leathers treated with the nanocomposite were evaluated according to appropriate standards. The results indicated that the use of TiO2-SiO2 nanocomposite improved certain performance characteristics of leather such as dry and wet rubbing fastness, color fastness to UV light and finish adhesion. <![CDATA[Multistage Deep Drawing with Ironing of Al-killed AISI 1040 Graded Medium Carbon Steel: a Parametric Study]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401111&lng=pt&nrm=iso&tlng=pt Analysis of multistage deep drawing with ironing was made while manufacturing of cups from 12 mm thick, 60 mm diameter circular blanks of Al-killed AISI 1040 graded medium carbon steel. Quality requirements of the steel in heat treated condition were examined in terms of tensile properties, formability characteristics, and formability limit diagram. Drawability and ironability parameters in multistage cup drawing processes were evaluated in terms of draw ratio; draw reduction; ironing ratio; ironing reduction and thus its press formability in an actual state of practice was shown. Further, were analysed the influences of process parameters such as: semi die angle; interfacial friction coefficient; die-punch clearance on draw and ironing punch forces in each draw stage. The spring back tendency of cups in terms of their trends and degrees with respect to cup heights and draw stages were experimentally determined by conducting split ring test. Thus, a data bank was created as potential references for process engineers to improve the manufacturing process and draw tools as well, particularly for the selected steel. <![CDATA[Temperature and Deposition Time Effect on Properties and Kinetics of CdSe and CdS<sub>0.25</sub>Se<sub>0.75</sub> Films Deposited by CBD]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401121&lng=pt&nrm=iso&tlng=pt CdSe and CdS0.25Se0.75 thin films were grown by the Chemical Bath Deposition technique at different temperatures (50-90°C) and deposition times (5-180 min). Both kinds of films are polycrystalline, constituted by nanostructured clusters of particles. CdSe films consist in a mixture of cubic and hexagonal phases (4-8 nm crystal size), whereas only the hexagonal phase is observed in the CdS0.25Se0.75 ones (6±1 nm crystal size). A decrease on the CdSe films density was observed due to the sulfur introduction into the crystal lattice. The composition of the ternary films is affected by both temperature and deposition time. The Band gap values (Eg) are affected by temperature, atomic composition and deposition time, decreasing from 2.09 to 1.93 eV, showing a quantum confinement effect mainly in the CdSe films. The films thickness, ranging from 30 to 600 nm, increases as a function of temperature and deposition time. Photoluminiscence signal is improved after thermal treatment, evidenced by the radiative broad bands observed at 1.84 and 2.20 eV. <![CDATA[Macrosegregation of Impurities in a Metallurgical Silicon Ingot After Transient Directional Solidification]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401129&lng=pt&nrm=iso&tlng=pt Metallurgical grade silicon was melted and directionally solidified in transient conditions by extracting heat from the base of a cylindrical ingot and inserting heat at the ingot top. A heat-transfer mathematical model was implemented to predict the solidification velocity and temperature gradient using cooling curves measured directly in the silicon melt. Nearly 70% of the resulting ingot displays a region of columnar grains aligned with the ingot axis. In this region, the concentration of metallic impurities is usually below the quantification limit of the analytical technique and intermetallic particles are absent, strongly indicating significant purification. The transition from the purified region of the ingot to the ingot top, where impurity concentrations increase and intermetallic particles are seen, is consistent with a change of the solid-liquid interface morphology from planar to cellular/dendritic, as similarly reported in the literature and as indicated by a preliminary analysis with the constitutional undercooling criterion. <![CDATA[Ordered Silica Particles Made by Nonionic Surfactant for VOCs Sorption]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401136&lng=pt&nrm=iso&tlng=pt Adsorption of light organic compounds such acetone, 1-propanol and carbon dioxide was tested by using mesoporous silica materials made from non ionic surfactant with long chain and silica sources as tetraethylorthosilicate TEOS and modified Na-X and Li-A Zeolites. X-ray powder diffraction (XRD), nitrogen adsorption-desorption analysis and scanning electron microscopy (SEM) were applied to characterize the silica particles of a variety prepared samples. Acetone, 1-propanol and CO2 adsorption at 298K was evaluated by a volumetric method and indicate a high sorption capacity of organic compounds depending essentially on the porous texture of adsorbents. An adsorption kinetic model was proposed to describe the adsorption of VOCs over template-free mesoporous silica materials. A good agreement with experimental data was found. <![CDATA[Laser Surface Modification of Ti6Al4V-Cu for Improved Microhardness and Wear Resistance Properties]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401143&lng=pt&nrm=iso&tlng=pt To modify the properties of Ti6Al4V alloy, Cu has been added to host an antimicrobial effect in the revised alloy for marine application. The Laser Metal Deposition (LMD) process on the Ti6Al4V alloy and Cu was been investigated for surface modification in order to combat the problem of biofouling in the marine industry. The investigations focused on the microstructural observations, micro-hardness measurements and dry sliding wear in the presence of 3 and 5 weight percents of Cu. The microstructure results showed that Widmanstätten microstructures were formed in all the samples and lose their robustness towards the fusion zone as a result of the transition of heat sink towards the substrate. The microhardness values of Ti6Al4V-3Cu and Ti6Al4V-5Cu alloys were greatly improved to 547±16 VHN0.5 and 519±54 VHN0.5 respectively. Furthermore, the behaviour of wear loss on the surface of the Ti6Al4V-Cu alloys exhibited great improvement as compared with the parent material. <![CDATA[[RETRACTED ARTICLE]: Load Dependent Wear Analysis of Manganese Steels - Influence of Al Content]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401153&lng=pt&nrm=iso&tlng=pt In this paper influence of load on change in weight loss (mg), hardness and wear transition of 0.12 wt.% Al-Mn-steel (Steel A), 0.35 wt.% Al-Mn-steel (Steel B) and Mn-steel (Steel C) has been examined. With the increase in load these steels shows remarkable decrease in weight loss due to change in surface microstructure from austenite to ε or ά - martensite which results in increase in hardness of material. With the increase in hardness transition in wear mechanism has been noticed. In future aspect these steel would prove to be better material as wear resistant liner in many industrial application. <![CDATA[Retraction]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392017000401160&lng=pt&nrm=iso&tlng=pt In this paper influence of load on change in weight loss (mg), hardness and wear transition of 0.12 wt.% Al-Mn-steel (Steel A), 0.35 wt.% Al-Mn-steel (Steel B) and Mn-steel (Steel C) has been examined. With the increase in load these steels shows remarkable decrease in weight loss due to change in surface microstructure from austenite to ε or ά - martensite which results in increase in hardness of material. With the increase in hardness transition in wear mechanism has been noticed. In future aspect these steel would prove to be better material as wear resistant liner in many industrial application.