Resumo em Inglês:

Hydration products of Portland cement pastes, hydrated in water and in the presence of zinc ions were studied comparatively at different ages. Hydration products were studied by X ray diffractions (XRD) and infrared spectroscopy (IR). Although IR is not frequently used in cement chemistry, it evidenced a new phase Ca(Zn(OH)3)2. 2H2O formed during cement hydration in the presence of zinc. The significant retardation of early cement hydration in the presence of zinc is assessed in detail by differential calorimetry as a complement to the study carried out by IR and XRD, providing evidence that permits to evaluate the kinetic of the early hydration.

Resumo em Inglês:

In the present work, polyesters were prepared from the polycondensation between glycerol and adipic acid using dibutyltin dilaurate as catalyst. Three glycerol: adipic acid molar ratio were used for the bulk polymerization namely: 2:2; 2:3 and 2:4. FTIR confirmed the esterification of glycerol by the acid for all the polymers. DSC and XRD indicated no crystallinity for all the polymers. The morphology of the materials are characterized by globular structure, which may suggest compositional fluctuations throughout the samples.

Resumo em Inglês:

The thermal behavior of a mixture of recycled polyolefins (PE/PP mix), variously colored recycled polyolefins, recycled polyolefin blends and recycled polyolefin/PET blends was analyzed by thermogravimetry. Atmospheres of nitrogen and synthetic air were used to compare the effects of inert and oxidative medium. Four characteristic temperatures, T1, T2, T3 and T4, related to oxidative processes and atmospheric conditions, were defined. Relationships between T1, T2, T3 and T4 and comparing pigmented and transparent material allow assessing the effect of different pigments on volatilization, oxidation and onset temperatures of decomposition processes. These analyses provide preliminary parameters for selecting acceptable processing temperature conditions of recycled household and engineering plastics, and provide a few criteria to select colored recycled polyolefins.

Resumo em Inglês:

Chitosan microspheres can be used in several applications, as biomaterials, in biotechnology processes and as adsorbents. The control of particle size in microsphere production is important to make these applications viable. This study focuses on the production and morphological characterization of chitosan microspheres. Microspheres were prepared by a spraying and coagulation process. Particles underwent chemical modifications with glutaraldehyde, epichlorohydrin or acetic anhydride treatments. The microspheres presented a fairly good sphericity (0.74) but an irregular micro-surface morphology. The mean particle size (MPS) ranged from 140 to 281 mum and the mean standard deviation (MSD) from 119 to 238 mm. The conditions were modelled to provide desired MPS and MSD by using the response surface methodology (RSM).

Resumo em Inglês:

Development of polymeric materials has been increasingly emphasized in Biomedicine. Here, we evaluate the use of microcapsules made of Biodritin®, a biocompatible polymer compound which contains sodium alginic acid, a natural polymer extracted from algae, and Cis-Chondroitin sulfate, a glycosaminoglycan from the extracellular matrix. Gelation of this polymer into microcapsules is achieved by dropping the compound into BaCl2 or CaCl2 gelling solutions. A functional microcapsule is dependent on its permeability, mechanical stability, immunoisolation capacity and biocompatibility. The mechanical stability of Biodritin-barium and Biodritin-calcium microcapsules was investigated after rotational stress upon in vitro culture and in vivo implantation. Viability studies of encapsulated cells were also performed to assess other functional parameters of the microcapsules. When subject to rotational stress, Biodritin-barium microcapsules exhibited breaks, whereas the Biodritin-calcium microcapsules did not. Both kinds of Biodritin® microcapsules proved to be mechanically resistant in in vitro and in vivo studies. However, the Biodritin-calcium material was found to be more elastic while the Biodritin-barium microcapsules displayed a more plastic behavior. These properties seem to be determinant for viability of the encapsulated cell’s, since the Biodritin-calcium microcapsules presented more viable cells than the Biodritin-barium microcapsules.

Resumo em Inglês:

In austenitic stainless steels, plastic deformation can induce martensite formation. The induced martensite is related to the austenite (gamma) instability at temperatures close or below room temperature. The metastability of austenite stainless steels increases with the decreasing of stacking fault energy (SFE). In this work, the deformation induced martensite was analyzed by X ray diffraction, electron back scatter diffraction (EBSD), magnetic methods and atomic force microscope (AFM) in samples of a low SFE austenitic stainless steel, AISI 301LN and compared with a medium SFE stainless steel, AISI 316L. Both techniques, X ray diffraction and EBSD, presented similar quantities for the alpha’-martensite. Texture results indicate that the crystallographic orientation of the formed alpha’-martensite is {001}<110> and {103}<110>. The morphology of alpha’-martensite was analyzed by AFM. Corrosion tests showed that deformation reduces pitting corrosion and generalized corrosion resistance in both steels.

Resumo em Inglês:

PtRu/C electrocatalysts (carbon-supported PtRu nanoparticles) were prepared submitting water/ethylene glycol mixtures containing Pt(IV) and Ru(III) ions and the carbon support to electron beam irradiation. The electrocatalysts were characterized by energy dispersive X ray analysis (EDX), X ray diffraction (XRD) and cyclic voltammetry and tested for methanol electro-oxidation aiming fuel cell application. The obtained PtRu/C electrocatalysts showed superior performance for methanol electro-oxidation at room temperature compared to commercial PtRu/C electrocatalyst.

Resumo em Inglês:

Grain growth theories normally describe a grain using the concept of ‘grain radius’. However, this assumption bypasses all topological information relating to the grain, viz., the number of its faces, edges, etc. This study, by contrast, introduces a new methodology, treating normal and abnormal grain growth in three dimensions in terms of both metrical and topological properties of the grains.

Resumo em Inglês:

In the present work, the electrochemical behavior of WC-CoCr coatings with 10 (W10), 15 (W15) and 20 (W20) torch passes sprayed by High Velocity Oxygen-Fuel (HVOF) flame on AA7050 aluminum alloy substrate, evaluated in 3.5% NaCl solution, were compared using open-circuit potential (E OC) measurements, electrochemical impedance spectroscopy (EIS) and polarization curves. The coating surfaces and their cross sections were characterized by X ray diffraction and the Rockwell-C hardness test, and also by optical (OM) and scanning electron microscopy (SEM) before and after the corrosion tests. The electrochemical data showed that sample W10 presented higher corrosion resistance than the others in chloride solutions. In some tests, aluminum salts on the coating surface were identified by EDS, indicating the corrosion of the substrate. And using aluminon, aluminum ions were detected and analyzing the surface via stereomicroscopy, hydrogen bubbles were observed, both showing that the electrolyte reached the substrate and galvanic corrosion possibly occurred. The physical characterization showed that sample W10 presented a lower number of cracks and pores, justifying its higher corrosion resistance.

Resumo em Inglês:

A mechanical model for pseudoelastic behavior of NiTi wires is proposed with the aim to predict the behavior of Shape Memory Alloys(SMA) damping wire elements in model structures. We have considered at first a simple linearwise stress-strain relationship to describe the basic isothermal behavior of the SMA members. Then, this basic model is modified in order to include the effect of the strain rate. The model is based on detailed experimental characterization performed on a Ni rich NiTi superelastic wire which included the study of the localized character of the deformation and the local heat generation associated with the stress induced martensitic transformation occurring in these alloys. Heat conduction along the wire and heat interaction with the surroundings was also considered. In that way, the resulting local temperature field around the transformation front is assessed and its effect on the progression of the transformation is evaluated. It is shown how the simple mechanical model reproduces the global mechanical behavior, including the existence of a maximum in the damping capacity with the transformation rate.

Resumo em Inglês:

The purpose of this study was to evaluate the fracture resistance and the fracture surface of NiTi SMA engine-driven endodontics files submitted to clockwise torsion. The maximum angular deflection and the maximum torque were analyzed without axial loading. The helical plastic deformations and the fracture surface morphology were evaluated by Scanning Electron Microscopic. The results showed that there was a significant statistical difference in the maximum fracture torque and no statistical difference for the angular deflection for the analyzed files. In relation to the maximum torque at the instant of the fracture, one of the brand presented better performance than the other. According to Scanning Electron Microscopic evaluation, all the files showed ductile fracture morphology.

Resumo em Inglês:

Cerium conversion layers and silane films are among the potential substitutes for the carcinogenic chromate conversion layers used to protect high-strength Al alloys. In the present work the adhesion of a cerium conversion layer and of a silane film to an aluminium alloy (AA) 2024-T3 substrate was investigated using mechanical and electrochemical tests. Scanning electron microscopy (SEM)- X ray energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FT-IR) and X ray photoelectron spectroscopy (XPS) were used to characterize the layers prior and after the mechanical test consisting of ultrasonic rinse in deionized water during 30 minutes. Mechanically tested and untested layers were also submitted to electrochemical impedance spectroscopy (EIS) and anodic polarization measurements in 0.1 M NaCl solution. The results of the characterization tests have pointed to a stronger adhesion of the Ce layer to the substrate in comparison with the silane film, which was confirmed by the electrochemical tests. The adhesion between the silane film and the Ce conversion layer was also tested, to evaluate the possibility of using the system as a protective bi-layer in accordance with the new trends being developed to substitute chromate conversion layers.

Resumo em Inglês:

This work presents studies of modification of a natural zeolite by activation with Na+ cations and functionalisation with Ba+2 and/or Cu2+ ions (FZ). The zeolite was characterized, modified and applied in adsorption studies of sulphate and isopropilxanthate ions as flocculated and powdered forms. The reuse of SO4Ba-FZ was investigated by adsorption-removal of either Ba2+ or sulphate ions in stages. Equilibrium data showed that the FZ, flocculated or as powder, provide considerable removal of sulphate ions (q mLangmuir: 1.15 and 1.35 meq.g-1, respectively) and isopropilxanthate (q mLangmuir: 0.35 and 0.93 meq.g-1, respectively). The reuse of the SO4-FZ, either powdered or flocculated also uptake significant amount of Ba2+ or sulphate ions (q mLangmuir: 1.15 meq.g-1), providing a new alternative for the exhausted adsorbent. Thus the activated and functionalised zeolites create new options on the materials engineering area with applications in environmental applied adsorption processes.

Resumo em Inglês:

TiO2 films have various applications, among them solar cells and photodegradation of pollutants. In this study, we investigated TiO2 films functionalized with the organic dye cyanidin extracted from black mulberry (Morus nigra). The TiO2 was functionalized by the sol-gel method and the film was deposited on glass substrates by dip-coating. Our aim was to investigate the interaction between the semiconductor and the dye, as well as the influence of the velocity and number of deposits on the characteristics of the film. Using ultraviolet-visible spectroscopy, we observed a shift from the maximum absorption band at 545 nm for the dye’s ethanol solution to 595 nm for the film, indicating interaction of the cyanidin with the TiO2. The absorption spectra in the infrared region of the functionalized TiO2 particles showed bands characteristic of the oxide and indicated their interaction with the dye. Using profilometry and m-line techniques, we found that the films presented thicknesses in the order of 100 nm. A SEM analysis confirmed the high density of the films.

Resumo em Inglês:

Nowadays, synthetic diamond has been studied for its application in wastewater treatment, electroanalysis, organic synthesis and sensor areas; however, its use in the water disinfection/purification is its most relevant application. The new electrochemistry applications of diamond electrodes open new perspectives for an easy, effective, and chemical free water treatment. This article highlights and summarizes the results of a selection of papers dealing with electrochemical disinfection using synthetic diamond films.

Resumo em Inglês:

Polyaniline (PAni), an electronic conductive polymer, has poor mechanical properties, such as low tensile, compressive and flexural strength that render PAni a non-ideal material to be processed for practical applications. Desired properties of polyaniline can be enhanced by mixing it with a polymer that has good mechanical properties. In this work, PAni was synthesised using functionalized sulfonic acids like camphorsulfonic acid (CSA) and dodecilbenzene sulfonic acid (DBSA) in order to promote PAni doping and improve its solubility, making possible conductive blends manufacture. The different forms of PAni were characterized by infra-red spectroscopy, thermal analysis, scanning electron microscopy and conductivity measurements. A conductive blend composed of PAni/DBSA and lower density polyethylene (LDPE) was obtained via solubilization method and its thermal, morphological and electrical properties were investigated. Concentrations as low as 5 wt. (%) of PAni was able to lead to electrical conductivities of PAni/LDPE blends in the range of 10-3 S.cm-1, showing great potential to be used in antistatic packing, electromagnetic shielding, anti-corrosion shielding or as a semiconductor.

Resumo em Inglês:

In the present study two novel composites of Calcium phosphates (CaP) and Collagen (COL) were synthesized, hydroxyapatite/Collagen (HA/COL) and hydroxyapatite-btricalcium phosphate/COL (HAbTCP/COL). Collagen was extracted from bovine pericardium submitted to enzymatic digestion and purification by ion-exchange chromatography yielding high purity grade type I collagen. Biocomposites of HAP/COL and HAbTCP/COL were produced with a calcium phosphate/COL ratio of 80/20 (wt. (%)) and were characterized by chemical analysis, light microscopy and scanning electron microscopy, X ray diffraction and FT-infrared spectroscopy. SEM results of the CaP powders showed agglomerates of particles at the nanometric size range with predominantly columnar shape and average chemical composition of [Ca/P] = 1.67. FTIR analysis of collagen has confirmed the major vibrational bands associated with chemical groups like amides and hydroxyls usually found in proteins. SEM micrographs have indicated that both morphological and structural features and chemical composition of the composites were very similar to their precursors, collagen and calcium phosphate components. SDS-PAGE characterization results of protein extracted and purified has showed that bovine type I collagen was successfully obtained. Finally, the biocomposites presented a homogeneous aspect with the calcium phosphate particles aggregated to the collagen fibers. Hence, the novel developed biocomposites have high potential to be used for rebuilding small lesions in bone tissue engineering.

Resumo em Inglês:

Depth sensing indentation study was conducted in a Fischerscope H100V machine, equipped with a Vickers indenter with a tip roundness of approximately 1330 nm. Tests were carried out on soda-lime glass, fused silica, sapphire, aluminum (1100 alloy), high alloyed steel, titanium and copper. The widely used iterative method of Oliver and Pharr was unsuccessful in the attempts to analyze machine compliance and indenter area function. Therefore, an alternative procedure was adopted. The alternative procedure is based on the ratio between maximum load and unload stiffness squared, Pm/Su². It was found that this procedure, which is not iterative, gives good results. A careful study of the Pm/Su² ratio, lead us to conclude that the Fischercope machine has a low compliance which depends on the sample mounting. This low compliance in conjunction with the recent discovery of the dependence of beta factor on the tip roundness/maximum depth ratio, which appears in the relation between contact stiffness and contact area, explains why the iterative method does not converge. However, variations in beta and machine compliance produces deviation on the hardness and elastic modulus lower that 6% with respect to expected values for the materials and the machine studied in this work.

Resumo em Inglês:

Due to the relevance of the critical cooling rate, Rc, for glasses, Barandiarán and Colmenero (BC) developed a method for calculating Rc as a function of the crystallization temperature on cooling obtained from thermal analysis. The critical cooling rate is obtained by the extrapolation method to conditions of infinity undercooling. However, for polymers, there is a strong reason for modifying the original BC method. In this case, the extrapolation must be extended only to the undercooling associated to the glass transition temperature, Tg, because no crystallization can occur below this temperature. Following this modified method (MBC) proposed by the present authors, the critical cooling rate for PP, PEEK, P10MS and PET were determined. The results showed that the new values are much lower than those obtained by the original BC method.

Resumo em Inglês:

Wrought austenitic stainless steels are widely used in high temperature applications. This short review discusses initially the processing of this class of steels, with emphasis on solidification and hot working behavior. Following, a brief summary is made on the precipitation behavior and the numerous phases that may appear in their microstructures. Creep and oxidation resistance are, then, briefly discussed, and finalizing their performance is compared with other high temperature metallic materials.

Resumo em Inglês:

An automotive shaft was surface-remelted and hardened using a 2 kW fiber laser and an adapted linear axis whose rotating axis produced helical tracks at 120 RPM. The process variable was the laser power, ranging from 300 to 1100 W, which produced two regions in the material: a martensitic region (MR) and a partially transformed region (PTR). The MR is formed after rapid solidification or austenitization followed by rapid cooling (10(7) K.s-1). The PTR is composed of martensite, unchanged pearlite and proeutectoid ferrite. The maximum case depth was about 0.3 mm. The microhardness inside the martensitic regions are at least double that of the base material, i.e. between 800 than 600 HV compared to 300 HV. Thermal simulations using a modified Rosenthal formalism help elucidate the phase transformation inside the material and show good agreement with experimental results. The experimental laser-steel absorptivities were measured; they ranged between 38 and 59% depending on the laser power and the amount of liquid at the surface.

Resumo em Inglês:

Surfaces of pure titanium and Ti coated with cellulose acetate propionate (CAP) have been characterized by means of scanning electron microscopy X ray coupled with elemental microanalysis (SEM-EDS), ellipsometry, atomic force microscopy (AFM) and contact angle measurements. Coating Ti surfaces with CAP ultrathin films reduced original surface roughness. Surface energy and wettability of CAP covered Ti surfaces pure Ti surfaces were similar. The adsorption of lysozyme (LYZ), an antibacterial protein, onto Ti and CAP-coated Ti surfaces has been studied by means of ellipsometry and atomic force microscopy (AFM). The adsorption of LYZ was mainly driven by hydrophobic interaction between protein hydrophobic residues and CAP propyl groups. Pure Ti and CAP coated Ti surfaces presented no cytotoxicity effect and proved to be adequate substrates for cell adhesion. The biocompatibility of CAP coated Ti surfaces was attributed to the surface enrichment in glucopyranosyl residues and short alkyl side groups.