Abstract in English:

This work describes the hydrolytic sol-gel synthesis of silica particles prepared by a modified Stöber route, using the organofunctionalized alkoxide 3-methacryloxypropyl trimethoxysilane and tetraethylorthosilicate. The silica particles were obtained through basic catalysis from a mixture of precursor alkoxides, water, and isopropyl alcohol. Samples were prepared with change to the pre-hydrolysis and condensation time of tetraethylortosilicate, followed by addition of the organosilane 3-methacryloxypropyl trimethoxysilane. Eu3+ ions were added to the alkoxides mixture, in order to obtain structural information about the silica particles. The samples were centrifuged, washed with ethanol, and dried at 50 ºC. The xerogel was analyzed by thermogravimetric analysis, photoluminescence, transmission electron microscopy, and infrared spectroscopy. The photoluminescence spectra revealed Eu3+ lines characteristic of the ion 5D0 <img src="/img/revistas/mr/2011nahead/aop_0408-10_set.jpg" alt="" align="absmiddle"> 7F J (J = 0, 1, 2, 3, 4) transition. The thermogravimetric curve and infrared spectra confirmed the presence of the alkoxide organic group and water in the materials. Transmission electron microscopy showed spherical particles with varied size. The time of pre-hydrolysis and condensation as well as the addition of 3-methacryloxypropyl trimethoxysilane affect the final shape and size of the materials, so they can be used as control factors.

Abstract in English:

Kinetic studies for the non-isothermal decomposition of un-irradiated and γ-irradiated indium acetyl acetonate In(acac)3 with 10² kGy total γ-ray dose were carried out in static air. The results showed that the decomposition proceeds in one major step in the temperature range of 150-250 °C with the formation of In2O3 as solid residue. The non-isothermal data for un-irradiated and γ-irradiated In(acac)3 were analysed using linear Flynn-Wall-Ozawa (FWO) and nonlinear Vyazovkin (VYZ) iso-conversional methods. The results of application of these free models on the investigated data showed a systematic dependence of Ea on α indicating a simple decomposition process. No significant changes were observed in both decomposition behaviour and (Eα-α) dependency between unirradiated and γ-irradiated In(acac)3. Calcination of In(acac)3 at 400 °C for 5 hours led to the formation of In2O3 monodispersed nanoparticles. X-ray diffraction, FTIR and SEM techniques were employed for characterization of the synthesised nanoparticles. This is the first attempt to prepare In2O3 nanoparticles by solid state thermal decomposition of In(acac)3.

Abstract in English:

This study compared the effect of two bioceramics on the process of bone repair: α-tricalcium phosphate (α-TCP) cement and β-tricalcium phosphate hydroxyapatite particles (β-TCP/HA). Calvarial defects were created in 50 rats, divided into two groups (α and β/HA). Software was used at 7, 21, 60, 90 and 120 days to assess bone formation. Mean new bone formation rates were as follows: α group, 1.6% at 7 days, 5.24% at 21 days, 24% at 60 days, 30.21% at 90 days and 50.59% at 120 days; β/HA group, 1.94% at 7 days, 2.53% at 21 days, 12.47% at 60 days, 26.84% at 90 days and 38.82% at 120 days; control group, 0.15% at 7 days, 10.12% at 21 days, 15.10% at 60 days, 18.94% at 90 days, 48.50% at 120 days. Both materials are osteoconductive and biocompatible. Perhaps the larger rate of new bone formation observed in the α-TCP group, it also occurs in the β-TCP/HA group within a longer time period.

Abstract in English:

A simple and cost effective chemical technique has been utilized to grow cadmium sulphide (CdS) nanoparticles at room temperature. The sample is characterized with XRD (X-ray diffractometer), SEM (Scanning electron microscope), TEM (Transmission electron microscope) and UV-VIS spectrophotometer. The particle size estimated using X-ray line broadening method is approximately 5 nm. Instrumental broadening was taken into account while particle size estimation. The lattice strain was evaluated using Williamson-Hall equation. SEM illustrates formation of sub-micron size crystallites and TEM image gives particle size approximately between 4-5 nm. Optical absorption study exhibits a band gap energy value of about 2.6 eV.

Abstract in English:

Ceramic seeds were synthesized by the sol-gel technique with Si:Sm:Ca. One sample was irradiated in the TRIGA nuclear reactor IPR-R1. After irradiation, the seeds were submitted to instrumental neutron activation analysis to determine the 153Sm concentration in weight. The same irradiated seed sample was submitted to gamma spectrometry analysis to determine all existing radionuclides as well as its individual activities. A second sample was submitted to ICP-AES atomic emission spectrometry. A third sample was submitted to X-ray fluorescence spectrometry to determine qualitative chemical composition. The measured activity was due to 153Sm with a well-characterized gamma spectrum. The X-ray fluorescence spectrum demonstrates that there is no discrepancy in seed composition. Maximum range of beta particles from 153Sm were evaluated, as well as the total dose and dose rate on its range´s volume. The results are relevant for investigation of the viability of producing 153Sm radioactive seeds for use in brachytherapy.

Abstract in English:

Coralina® HAP-200 (coralline hydroxyapatite obtained by hydrothermal treatment of marine corals) and POVIAC® (polymeric matrix based on PVAc), commercial trade marks were mixed with a natural product from the Cuban sea costs, i.e. calcium carbonate from Porites Porites coral, to obtain a novel bioactive composite with potential use as bone restoration material. The samples were characterized by physical-chemical (FTIR, XRD, SEM, EDS) and mechanical studies. It was shown that there is no chemical interaction between the inorganic filler and the polymer matrix, each conserving the original properties of the raw materials. The studied formulation had a compressive strength similar to that reported for trabecular bone. Scanning electron microscopy examination revealed that the addition of CaCO3 induces a change on the morphologic structure of the composite obtained after 30 days of SBF immersion. These composites generate novel biomaterials capable of promoting the deposition of a new phase, a Ca-P layer due to the bioactivity of a Ca2+ precursors.

Abstract in English:

This paper reports a research programme aimed at giving a better understanding of the phenomena involved in the chloride penetration in cement-based materials. The general approach used was to solve the Nernst-Planck equation numerically for two physical ideal states that define the possible conditions under which chlorides will move through concrete. These conditions are named in this paper as voltage control and current control. For each condition, experiments and simulations were carried out in order to establish the importance of electrical variables such as voltage and current in modelling chloride transport in concrete. The results of experiments and simulations showed that if those electrical variables are included as key parameters in the modelling of chloride penetration through concrete, a better understanding of this complex phenomenon can be obtained.

Abstract in English:

Starch consolidation casting has been successfully used to produce porous ceramics with complex shapes at a relatively low producing cost. In this work, porous 3Y-ZrO2 ceramics were produced using two types of starch (corn and potato). Concentrated (50-52 vol. (%)) aqueous suspensions of the different 3Y-ZrO2-starch mixtures (i.e. starch to zirconia weight ratios between 0.20 and 0.52) were thermally consolidated and the effect of the type and amount of added starch on properties of resultant dried product was examined. After starch granules burnout, the effect of sintering temperature varying between 1000 and 1500 ºC on the porosity evolution, interconnection and morphology of pores and microstructure of final ceramic was followed by water absorption measurements, Hg porosimetry and scanning electron microscopy SEM. Typical microstructure of the ceramic sintered at 1500 ºC consisted of large nearly spherical pores (created by starch) uniformly distributed in a dense ZrO2 matrix. As the content of starch in the dried product (expressed as volume fraction) Xst is increased from 0.23 to 0.65, porosity of the ceramic sintered at 1500 ºC increased from 38 to 52 vol. (%) for corn starch, while it achieved 50 to 54 vol. (%) for potato starch; thus, lower Xst of potato starch developed a porous zirconia with higher porosity. In this case, the pore structure contained pores having sizes above 50 µm and resulted completely interconnected while for those prepared using corn starch the pore interconnection occurred for Xst above 0.50.

Abstract in English:

The objective of this work was to compare the fracture energy of mortar and concretes produced with crushed rock and pebble aggregates using zero, 10, 20, 30 and 40% of aggregates mixed with standard mortar and applying the wedge splitting method to achieve stable crack propagation. The samples were cast in a special mold and cured for 28 days, after which they were subjected to crack propagation tests by the wedge splitting method to determine the fracture energies of the mortar and concrete. The concretes showed higher fracture energy than the mortar, and the concretes containing crushed rock showed higher resistance to crack propagation than all the compositions containing pebbles. The fracture energy varied from 38 to 55 J.m-2. A comparison of the number of aggregates that separated from the two concrete matrices with the highest fracture energies indicated that the concrete containing pebbles crumbled more easily and was therefore less resistant to crack propagation.

Abstract in English:

Timber-concrete composite structures work appropriately when a suitable connection system is included because the degree of interaction between the materials stiffs the structural system. Thereby, it is extremely important to improve the knowledge about their connection system. The purpose of this paper is to show the results obtained by experimental investigation into push-out shear tests of glulam-concrete specimens. The specimens were designed to simulate the behaviour of composite T beams and the connection system was constituted by steel hooks - got by the division of steel bars used in reinforced concrete members - and by perforated steel plates, both glued with epoxy adhesive. They were tested under shear forces with constant loading rate. Six specimens of each group were made, considering two different diameters for the hooks (8 and 10 mm) and 4.75 mm thick perforated steel plates. The stiffness reached by steel hooks confirms their suitability for the use in composite timber-concrete systems.

Abstract in English:

Red mud, the main waste generated in aluminum and alumina production by the Bayer process, is considered hazardous due to its high pH, according to the Brazilian standard NBR 10004/2004, and worldwide generation of this waste exceeds 117 million tons/year. In this work, non-calcined red mud was used, thus requiring less energy and time and reducing costs, which is the ideal condition for reusing wastes. Mortars containing 30 wt. (%) of cement substituted by red mud showed higher strength of hardened products. The pozzolanic activity index was evaluated based on physical and mechanical parameters (Brazilian NBR 5751 and NBR 5752 standards) and on a chemical analysis (European EN 196-5 standard). A comparison of the reference mixture (without red mud) and the results obtained with red mud confirm the potential of non-calcined red mud for use a as pozzolanic additive in cementitious materials. The setting time (according to the MERCOSUL NM 65 standard) tends to increase but workability remains almost unchanged.

Abstract in English:

Natural fiber reinforced plastics (NFRP) have awakened considerable interest in the area of polymer composites, because of the need to develop new, environmentally friendly materials. One of the most complex ways of manufacturing this type of material is in the form of ultrathin laminar layers; however, this process hinders mechanical testing, mainly three and four-point bending. The present investigation faces this challenge and shows the influence of parameters, such as the grammage of reinforcing fabric and lamination process, on strength, stiffness and fracture characteristics for three-point bending in this type of structural element. The industrially manufactured laminas were composed of orthophthalic polyester resin reinforced with licuri fibers. Macromechanical and micromechanical analyses were conducted in the study of fracture characteristics for all the parameters. The mechanical behavior in the three-point bending of the laminar composite showed that the use of licuri fiber to obtain natural fiber-based plastic is completely viable.

Abstract in English:

A model based on transport equations was numerically implemented by the finite volume method (FVM) in a computational code in order to simulate the influence of the heat input, base metal thickness and preheating temperature on the thermal evolution and the cooling rate during the welding of the low alloy ferritic steels T/P23 and T/P24. As a consequence, it was possible to evaluate qualitatively the microstructure at the heat affected zone (HAZ) of these steels when a single weld bead was deposited on their surface and calculate the maximum hardness reached at this region. Goldakfs double-ellipsoid heat source model for power density distribution was utilized in order to obtain a good estimate of the cooling rate and dimensions of the fusion zone (FZ). The results are discussed in light of previous work and good agreement between experimental and simulated results was verified.

Abstract in English:

Polycrystalline strontium-doped lanthanum manganite (LSM) powders with 0.15, 0.22, and 0.30 mol % Sr were synthesized by the polymeric precursor route using a molar ratio of 3:1 citric acid and metal cations. The powders were characterized by Fourier transform infrared spectroscopy, thermal analysis, high-temperature X-ray diffraction to determine the crystalline perovskite phase and crystallite sizes, scanning electron microscopy for the morphological analysis, nitrogen adsorption to determine the specific surface area, and laser scattering to evaluate the particle size distribution. The LSM perovskite-type oxides containing intermediate 0.22 mol % Sr were found to exhibit a tendency to decrease in crystallite size and increase in specific surface area and, when calcined at 700-900 ºC exhibited a pure phase of perovskite, had a crystallite size of about 17-20 nm and a specific surface area for 900 ºC of 34.3 m².g-1.

Abstract in English:

This work reviews issues and advances a formalism for quantitative interpretation of martensite microstructure, heeding the influence of transformation uniformity and the interaction of martensite with its surroundings. The relationship of volume fraction and number density of martensite units required for kinetics analysis is derived. Additionally we apply the new model to obtain the microstructural path function (MPF) of martensite, and to analyze the autocatalytic spread of the transformation during the martensite burst in Fe-31 wt. (%) Ni-0.02 wt. (%) C. The growth of an autocatalytic spread event relates to the chemical driving force, whereas the number of such events relates to the probability of finding a nucleation site to initiate the reaction.

Abstract in English:

The direct three-dimensional characterization of opaque materials through serial sectioning makes possible to visualize and better quantify a material microstructure, using classical metallographic techniques coupled with computer-aided reconstruction. Titanium alloys are used as biomaterials for bone implants because of its excellent mechanical properties, biocompatibility and enhanced corrosion resistance. The Ti-6Al-4V alloy (in wt. (%)) with porous microstructure permits the ingrowths of new-bone tissues improving the fixation bone/implant. This is important to understand connectivity, morphology and spatial distribution of pores in microstructure. The Ti-6Al-4V alloy compacts were produced by powder metallurgy and sintered at three distinct temperatures (1250, 1400 and 1500 °C) to obtain distinct microstructures in terms of residual porosity. The visualization of the reconstructed 3D microstructure provides a qualitative and quantitative analysis of the porosity of Ti6Al4V alloy (volume fraction and pore morphology).

Abstract in English:

With the increase in life expectancy, biomaterials have become an increasingly important focus of research because they are used to replace parts and functions of the human body, thus contributing to improved quality of life. In the development of new biomaterials, the Ti-15Mo alloy is particularly significant. In this study, the Ti-15Mo alloy was produced using an arc-melting furnace and then characterized by density, X-ray diffraction, optical microscopy, hardness and dynamic elasticity modulus measurements, and cytotoxicity tests. The microstructure was obtained with β predominance. Microhardness, elasticity modulus, and cytotoxicity testing results showed that this material has great potential for use as biomaterial, mainly in orthopedic applications.

Abstract in English:

Tin dioxide (SnO2) thin films are deposited by the dip-coating technique from colloidal suspensions prepared with distinct pH through the sol-gel method. The decrease of the pH contributes to the destruction of an electrical layer adjacent to particles in solution, leading to a high degree of aggregation among these particles due to the generation of cross-linked bonds (Sn-O-Sn) between them. The aggregation affects the electrical properties of films, because the pH variation produces particle with distinct sizes in the film. Undoped samples prepared from pH 6 leads to the highest conductivity among the investigated undoped samples, in agreement with X-ray diffractograms, which indicate higher crystallinity for lower pH. Arrhenius plot evaluated from temperature dependent conductivity data leads to activation energies of the deepest level between 67 to 140 meV, for the films prepared from suspensions with pH 6 to 11. The most probable explanation for this variation in the conductivity and activation energy is related to distinct potential barriers between grains, due to distinct packing caused by cross-linked bonds formed during suspension phase. Characterization of samples lightly doped with Er3+ confirms that acid pH leads to higher conductivity, but the highest conduction takes place at even lower pH when compared to undoped thin films.

Abstract in English:

Steatite is a mineral which has been employed in the carving of elements in facades of Brazilian historical buildings and churches since the 17th century. Over the years, many of those historical buildings suffered the consequences of weathering with a current need for restoration. Recently a special cement-based mortar containing additions of fine powder waste from mineral extraction of steatite has been developed in Brazil, as a composite material for restoration of steatite elements. However, the incorporation of steatite waste reduces the flexural strength of the mortar and compromises the restoration of elements where gravity imposes tensile stresses. The addition of carbon fibres may overcome this issue and increase the flexural strength of the cement-steatite composite mortar. This work investigates the effect of carbon fibre addition on the bulk density and flexural strength of compacted precast cement-steatite composites. The results show that the addition of carbon fibres (i) effectively increases the mechanical strength, allowing for a higher amount of steatite powder waste in the mixes; (ii) reduces the weight of the structural elements. This new composite material would help to develop restoration techniques of historical buildings and serve as a disposal route of steatite powder waste in Brazil.

Abstract in English:

The grain refining technique of AZ91D magnesium alloy by MgCO3 has been investigated. The refining mechanism and tensile properties of the resulting alloy have also been discussed. The results indicate that MgCO3 can decrease its grain size from 311 to 53µm. Correspondingly, the tensile properties are obviously improved. The higher the cooling rate from addition temperature to pouring temperature or the higher the addition temperature, the finer the grains. The melt treated by MgCO3 should be poured as soon as possible because the inoculation fading is quite quick. The microstructure sensitivity to the diameter of a cast rod is relatively high and the microstructures of the rods with large diameters are quite inhomogeneous. The refining mechanism of MgCO3 belongs to heterogeneous nucleation and the nucleant substrates are believed to be the Al4C3 particles formed from the reactions between the MgCO3 and the molten alloy.