992 resultados para thermal treatments


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The purpose of this study was to evaluate the effectiveness of complementary heat treatment and water storage in reducing cytotoxicity of acrylic resins denture bases used in Brazil by the MTT assay. Material and Methods: First, nine specimens were fabricated from metal matrix in the form of discs with 14 mm in diameter and 1.2 mm of thick. Immediately after making, 24 or 48 hours after storage in distilled water, the samples of heat-polymerized resins were divided into 3 groups (n = 3) according to the type of thermal treatment: Group 1: samples were individually exposed to microwave energy (500 W for 3 minutes); Group 2: samples were immersed in water at 550 C for 60 minutes; Group 3: samples did not receive heat treatment. To prepare the extracts, 3 samples of each group were placed into vials containing 3 mL of culture medium and stored at 37°C for 24 hours. L929 cells were used and the MTT assay was performed to analyze the cellular metabolism. Two-factor analysis of variance was used to detect significant among groups at 5% significance. Results: After statistical analysis, the materials were classified according to the cytotoxic effect: non-cytotoxic, slightly cytotoxic; moderately cytotoxic; and strongly cytotoxic. The results showed that the resins ranged from moderately cytotoxic to non-cytotoxic, but no statistically significant difference among experimental groups. Furthermore, the water storage and thermal treatments reduced the cytotoxicity of the resins. Conclusions: It was concluded that the resins studied are potentially toxic and that treatments can decrease their cytotoxicity.

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Semiconductor-mediated photocatalytic oxidation is an interesting method for water decontamination and a specially modified TiO2 is said to be a promising material. This study verified that the synthesis of 1wt%Ag modified-Sc0.01Ti0.99O1.995 powder samples prepared by Polymeric Precursor Method is capable of forming a mixture of anatase-rutile phase with high photocatalytic performance. This kind of material is found to have a lower bandgap compared to the TiO2-anatase commercial powders, which can be associated to an innovative hybrid modification. The simultaneous insertion of scandium in order to generate a p-type semiconductor and a metallic silver nanophase acting as an electron trapper demonstrated being capable of enhancing the degradation of rhodamine B compared to the commercial TiO2. In spite of the different thermal treatments or phase amounts, the hybrid modified powder samples showed higher photocatalytic activity than the commercial ones.

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Pós-graduação em Ciência e Tecnologia de Materiais - FC

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The assessment of the thermal process impact in terms of food safety and quality is of great importance for process evaluation and design. This can be accomplished from the analysis of the residence time and temperature distributions coupled with the kinetics of thermal change, or from the use of a proper time-temperature integrator (TTI) as indicator of safety and quality. The objective of this work was to develop and test enzymic TTIs with rapid detection for the evaluation of continuous HTST pasteurization processes (70-85 degrees C, 10-60 s) of low-viscosity liquid foods, such as milk and juices. Enzymes peroxidase, lactoperoxidase and alkaline phosphatase in phosphate buffer were tested and activity was determined with commercial reflectometric strips. Discontinuous thermal treatments at various time-temperature combinations were performed in order to adjust a first order kinetic model of a two-component system. The measured time-temperature history was considered instead of assuming isothermal conditions. Experiments with slow heating and cooling were used to validate the adjusted model. Only the alkaline phosphatase TTI showed potential to be used for the evaluation of pasteurization processes. The choice was based on the obtained z-values of the thermostable and thermolabile fractions, on the cost and on the validation tests. (C) 2012 Elsevier Ltd. All rights reserved.

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Calcium tantalite (CaTa2O6) single crystal fibers were obtained by the laser-heated pedestal growth method (LHPG). At room temperature, this material can present three polymorphic modifications. The rapid crystallization inherent to the LHPG method produced samples within the Pm3 space group, with some chemical disorder. In order to check for polymorphic-induced transformations, the CaTa2O6 fibers have been submitted to different thermal treatments and investigated by micro-Raman spectroscopy. For short annealing times (15 min) at 1200 °C, the cubic modification was maintained, though with an improved crystalline quality, as evidenced by the enhanced inelastic scattered intensity (by ca. 250%) and narrowing of Raman bands. The polarized Raman spectra respected very well the predicted symmetries and the selection rules for this cubic modification. On the other hand, long annealing times (24 h) at 1200 °C led to a complete (irreversible) polymorphic transformation. The Raman bands became still more intense (ca. 15 times larger than for the as-grown fibers), narrower, and several new modes appeared. Also, the spectra became unpolarized, demonstrating a polycrystalline nature of the transformed crystals. The observed Raman modes could be fully assigned to an orthorhombic modification of CaTa2O6 belonging to the Pnma space group.

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This work reports on the construction and spectroscopic analyses of optical micro-cavities (OMCs) that efficiently emit at ~1535 nm. The emission wavelength matches the third transmission window of commercial optical fibers and the OMCs were entirely based on silicon. The sputtering deposition method was adopted in the preparation of the OMCs, which comprised two Bragg reflectors and one spacer layer made of either Er- or ErYb-doped amorphous silicon nitride. The luminescence signal extracted from the OMCs originated from the 4I13/2→4I15/2 transition (due to Er3+ ions) and its intensity showed to be highly dependent on the presence of Yb3+ ions.According to the results, the Er3+-related light emission was improved by a factor of 48 when combined with Yb3+ ions and inserted in the spacer layer of the OMC. The results also showed the effectiveness of the present experimental approach in producing Si-based light-emitting structures in which the main characteristics are: (a) compatibility with the actual microelectronics industry, (b) the deposition of optical quality layers with accurate composition control, and (c) no need of uncommon elements-compounds nor extensive thermal treatments. Along with the fundamental characteristics of the OMCs, this work also discusses the impact of the Er3+-Yb3+ ion interaction on the emission intensity as well as the potential of the present findings.

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In order to improve the animal welfare, the Council Directive 1999/74/EC (defining minimum standards for the welfare of laying hens) will ban conventional cage systems since 2012, in favour of enriched cages or floor systems. As a consequence an increased risk of bacterial contamination of eggshell is expected (EFSA, 2005). Furthermore egg-associated salmonellosis is an important public health problem throughout the world (Roberts et al., 1994). In this regard the introduction of efficient measures to reduce eggshell contamination by S. Enteritidis or other bacterial pathogens, and thus to prevent any potential or additional food safety risk for Human health, may be envisaged. The hot air pasteurization can be a viable alternative for the decontamination of the surface of the egg shell. Few studies have been performed on the decontamination power of this technique on table eggs (Hou et al, 1996; James et al., 2002). The aim of this study was to develop innovative techniques to remove surface contamination of shell eggs by hot air under natural or forced convection. Initially two simplified finite element models describing the thermal interaction between the air and egg were developed, respectively for the natural and forced convection. The numerical models were validated using an egg simulant equipped by type-K thermocouple (Chromel/Alumel). Once validated, the models allowed the selection of a thermal cycle with an inner temperature always lower than 55°C. Subsequently a specific apparatus composed by two hot air generators, one cold air generator and rolling cylinder support, was built to physically condition the eggs. The decontamination power of the thermal treatments was evaluated on shell eggs experimentally inoculated with either Salmonella Enteritidis, Escherichia coli, Listeria monocytogenes and on shell eggs containing only the indigenous microflora. The applicability of treatments was further evaluated by comparing quality traits of treated and not treated eggs immediately after the treatment and after 28 days of storage at 20°C. The results showed that the treatment characterized by two shots of hot air at 350°C for 8 sec, spaced by a cooling interval of 32 (forced convection), reduce the bacterial population of more than 90% (Salmonella enteritidis and Listeria monocytogenes). No statistically significant results were obtained comparing E. coli treated and not treated eggs as well as indigenous microflora treated and not treated eggs. A reduction of 2.6 log was observed on Salmonella enteritidis load of eggs immediately after the treatment in oven at 200°C for 200 minutes (natural convection). Furthermore no detrimental effects on quality traits of treated eggs were recorded. These results support the hot air techniques for the surface decontamination of table eggs as an effective industrial process.

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Lo scopo di questa tesi è stato la produzione di un elettrolizzatore ad ossidi solidi (SOEC) mediante tecniche economiche e facilmente industrializzabili. Fondamentale a questo scopo è stata la realizzazione di una semicella costituita da un anodo poroso a base di La0.8Sr0.2MnO3-Ce0.8Gd0.2O2-δ (LSM-GDC) ed un elettrolita denso a base di Ce0.8Gd0.2O2-δ (GDC). Le tecniche utilizzate per la produzione di questo sistema sono state il colaggio su nastro e la serigrafia. Anche se generalmente, le celle SOEC vengono prodotte catodo supportate, in questo studio, l’elemento supportante scelto è stato l’anodo poiché questo garantisce una migliore stabilità meccanica all’intera cella. Tale substrato è stato ottenuto mediante colaggio su nastro accoppiato con un metodo innovativo di sinterizzazione denominato sinterizzazione reattiva, processo che prevede la formazione della fase di interesse durante un unico trattamento termico di eliminazione degli additivi organici e consolidamento del manufatto finale. La membrana elettrolitica per l’ottenimento del bilayer anodo-elettrolita, è stata prodotta mediante sia serigrafia che colaggio su nastro. L’accurato studio dell’evoluzione di fase della polvere anodica, l’ottimizzazione della sospensione per colaggio su nastro e dei trattamenti termici hanno permesso l’ottenimento di anodi (fino a dimensioni di 10x10 cm2). Lo studio dei profili di sinterizzazione delle polveri anodica ed elettrolitica e dell’influenza della tecnica di formatura sulla sinterabilità dei layer elettrolitici prodotti hanno inoltre permesso l’ottenimento di una semicella planare costituita da un elettrodo poroso ed una membrana elettrolitica densa adatte per applicazioni SOEC.

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Several CFCC (Continuous Fiber Composite Ceramics) production processes were tested, concluding that PIP (Polymer Impregnation, or Infiltration, Pyrolysis) and CBC (Chemically Bonded Ceramics) based procedures have interesting potential applications in the construction and transportation fields, thanks to low costs to get potentially useful thermomechanical performances. Among the different processes considered during the Doctorate (from the synthesis of new preceramic polymers, to the PIP production of SiC / SiC composites) the more promising results came from the PIP process with poly-siloxanes on basalt fabrics preforms. Low processing time and costs, together with fairly good thermomechanical properties were demonstrated, even after only one or two PIP steps in nitrogen flow. In alternative, pyrolysis in vacuum was also tested, a procedure still not discussed in literature, but which could originate an interesting reduction of production costs, with only a moderate detrimental effect on the mechanical properties. The resulting CFCC is a basalt / SiCO composite that can be applied for continuous operation up to 600°C, also in oxidant environment, as TG and XRD demonstrated. The failure upon loading is generally pseudo-plastic, being interlaminar delamination the most probable rupture mechanism. . The strength depends on several different factors (microstructure, polymer curing and subsequent ceramic phase evolution, fiber pull-out, fiber strength, fiber percentage) and can only be optimized empirically. In order to be open minded in selecting the best technology, also CBC (Chemically Bonded Ceramics) matrixes were considered during this Doctorate, making some preliminary investigations on fire-resistant phosphate cements. Our results on a commercial product evidenced some interesting thermomechanical capabilities, even after thermal treatments. However the experiments showed also phase change and possible cracking and deformations even on slow drying (at 130°C) and easy rehydration upon exposure to environmental humidity.

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Minor components are of particular interest due to their antioxidant and biological properties. Various classes of lipophilic minor components (plant sterols (PS) and α-tocopherol) were selected as they are widely used in the food industry. A Fast GC-MS method for PS analysis in functional dairy products was set up. The analytical performance and significant reduction of the analysis time and consumables, demonstrated that Fast GC-MS could be suitable for the PS analysis in functional dairy products. Due to their chemical structure, PS can undergo oxidation, which could be greatly impacted by matrix nature/composition and thermal treatments. The oxidative stability of PS during microwave heating was evaluated. Two different model systems (PS alone and in combination) were heated up to 30 min at 1000 W. PS degraded faster when they were alone than in presence of TAG. The extent of PS degradation depends on both heating time and the surrounding medium, which can impact the quality and safety of the food product destined to microwave heating/cooking. Many minor lipid components are included in emulsion systems and can affect the rate of lipid oxidation. The oxidative stability of oil-in-water (O/W) emulsions containing PS esters, ω-3 FA and phenolic compounds, were evaluated after a 14-day storage at room temperature. Due to their surface active character, PS could be particularly prone to oxidation when they are incorporated in emulsions, as they are more exposed to water-soluble prooxidants. Finally, some minor lipophilic components may increase oxidative stability of food systems due to their antioxidant activity. á-tocopherol partitioning and antioxidant activity was determined in the presence of excess SDS in stripped soybean O/W emulsions. Results showed that surfactant micelles could play a key role as an antioxidant carrier, by potentially increasing the accessibility of hydrophobic antioxidant to the interface.

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On the basis of studies of Holocene samples,submarine basaltic glass (SBG) is thought to be an ideal paleointensity recorder because it contains unaltered single domain magnetic inclusions that yield Thellier paleointensity data of exceptional quality. To be useful as a recorder of the long-term geomagnetic field, older SBG must retain these optimal properties. Here, we examine this issue through rock magnetic and transmission electron microscope (TEM) analyses of Cretaceous SBG recovered at Ocean Drilling Program Site 1203 (northwestern Pacific Ocean). These SBG samples have very low natural remanent magnetization intensities (NRM <50 nAm**2/g) and TEM analyses indicate a correspondingly low concentration of crystalline inclusions. Thellier experiments on samples with the strongest NRM intensity (>5*10**-11 Am**2) show a rapid acquisition of thermoremanent magnetization (TRM) with respect to NRM demagnetization. Taken at face value,this behavior implies magnetization in a very weak (617 WT) ambient field. But monitoring of magnetic hysteresis properties during the Thellier experiments (on subsamples of the SBG samples used for paleointensity determinations) indicates systematic variations in values over the same temperature range where the rapid TRM acquisition is observed. A similar change in properties during heating is observed on monitor SBG specimens using low-temperature data: with progressive heatings the Verwey transition becomes more distinct. We suggest that these experimental data record the partial melting and neocrystallization of magnetic grains in SBG during the thermal treatments required by the Thellier method,resulting in paleointensity values biased to low values. We further propose that this process is pronounced in Cretaceous and Jurassic SBG (relative to Holocene SBG) because devitrification on geologic time scales (i.e., tens of millions of years) lowers the transition temperature at which the neocrystallization can commence. Magnetic hysteresis monitoring may provide a straightforward means of detecting the formation of new magnetic inclusions in SBG during Thellier experiments.

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TbxFe1−x thin films deposited by sputtering on Mo were investigated structurally and magnetically. The microstructure consists of TbFe2 nanoparticles embedded in an amorphous matrix, and the Tb content can be correlated with an increase in the volume of these nanoparticles. Similar microstructure and behavior were found when TbFe2 was deposited on glass and on a Pt buffer layer. Nevertheless, thermal treatments promote a different effect, depending on the mechanical stiffness of the buffer layer. The layers deposited on Mo, a rigid material, show crystalline TbFe2 together with α-Tb phase upon thermal treatment. In contrast, TbFe2 does not crystallize properly on Pt, a material with a lower stiffness than Mo. Intermediate results were observed on the film deposited on glass. Experimental results show the impact of the buffer stiffness on the crystallization process. Moreover, the formation of α-Tb appears to be fundamental to crystallized TbFe2 on layers deposited on rigid buffers

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We have analyzed the structural and magnetic properties of as-grown and annealed [TbFe2/Fe3Ga]n heterostructures grown by sputtering. Evidence of the bcc structure in the Fe3Ga layers has been found. The diffraction peak related to this structure shifts to high angles with the annealing temperature. Also, we have observed a change in the microstructure of the Tb-Fe layers when the thickness layer is reduced in the as-grown heterostructures. Moreover, the Tb content is lower than 33% of the TbFe2 Laves phase and it depends on the layer thickness. The thermal treatments promote the increase of the Tb content, but only in the heterostructures with thick layers. The strong lattice mismatch between the Tb-Fe and Fe-Ga layers seems to prevent a complete Tb diffusion upon the annealing process. Thus, the crystallization of the TbFe2 Laves phase is inhibited in the heterostructures with thin layers, although our experimental results indicate the presence of potential magnetostrictive TbFeGa alloys