55 resultados para Thermal Microscopy

em Repositório Institucional UNESP - Universidade Estadual Paulista "Julio de Mesquita Filho"


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Thermogravimetry (TG), differential scanning calorimetry (DSC), polarized light thermal microscopy (PLTM), as well as X-ray powder diffraction (XRD) and Fourier transformed infrared spectroscopy (FTIR) were used to study the thermal behavior and the chemical structure of cimetidine, famotidine, ranitidine-HCl, and nizatidine. The TG-DSC curves show that the famotidine and ranitidine-HCl suffer decomposition during melting and they are thermally less stable in comparison with cimetidine and nizatidine, the latter being the most stable of all the drugs studied in this study. The DSC curves of famotidine and ranitidine-HCl show exothermic peaks immediately after the melting, confirming the occurrence of thermal decomposition. The DSC curves also show that the cimetidine and nizatidine have some thermal stability after melting. The thermal events shown in the PLTM images are consistent with the results shown in the TG-DSC and DSC curves. The XRD patterns show that the cimetidine and famotidine are less crystalline compared with ranitidine-HCl and nizatidine. The theoretical FTIR bands are in agreement with those obtained experimentally, and in some cases, no difference is observed between the theoretical and experimental values, even being identical in one of the cases. © 2012 Akadémiai Kiadó, Budapest, Hungary.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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In this work, cellulose nanofibers were extracted from banana fibers via a steam explosion technique. The chemical composition, morphology and thermal properties of the nanofibers were characterized to investigate their suitability for use in bio-based composite material applications. Chemical characterization of the banana fibers confirmed that the cellulose content was increased from 64% to 95% due to the application of alkali and acid treatments. Assessment of fiber chemical composition before and after chemical treatment showed evidence for the removal of non-cellulosic constituents such as hemicelluloses and lignin that occurred during steam explosion, bleaching and acid treatments. Surface morphological studies using SEM and AFM revealed that there was a reduction in fiber diameter during steam explosion followed by acid treatments. Percentage yield and aspect ratio of the nanofiber obtained by this technique is found to be very high in comparison with other conventional methods. TGA and DSC results showed that the developed nanofibers exhibit enhanced thermal properties over the untreated fibers. (C) 2010 Elsevier Ltd. All rights reserved.

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It is known that chromium electroplating is related to the reduction in the fatigue strength of base metal. However, chromium results in protection against wear and corrosion combined with chemical resistance and good lubricity. Environmental requirements are an important point to be considered in the search for possible alternatives to hard chrome plating. Aircraft landing gear manufactures are considering WC thermal spray coating applied by the high-velocity oxygen-fuel (HVOF) process an alternative candidate, which shows performance at least comparable to results, obtained for hard chrome plating. The aim of this study is to compare the influence of WC-17Co and WC-10Co-4Cr coatings applied by HVOF process and hard chromium electroplating on the fatigue strength of AISI 4340 steel, with and without shot peening. S-N curves were obtained in axial fatigue test for base material, chromium plated and tungsten carbide coated specimens. Tungsten carbide thermal spray coating results in higher fatigue strength when compared to hard chromium electroplated. Shot peening prior to thermal spraying showed to be an excellent alternative to increase fatigue strength of AISI 4340 steel. Experimental data showed higher axial fatigue and corrosion resistance in salt fog exposure for samples WC-10Co-4Cr HVOF coated when compared with WC-17Co. Fracture surface analysis by scanning electron microscopy (SEM) indicated the existence of a uniform coverage of nearly all substrates. (C) 2004 Elsevier B.V. All rights reserved.

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

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Currently, high-strength materials, particularly AISI 4340 steel, are used in several landing gear components. Due to the high resistance to wear and corrosion required, the components are usually coating by hard chromium. This treatment produces waste, such as Cr+ 6 (hexavalent chromium), generally after applying the coating of hard chromium which is harmful to health and the environment. The process HVOF (High-velocity-oxygen-fuel) is considered a promising technique for deposition of hard chromium alternative coatings, for example, coatings based on tungsten carbide. This technique provides high hardness and good wear strength and more resistance to fatigue when compared to AISI 4340 hard chromium coated. To minimize loss fatigue due to the process of deposition, shot peening is used to obtain a compressive residual stress. The aim of this study was to analyze the effects of the tungsten carbide thermal spray coating applied by the HVOF, in comparison to the conventional hard chromium electroplating on the AISI 4340 high strength steel behavior in fatigue. Optical microscopy and scanning electron microscopy were used to observe crack origin sites, thickness and adhesion of the coating. (C) 2010 Published by Elsevier Ltd.

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The present work studied the influence of thermal treatment in oxygen rich atmosphere on heterogenous junctions in Mn-doped SnO2 polycrystalline system presenting varistor behavior. The samples were prepared by conventional oxide mixture methodology, and were submitted to heat treatment in oxygen rich atmosphere at 900 degrees C for 2h. The samples were characterized by X-ray diffraction, scanning electron microscopy, dc and ac electrical measurements. The results showed that there is an evident relationship between the microstructure heterogeneity and non-ohmic electrical properties. It was found that for this SnO2 center dot MnO-based varistor system the heat treatment in oxygen rich atmosphere does not necessarily increase the varistors properties, which was related to the decrease in the grain boundary resistance. The results are compared with Co-doped SnO2 varistors and ZnO based varistors. (C) 2008 WILEY-VCH Verlay GmbH & Co. KGaA, Weinheim.

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Cellulose nanowhiskers were prepared by sulfuric acid hydrolysis from coconut husk fibers which had previously been submitted to a delignification process. The effects of preparation conditions on the thermal and morphological behavior of the nanocrystals were investigated. Cellulose nanowhisker suspensions were characterized by Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), thermogravimetric analysis (TGA) and X-ray diffraction. Results showed that it was possible to obtain ultrathin cellulose nanowhiskers with diameters as low as 5 nm and aspect ratio of up to 60. A possible correlation between preparation conditions and particle size was not observed. Higher residual lignin content was found to increase thermal stability indicating that by controlling reaction conditions one can tailor the thermal properties of the nanowhiskers. Published by Elsevier Ltd.

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Background: the aim of the present study was to compare the effects of Er:YAG and diode laser treatments of the root surface on intrapulpal temperature after scaling and root planing with hand instruments.Methods: Fifteen extracted single-rooted teeth were scaled and root planed with hand instruments. The teeth were divided into 3 groups of 5 each and irradiated on their buccal and lingual surfaces: group A: Er:YAG laser, 2.94 mum/100 mJ/10 Hz/ 30 seconds; group B: diode laser, 810 nm/1.0 W/0.05 ms/30 seconds; group C: diode laser, 810 nm/1.4 W/0.05 ms/30 seconds. The temperature was monitored by means of a type T thermocouple (copper-constantan) positioned in the pulp chamber to assess pulpal temperature during and before irradiation. Afterwards, the specimens were longitudinally sectioned, and the buccal and lingual surfaces of each root were analyzed by scanning electron microscopy.Results: In the Er:YAG laser group, the thermal analysis revealed an average temperature of -2.2 +/- 1.5degreesC, while in the diode laser groups, temperatures were 1.6 +/- 0.8degreesC at 1.0 W and 3.3 +/- 1.0degreesC at 1.4 W. Electronic micrographs revealed that there were no significant morphological changes, such as charring, melting, or fusion, in any group, although the specimens were found to be more irregular in the Er:YAG laser group.Conclusions: the application of Er:YAG and diode lasers at the utilized parameters did not induce high pulpal temperatures. Root surface irregularities were more pronounced after irradiation with an Er:YAG laser than with a diode laser.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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The thermal behavior of Cu-Al alloys with 17, 19 and 21 at.%Al was examined by differential thermal analysis (DTA), differential scanning calorimetry (DSC), X-ray diffractometry (XRD), optical microscopy (OM) and scanning electron microscopy (SEM). The presence of the gamma phase (Al4Cu9) was clearly detected for the Cu-19 at.%Al alloy and caused the alpha (2) phase disordering process in two stages. The tendency to increase the alpha (2) dissolution precipitates with the increase in the Al content seems to be reverted for compositions at about 21 at.%Al and the heating/cooling ratio seems to influence the thermal response of this process. The presence of the endothermic peak corresponding to the beta (1)--> beta transformation depends on an incomplete beta decomposition reaction. The variation of the heating rate showed that the beta (1)-->(alpha+gamma (1)) decomposition is the dominant reaction for alloys containing 19 and 21 at.%Al.

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The effect of 4 mass% Ag addition on the thermal behavior of the Cu-9 mass% Al alloy was studied using differential scanning calorimetry (DSC), optical microscopy (OM), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffractometry (XRD). The results showed that the presence of silver causes (Cu)-alpha+(alpha+gamma1)-->(Cu)-alpha+beta transformation to occur in two stages. In the first one, part of the produced beta phase combines with the precipitated Ag to give a silver-rich phase and in the second one the transformation is completed. The formation of this silver-rich phase seems to be enhanced at very low cooling rates.

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Thermally sprayed HVOF coatings are increasingly being used in industrial applications where high wear and corrosion resistance are needed [1,2]. In this paper, electrochemical ac and de experiments were used in order to obtain the corrosion resistance of coated steel with different numbers of Cr3C2-NiCr layers. This work has been performed in order to determine the role of coating thickness in the corrosion behaviour of a steel protected with cermet thermally sprayed coatings. It is known that a thicker layer protects better against corrosion when a metallic coating is evaluated. But cermet coatings, such as Cr3C2-NiCr, contain higher levels of porosity and residual stresses than metallic coatings, which really could influence the corrosion resistance of the deposited layer. Electrochemical measurements, such as Open-Circuit Potential (E-Osubset of), Polarisation Resistance (RP) and Cyclic Voltammetry (CV), were performed in an aerated 3.4 NaCI media (%wt.). Electrochemical Impedance Measurements (EIS) were also done in order to obtain a mechanism that explains the corrosion process. Structural Characterisation was carried out by means of Optical and Scanning Electron Microscopes (OM, SEM) with an Energy Dispersive Spectrometry analyser (EDS). Results show that the corrosion resistance of the complete system is mainly influenced by the substrate behaviour. The application of a higher number of deposited layers did not substantially increase their anticorrosive properties. Stress generation during the spraying deposition process plays an important role in the behaviour of the coated steel against corrosion phenomena. (C) 2002 Elsevier B.V. B.V All rights reserved.

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Ferroelectric thin films belong to a class of materials with great technological importance in optic fibers, micro-electromechanical systems, and microprocessors and computers memories.The (1-x)PbMg1/3Nb2/3O3(x)PbTiO3 (PMN-PT) thin films, with x=0, 0.1, 0.35 and 0.5, were prepared by Pechini's process and deposited by spin-coating on Si(100), Pt/Ti/SiO2/Si(100) and quartz substrates. The goal of the present paper is to verify the thermal treatment influence on the perovskite phase formation, which is desirable for these applications. The phase formation was analyzed by X-ray diffraction. The film's surface was characterized by atomic force microscopy to analyze the roughness and the homogeneity. The results of this study indicate that the optimum conditions for obtaining the perovskite phase using a Pt/Ti/SiO2/Si(100) substrate, were drying each deposited layer at 140 degreesC (heating plate), and a final thermal treatment at 600 degreesC for 3 h in a closed system with a lead-rich atmosphere. (C) 2003 Elsevier B.V. All rights reserved.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)