990 resultados para Thermal Microscopy
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Strontium barium niobate (SBN) thin films were crystallized by conventional electric furnace annealing and by rapid-thermal annealing (RTA) at different temperatures. The average grain size of films was 70 nm and thickness around 500 nm. Using x-ray diffraction, we identified the presence of polycrystalline SBN phase for films annealed from 500 to 700 °C in both cases. Phases such as SrNb2O6 and BaNb2O6 were predominantly crystallized in films annealed at 500 °C, disappearing at higher temperatures. Dielectric and ferroelectric parameters obtained from films crystallized by conventional furnace and RTA presented essentially the same values.
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Thermal spray coatings as Cr3C2-NiCr obtained by high velocity oxy-fuel spraying (HVOF) are mainly applied due to their behaviour against aggressive erosive-abrasive and corrosive atmospheres and their thermal stability at high temperatures [1]. In order to increase the corrosion protection that it offers to the substrate trying to close the interconnected pores, it is possible to apply a thermal treatment with the gun during the spraying of the coating. This treatment could be applied in different ways. One of these ways consists of spraying only a few layers of coating followed by thermal treatment and finally the spray of the rest of layers. This thermal treatment on spraying is studied related to the corrosion properties of the system. The study comprises the electrochemical characterisation of the system by open circuit potential (OC), polarisation resistance (Rp), cyclic voltammetry (CV) and impedance spectroscopy measurements (EIS). Optical and scanning electron microscopy characterisation (OM and SEM) of the top and cross-section of the system has been used in order to justify the electrochemical results.
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Nylon6/ABS binary blends are incompatible and need to be compatibilized to achieve better performance under impact tests. Poly(methyl methacrylate/maleic anhydride) (MMA-MA) is used in this work to compatibilize in situ nylon6/ABS immiscible blends. The MA functional groups, from MMA-MA copolymers, react with NH2 groups giving as products nylon molecules grafted to MMA-MA molecules. Those molecular species locate in the nylon6/ABS blend interfacial region increasing the local adhesion. MMA-MA segments are completely miscible with the SAN rich phase from the ABS. The aim of this work is to study the effects of ABS and compatibilizing agent on the melting and crystallization of nylon6/ABS blends. This effect has been investigated by differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMTA). Incorporation of this compatibilizer and ABS showed little effect on the melting behavior of the PA6 crystalline phase, in general. DMTA analysis confirmed the system immiscibility and showed evidence of compatibility between the two phases, nylon6 and ABS, produced by MMA-MA copolymer presence. The nylon6/ABS blend morphology, observed by transmission electron microscopy (TEM), changes significantly by the addition of the MMA-MA compatibilizer. A better dispersion of ABS in the nylon6 phase is observed. © 2004 Kluwer Academic Publishers.
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The discovery of the spatial uniform coexistence of superconductivity and ferromagnetism in rutheno-cuprates, RuSr2GdCu2O8 (Ru-1212), has spurred an extraordinary development in the study of the competition between magnetism and superconductivity. However, several points of their preparation process and characterization that determine their superconductive behavior are still obscure. The improvement of sample preparation conditions involves some thermal treatments in inert atmosphere. The first treatment results in the immediate formation of Sr2GdRuO 6. Using the CuO composition as a precursor, we produced Ru-1212. To turn it metallic and superconductor, besides the previous treatment, a final sinterization is carried out in oxygen flow for several days. Three Ru-1212 samples were produced by varying the last sinterization time (two, four, and six days under oxygen flow). Through measurements of x-ray diffraction, scanning electron microscopy, differential thermal analysis, magnetic susceptibility and mechanical spectroscopy, it was studied the influence of the treatments under oxygen atmosphere on the structural and superconducting properties of the material.
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Peat was taken from the Sergipe State, Brazil and characterized by several techniques: elemental and thermal analyses; Fourier infrared (FTIR) and solid state 13C nuclear magnetic resonance (NMR) spectroscopies; scanning electron microscopy (SEM), environmental scanning electron microscopy (ESEM) and X-ray diffractometry (XRD). Also, the Sergipe State peat samples were compared with other peat sample from later from Sao Paulo State, Brazil. The lowest O/C and E 4/E 6 ratios and differential thermal analysis (DTA) curves of the Santo Amaro (SAO) sample indicated that this sample had the highest degree of decomposition. FTIR results showed that Itabaiana (ITA) and São Paulo (SAP) samples presented more prominent peak at 1086 cm -1 attributed the presence of Si-O than SAO sample spectra. The SAO sample showed two more intense peaks at 2920 cm -1 and 2850 cm -1. These results were corroborated by 13C NMR and thermal gravimetric (TG) where the relative abundance of the alkyl-C groups was greater in the SAO sample. The X-ray diffractometry (XRD) of SAO sample is characteristic of amorphous matter however, the SAP and ITA samples revealed the large presence of quartz mineral. The scanning electron microscopy (SEM) and environmental scanning electron microscopy (ESEM) showed that the surface of peat samples have porous granules of organic material. The ITA and SAP peat samples are alike while SAO peat sample is richer in organic material. Only the SAO sample has truthful characteristics of peat. The results of this study showed that the samples are very different due to variable inorganic and organic material contents. ©2007 Sociedade Brasileira de Química.
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ZnO thin films were prepared by the polymeric precursor method. The films were deposited on silicon substrates using the spin-coating technique, and were annealed at 330°C for 32h under pressure-assisted thermal annealing and under ambient pressure. Their structural and optical properties were characterized, and the phases formed were identified by X-ray diffraction. No secondary phase was detected. The ZnO thin films were also characterized by field-emission scanning electron microscopy, Fourier transform infrared spectroscopy, photoluminescence and ultraviolet emission intensity measurements. The effect of pressure on these thin films modifies the active defects that cause the recombination of deep level states located inside the band gap that emit yellow-green (575nm) and orange (645nm) photoluminescence. © 2012 John Wiley & Sons, Ltd.
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Starch is arguably one of the most actively investigated biopolymer in the world. In this study, the native (untreated) cassava starch granules (Manihot esculenta, Crantz) were hydrolyzed by standard hydrochloric acid solution at different temperatures (30 °C and 50 °C) and the hydrolytic transformations were investigated by the following techniques: simultaneous thermogravimetry-differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), as well as non-contact atomic force microscopy (NC-AFM), X-ray diffraction (XRD) powder patterns, and rapid viscoamylographic analysis (RVA). After the treatment with hydrochloric acid at different temperatures, the thermal stability, a gradual loss of pasting properties (viscosity), alterations in the gelatinization enthalpy (ΔHgel), were observed. The use of NC-AFM and XRD allowed the observation of the surface morphology and topography of the starch granules and changes in crystallinity of the granules, respectively. © 2012 Elsevier B.V. All rights reserved.
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Composite films made of lead zirconate titanate ceramic particles coated with polyaniline and poly(vinylidene fluoride) - PZT-PAni/PVDF were produced by hot pressing the powder mixtures in the desired ceramic volume fraction. The ceramic particles were coated during the polyaniline synthesis and the conductivity of the conductor polymer was controlled by different degrees of protonation. Composites were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), ac and dc electrical measurements, the longitudinal d33 piezo coefficient and the photopyroelectric response. Results showed that the presence of PAni increased the dielectric permittivity of the composite and allowed better efficiency in the poling process, which increased the piezo- and pyroelectric activities of the composite film and reduced both the poling time and the poling electric field. The thermal sensing of the material was also analyzed, showing that this composite can be used as pyroelectric sensor. © 2013 IOP Publishing Ltd.
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The use of chemically modified starches is widely accepted in various industries, with several applications. In this research, natural cassava starch granules were treated with standard sodium hypochlorite solution at 0.8, 2.0, and 5.0 g Cl/100 g starch. The native and modified starch samples were investigated by means of the following techniques: simultaneous thermogravimetry-differential thermal analysis, which allowed us to verify the thermal decomposition associated with endothermic or exothermic phenomena; and differential scanning calorimetry that was used to determine gelatinization enthalpy as well as the rapid viscoamylographic analysis that provided the pasting temperature and viscosity. By means of non-contact-atomic force microscopy method and X-ray powder patterns diffractometry, it was possible to observe the surface morphology, topography of starch granules, and alterations in the granules' crystallinity. © 2012 Akadémiai Kiadó, Budapest, Hungary.
Sintering of porous alumina obtained by biotemplate fibers for low thermal conductivity applications
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In this research report, a sintering process of porous ceramic materials based on Al2O3 was employed using a method where a cation precursor solution is embedded in an organic fibrous cotton matrix. For porous green bodies, the precursor solution and cotton were annealed at temperatures in the range of 100-1600°C using scanning electron microscopy (SEM) and thermogravimetric (TG) analysis to obtain a porous body formation and disposal process containing organic fibers and precursor solution. In a structure consisting of open pores and interconnected nanometric grains, despite the low porosity of around 40% (calculated geometrically), nitrogen physisorption determined a specific surface area of 14m2/g, which shows much sintering of porous bodies. Energy dispersive X-ray (EDX) and X-ray diffraction (XRD) analytical methods revealed a predominant amount of α-Al2O3 in the sintered samples. Thermal properties of the sintered Al2O3 fibers were obtained by using the Laser Flash which resulted in the lower thermal conductivity obtained by α-Al2O3 and therefore improved its potential use as an insulating material. © 2012 Elsevier Ltd.
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Thermogravimetry (TG), energy dispersive X-ray microanalysis (EDX), scanning electron microscopy (SEM), mapping surface and X-ray diffraction (XRD) were used for the study of solid-state reaction on Pt-15%Rh with electrodeposited mercury. The results suggest when heated the mercury film react with the Pt-15%Rh alloy to form intermetallics having different thermal stabilities indicated by three mass loss steps. The first mass loss step occurs between room temperature and 184 degrees C only the bulk Hg is removed and PtHg4, PtHg2 and RhHg2 were characterized by XRD. The second step, between 184 and 271 degrees C, was attributed to PtHg4 decomposition with formation of PtHg2 stabilized by RhHg2. The third step, between 271 and 340 degrees C, was attributed to decomposition of a solid-solution of PtHg2/RhHg2. The fourth step, between 340 and 600 degrees C, was ascribed to: (1) a thermal decomposition of PtHg2, formed by a PtHg eutectoid reaction (similar to 340 degrees C) on the surface and (2) Hg removal from a solid solution of Pt-15%Rh(Hg). (C) 2013 Elsevier B.V. All rights reserved.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)