203 resultados para Energy dispersive X ray (EDX) spectroscopy


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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Pós-graduação em Ciência dos Materiais - FEIS

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Dissipadores de calor recobertos com filmes de diamante CVD foram desenvolvidos para acoplar a semicondutores, utilizando-se do Laboratório de Deposição de Filmes de Diamante CVD, na UNESP - Campus de Guaratinguetá e o Laboratório de Diamantes da Universidade São Francisco, em Itatiba, SP. Analisou-se o filme de diamante CVD sobre o silício, para emprego como dissipador de calor, porque o filme de diamante CVD pode ter o valor da condutividade térmica até cinco vezes superior ao do cobre e de dez vezes a do alumínio. Os filmes foram obtidos via deposição através de reator de filamento quente, trabalhando-se com vários filamentos retilíneos em paralelo, resultando assim em um processo que visou obter um filme mais uniforme e com grande área de deposição. Os dados para análises da composição química superficial dos filmes foram obtidos por Difração de Raios-X, Dispersão de Energia de Raios-X e para a verificação da morfologia e espessura do filme foi utilizada a Microscopia Eletrônica de Varredura. Para a verificação do comportamento da temperatura sobre o dissipador com o filme de diamante CVD foi utilizada uma câmera de imagem termográfica, marca Fluke, modelo Ti 40 FT. Foram obtidos filmes de 2 e 10 ?m sobre o silício. Estas espessuras ainda não oferecem um desempenho mecânico que o torne autosustentado. Do ponto de vista de desempenho térmico as análises mostraram que, mesmo com pequena espessura, o filme de diamante CVD apresentou bom resultado experimental. Os principais desafios de construção para esse dissipador de calor são a obtenção do filme com espessura acima de um mm e a garantia da qualidade do filme com a repetitividade do processo em cujo caso torna-se necessário definir as dimensões do dissipador antes da deposição do filme.

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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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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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The purpose of the study was to use scanning electron microscopy and energy dispersive x-ray spectrometry to assess possible morphologic and chemical changes after performing double-insertion and pullout tests of implants of different shapes and surface treatments. Four different types of implants were used—cylindrical machined-surface implants, cylindrical double-surface–treated porous implants, cylindrical surface-treated porous implants, and tapered surface-treated porous implants—representing a total of 32 screws. The implants were inserted into synthetic bone femurs, totaling 8 samples, before performing each insertion with standardized torque. After each pullout the implants were analyzed by scanning electron microscopy and energy dispersive x-ray spectrometry using a universal testing machine and magnified 35 times. No structural changes were detected on morphological surface characterization, only substrate accumulation. As for composition, there were concentration differences in the titanium, oxygen, and carbon elements. Implants with surface acid treatment undergo greater superficial changes in chemical composition than machined implants, that is, the greater the contact area of the implant with the substrate, the greater the oxide layer change. In addition, prior manipulation can alter the chemical composition of implants, typically to a greater degree in surface-treated implants.

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The aim of this study was to evaluate the physicochemical properties and bioactivity of two formulations of calcium silicate-based cements containing additives (CSCM) or resin (CSCR), associated with radiopacifying agents zirconium oxide (ZrO2) and niobium oxide (Nb2O5) as micro- and nanoparticles; calcium tungstate (CaWO4); and bismuth oxide (Bi2O3). MTA Angelus was used as control. Methods. Surface features and bioactivity were evaluated by scanning electron microscopy and the chemical composition by energy dispersive X-ray spectrometry (EDS-X). Results. CSCM and CSCR presented larger particle sizes than MTA. Hydroxyapatite deposits were found on the surface of some materials, especially when associated with the radiopacifier with ZrO2 nanoparticles. All the cements presented calcium, silicon, and aluminum in their composition. Conclusion. Both calcium silicate-based cements presented composition and bioactivity similar to MTA when associated with the radiopacifiers evaluated.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Background: the failure of osseointegration in oral rehabilitation has gained importance in current literature and in clinical practice. The integration of titanium dental implants in alveolar bone has been partly ascribed to the biocompatibility of the implant surface oxide layer. The aim of this investigation was to analyze the surface topography and composition of failed titanium dental implants in order to determine possible causes of failure.Methods: Twenty-one commercially pure titanium (cpTi) implants were retrieved from 16 patients (mean age of 50.33 +/- 11.81 years). Fourteen implants were retrieved before loading (early failures), six after loading (late failures), and one because of mandibular canal damage. The failure criterion was lack of osseointegration characterized as dental implant mobility. Two unused implants were used as a control group. All implant surfaces were examined by scanning electron microscopy (SEM) and energy-dispersive spectrometer x-ray (EDS) to element analysis. Evaluations were performed on several locations of the same implant.Results: SEM showed that the surface of all retrieved implants consisted of different degrees of organic residues, appearing mainly as dark stains. The surface topography presented as grooves and ridges along the machined surface similar to control group. Overall, foreign elements such as carbon, oxygen, sodium, calcium, silicon, and aluminum were detected in failed implants. The implants from control group presented no macroscopic contamination and clear signs of titanium.Conclusion: These preliminary results do not suggest any material-related cause for implant failures, although different element composition was assessed between failed implants and control implants.

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Small-angle X-ray scattering (SAXS) and electron paramagnetic resonance (EPR) have been carried out to investigate the structure of the self-aggregates of two phenothiazine drugs, chlorpromazine (CPZ) and trifluoperazine (TFP), in aqueous solution. In the SAXS studies, drug solutions of 20 and 60 mM, at pH 4.0 and 7.0, were investigated and the best data fittings were achieved assuming several different particle form factors with a homogeneous electron density distribution in respect to the water environment. Because of the limitation of scattering intensity in the q range above 0.15 angstrom(-1), precise determination of the aggregate shape was not possible and all of the tested models for ellipsoids, cylinders, or parallelepipeds fitted the experimental data equally well. The SAXS data allows inferring, however, that CPZ molecules might self-assemble in a basis set of an orthorhombic cell, remaining as nanocrystallites in solution. Such nanocrystals are composed of a small number of unit cells (up to 10, in c-direction), with CPZ aggregation numbers of 60-80. EPR spectra of 5- and 16-doxyl stearic acids bound to the aggregates were analyzed through simulation, and the dynamic and magnetic parameters were obtained. The phenothiazine concentration in EPR experiments was in the range of 5-60 mM. Critical aggregation concentration of TFP is lower than that for CPZ, consistent with a higher hydrophobicity of TFP. At acidic pH 4.0 a significant residual motion of the nitroxide relative to the aggregate is observed, and the EPR spectra and corresponding parameters are similar to those reported for aqueous surfactant micelles. However, at pH 6.5 a significant motional restriction is observed, and the nitroxide rotational correlation times correlate very well with those estimated for the whole aggregated particle from SAXS data. This implies that the aggregate is densely packed at this pH and that the nitroxide is tightly bound to it producing a strongly immobilized EPR spectrum. Besides that, at pH 6.5 the differences in motional restriction observed between 5- and 16-DSA are small, which is different from that observed for aqueous surfactant micelles.

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