932 resultados para Raman Spectroscopy and Scattering


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Este trabalho descreve detalhadamente o efeito da quantidade de cério na estrutura e morfologia da zeólita NH4USY. Ce-USY (2-25% m/m de CeO2) foi obtido por impregnação úmida de CeCl3 seguida de calcinação a 550ºC por 8 h. Em quantidades baixas (2-10%), foi observado que as espécies de cério encontram-se nas posições de troca iônica na rede, enquanto em maiores teores (15-25%) pequenos agregados formaram-se na superfície da HUSY. Difratometria de raios X (XRD) mostrou apenas reflexões relacionadas à HUSY, confirmando a alta dispersão das espécies de cério, porém as análises por espectroscopia Raman com transformada de Fourier (FT-Raman) detectaram CeOx para os materiais acima de 10%. A reação do CeCl3 com NH4USY produziu NH4Cl, o qual se decompõe em HCl, ocasionando a desaluminização da rede. Os materiais apresentaram um aumento da razão Lewis/Brønsted com o aumento da quantidade de cério, devido a interação do excesso de cério com os grupos OH da USY e consequente formação de espécies CeOx.

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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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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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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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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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This study compared the effect of physicochemical surface conditioning methods on the adhesion of bis-GMA-based resin cement to particulate filler composite (PFC) used for indirect dental restorations. PFC blocks (N (block)=54, n (block)=9 per group) were polymerized and randomly subjected to one of the following surface conditioning methods: a) No conditioning (Control-C), b) Hydrofluoric acid (HF)etching for 60s (AE60), c) HF for 90s (AE90), d) HF for 120s (AE120), e) HF for 180s (AE180), and f) air-abrasion with 30 mu m silica-coated alumina particles (AB). The conditioned surfaces were silanized with an MPS silane, and an adhesive resin was applied. Resin composite blocks were bonded to PFC using resin cement and photo-polymerized. PFC-cement-resin composite blocks were cut under coolant water to obtain bar specimens (1mmx0.8mm). Microtensile bond strength test (mu TBS)was performed in a universal testing machine (1mm/min). After debonding, failure modes were classified using stereomicroscopy. Surface characterization was performed on a set of separate specimen surfaces using Scanning Electron Microscopy (SEM), X-Ray Dispersive Spectroscopy (XDS), X-Ray Photoelectron Spectroscopy (XPS), and Fourier Transform-Raman Spectroscopy (FT-RS). Mean mu TBS (MPa) of C (35.6 +/- 4.9) was significantly lower than those of other groups (40.2 +/- 5.6-47.4 +/- 6.1) (p<0.05). The highest mu TBS was obtained in Group AB (47.4 +/- 6.1). Prolonged duration of HF etching increased the results (AE180: 41.9 +/- 7), but was not significantly different than that of AB (p>0.05). Failure types were predominantly cohesive in PFC (34 out of 54) followed by cohesive failure in the cement (16 out of 54). Degree of conversion (DC) of the PFC was 63 +/- 10%. SEM analysis showed increased irregularities on PFC surfaces with the increased etching time. Chemical surface analyses with XPS and FT-RS indicated 11-70% silane on the PFC surfaces that contributed to improved bond strength compared to Group C that presented 5% silane, which seemed to be a threshold. Group AB displayed 83% SiO2 and 17% silane on the surfaces.

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

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

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A synergistic electrocatalytic effect was observed in sensors where two electrocatalytic materials (functionalized gold nanoparticles and lutetium bisphthalocyanine) were co-deposited using the Langmuir-Blodgett technique. Films were prepared using a novel method where water soluble functionalised gold nanoparticles [(11-mercaptoundecyl)tetra(ethylene glycol)] (SAuNPs) were inserted in floating films of lutetium bisphthalocyanine (LuPc2) and dimethyldioctadecylammonium bromide (DODAB) as the amphiphilic matrix. The formation of stable and homogeneous mixed films was confirmed by pi-A isotherms, BAM, UV-vis and Raman spectroscopy, as well as by SEM and TEM microscopy. The synergistic effect towards hydroquinone of the electrodes modified with LuPc2:DODAB/SAuNP was characterised by an increase in the intensity of the redox peaks and a reduction of the overpotential. This synergistic electrocatalytic effect arose from the interaction between the SAuNPs and the phthalocyanines that occur in the Langmuir-Blodgett films and from the high surface area provided by the nanostructured films. The sensitivity increased with the amount of LuPc2 and SAuNPs inserted in the films and limits of detection in the range of 10(-7) mol L-1 were attained. (C) 2014 Elsevier B.V. All rights reserved.

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Perovskite, single multiferroic bismuth ferrite was prepared by two chemical methods: auto-combustion and soft chemical route. Influence of different fuels and complexing agents and thermal treatment on purity of bismuth ferrite powders and density of bismuth ferrite ceramics were investigated. X-ray diffraction technique (XRD) indicated that optimal temperatures and times for calcination and sintering are 600 degrees C for 2 h and 800 degrees C for 1 h with quenching, respectively. Scanning electron microscopy (SEM) analysis showed that soft route synthesized samples formed softer agglomerates and smaller grains with less secondary phases. Powders and pellets were characterized by Brunauer Emmett Teller (BET) specific surface area analysis, particle size distribution, Fourier transform infrared spectroscopy (FT-IR), dilatometry, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), dielectric and magnetic measurements. Resistivity and origin of electrical resistance were studied by means of impedance measurements. (C) 2014 Elsevier Ltd and Techna Group S.r.l. All rights reserved.