97 resultados para nitrogen adsorption isotherm


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This paper discusses the preparation and characterization of Zn 0.95Mn0.05O phase obtained by the polymeric precursor method for DMS applications. The as-obtained powders were calcined between 500 to 800°C and characterized by XRD, SEM and BET. The XRD analysis of the powder showed a crystalline material containing second phase. The crystallite sizes ranged from 20 to 51 nm. The micrographs showed that the powders consisted of soft and homogeneous agglomerations. The nitrogen adsorption/desorption curves of the Zn0.95Mn0.05O phases were type II curves, which is characteristic of mesoporous materials.

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This work involved the synthesis and characterization of Cu0.5Zn0.5Fe2O4 ferrite powders prepared by combustion reaction for use as soft magnetic materials. The powders were characterized by nitrogen adsorption (BET), XRD, Rietveld refinement, SEM, TEM and magnetic measures. The results indicate that the combustion reaction yielded crystalline powders containing spinel ferrite as the primary phase and traces of Fe2O3 as secondary phase. The crystallite size and lattice microdeformation calculated from Rietveld refinements were 36 and 0.24 nm, respectively. The micrographic analysis revealed particles smaller than 100 nm and fine particle agglomerates. The particles were approximately spherical and their size, calculated by TEM, was 29 nm. The magnetic parameters indicated that the Cu-Zn ferrite powders presented closed hysteresis loops and soft magnetic properties. © (2012) Trans Tech Publications, Switzerland.

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The catalytic properties of monomodal microporous and bimodal micro-mesoporous zeolites were investigated in the gas-phase dehydration of glycerol. The desilication methodology used to produce the mesoporous zeolites minimized diffusion limitations and increased glycerol conversion in the catalytic reaction due to the hierarchical system of secondary pores created in the zeolite crystals. The chemical and structural properties of the catalyst were studied by X-ray diffraction, nitrogen adsorption-desorption isotherms, NH3-TPD and pyridine chemisorption followed by IR-spectroscopy. Although the aim was to desilicate to create mesoporosity in the zeolite crystals, the desilication promoted the formation of extra-framework aluminum species that affected the conversion of glycerol and the products distribution. The results clearly show that the mesoporous zeolites with designed mesopore structure allowed a rapid diffusion and consequently improved the reaction kinetics. However, especial attention must be given to the desilication procedure because the severity of the treatment negatively interfered on the Brønsted and Lewis acid sites relative concentration and, consequently, in the efficiency of the catalysis performed by these materials. On the other hand, during the catalytic reaction, the intracrystalline mesopores allowed carbonaceous compounds to be deposited herein, resulting in less blocked micropores and catalysts with higher long-term stability.

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This paper proposes a response surface methodology to evaluate the influence of the particle size and temperature as variables and their interaction on the sulfation process using two Brazilian limestones, a calcite (ICB) and a dolomite (DP). Experiments were performed according to an experimental design [central composite rotatable design (CCRD)] carried out on a thermogravimetric balance and a nitrogen adsorption porosimeter. In the SO 2 sorption process, DP was shown to be more efficient than ICB. The best results for both limestones in relation to conversion and Brunauer-Emmett-Teller (BET) surface area were obtained under central point conditions (545 μm and 850 C for DP and 274 μm and 815 C for ICB). The optimal values for conversion were 52% for DP and 37% for ICB. For BET surface area, the optimal values were 35 m2 g-1 for DP and 45 m2 g-1 for ICB. A relationship between conversion and pore size distribution has been established. The experiments that showed higher conversions also exhibited more pores in the region between 20 and 150 Å and larger BET surface area, indicating that the amount of smaller pores may be an important factor in the reactivity of limestones. © 2013 American Chemical Society.

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Supercritical drying (SCD) and hydrophobic ambient pressure drying (APD) aerogels were prepared from hydrolysis of tetraethoxysilane in solutions of poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) (P123) in the range of composition below the threshold for the ordered mesoporous silica precipitation. APD was carried out after silylation of wet gels with trimethylchlorosilane (TMCS) or hexamethyldisilazane (HMDZ). The samples were analyzed by small-angle X-ray scattering and nitrogen adsorption. Wet gels are formed by mass-fractal domains, with fractal dimension close to 2, and larger pores superposing the pores belonging to the fractal structure in case of high P123 concentrations. Aerogels exhibit smaller-sized mass-fractal domains with larger mass-fractal dimension accounting for some porosity elimination on drying. The pore volume of the aerogels increases significantly with the P123 amount and it is even larger in the APD aerogels than in the SCD aerogels. © 2013 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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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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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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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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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Pós-graduação em Ciência dos Materiais - FEIS