Temperature-enhanced synthesis of DMSO-Melanin

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Influence of synthesis parameters on the formation of mesoporous SAPOs

The synthesis and characterization of high-quality mesoporous silicoaluminophosphates (SAPOs) with a hexagonally arranged pore structure and a good thermal stability are described. The influence of some important synthesis parameters including temperature, time, and Si content in the synthesis gel was examined. The local environments of Al, P, and Si were investigated using MAS NMR spectroscopy. The acidity of the mesoporous SAPOs was studied and compared with those of aluminosilicate MCM-41 and SAPO-5. Results show that both the synthesis temperature and time have a significant impact on the formation of mesoporous SAPOs, whereas the presence of Si in the synthesis gel has a direct influence on the structure type and the quality of the resulting mesoporous SAPO materials. High-quality mesoporous SAPOs can be synthesized from the synthesis gels with Si/Al ratio smaller than 0.5 in the presence of cationic surfactants in a weakly basic aqueous solution. The mesoporous SAPO materials show interesting acidity properties, possessing both strong and mild sites. (C) 2002 Elsevier Science Inc. All rights reserved.

Synthesis and properties of Co-doped titanate nanotubes and their optical sensitization with methylene blue

Agência Financiadora - Fundação para a Ciência e Tecnologia - PTDC/CTM NAN/113021/2009

Factorial design to optimize microwave-assisted synthesis of FDU-1 silica with a new triblock copolymer

The synthesis of FDU-1 silica with large cage-like mesopores prepared with a new triblock copolymer Vorasurf 504 (R) (Eo)(38)(BO)(46)(EO)(38) was developed. The hydrothermal treatment temperature, the dissolution of the copolymer in ethanol, the HCl concentration, the solution stirring time and the hydrothermal treatment time in a microwave oven were evaluated with factorial design procedures. The dissolution in ethanol is important to produce a material with better porous morphology. Increases in the hydrothermal temperature (100 degrees C) and HCl concentration (2 M) improved structural, textural and chemical properties of the cubic ordered mesoporous silica. Also, longer times induced better physical and chemical property characteristics. (C) 2010 Elsevier Inc. All rights reserved.

Synthesis and structure of cage-like mesoporous silica using different precursors

In this work the synthesis of cubic, FDU-1 type, ordered mesoporous silica (OMS) was developed from two types of silicon source, tetraethyl orthosilicate (TEOS) and a less expensive compound, sodium silicate (Na(2)Si(3)O(7)), in the presence of a new triblock copolymer template Vorasurf 504 (EO(38)BO(46)EO(38)). For both silicon precursors the synthesis temperature was evaluated. For TEOS the effect of polymer dissolution in methanol and the acid solution (HCl and HBr) on the material structure was analyzed. For Na(2)Si(3)O(7) the influence of the polymer mass and the hydrothermal treatment time were the explored experimental parameters. The samples were examined by Small Angle X-ray Scattering (SAXS) and Nitrogen Sorption. For both precursors the decrease on the synthesis temperature from ambient, -25 degrees C, to -15 degrees C improved the ordered porous structure. For TEOS, the SAXS results showed that there is an optimum amount of hydrophobic methanol that contributed to dissolve the polymer but did not provoke structural disorder. The less electronegative Br-ions, when compared to Cl-, induced a more ordered porous structure, higher surface areas and larger lattice parameters. For Na(2)Si(3)O(7) the increase on the hydrothermal treatment time as well as the use of an optimized amount of polymer promoted a better ordered porous structure. (C) 2011 Elsevier B.V. All rights reserved.

Synthesis and characterization of NiMn(2)O(4) nanoparticles using gelatin as organic precursor

Nanoparticles of NiMn(2)O(4) were successfully obtained by mixing gelatin and inorganic salts NiCl(2) center dot 6H(2)O and MnCl(2) center dot 4H(2)O in aqueous solution. The mixture has been synthesized at different temperatures and resulted in NiMn(2)O(4) nanoparticles with crystallites size in the range of 14-44 nm, as inferred from X-ray powder diffraction (XRPD) data. We have also observed that both the average crystallite size and the unit cell parameters increase with increasing synthesis temperature. Magnetic measurements confirmed the presence of a magnetic transition near 110K. (C) 2008 Published by Elsevier B.V.

Synthesis of YAP nanopowder by a soft chemistry route

Polycrystalline fine powder of YAlO(3) (YAP) was synthesized by the modified polymeric precursor method. A preliminary gradual pyrolytic decomposition under nitrogen flux was crucial in the removal process of organic residues to avoid the formation of molecular level inhomogeneities. YAP single phase was crystallized at temperatures between 950 degrees C and 1000 degrees C using chemically homogeneous ball-milled amorphous particles and very fast heating rates, corresponding to the lowest synthesis temperature of pure YAP nanopowder by soft chemistry routes. (C) 2009 Elsevier Ltd. All rights reserved.

Catalysis and temperature dependence on the formation of ZnO nanoparticles and of zinc acetate derivatives prepared by the sol-gel route

The chemical and structural nature of powders prepared from the zinc acetate-derived precursor using the sol-gel route is discussed. The influence of the synthesis temperature and of the hydrolytic catalyst on the structural features of the powder is focused on the basis of X-ray powder diffraction (XRPD) and extended X-ray absorption fine structure (EXAFS) measurements and complemented with density and thermoanalysis (TG-DTA) results. EXAFS and XRPD results show that no-washed nanoparticulate powders are composed of a mixture of ZnO (wurtzite), zinc acetate, and zinc hydroxyacetate. The latter has a layered structure typical of hydroxy double salts (HDS). The main component of no-washed powders is always unreacted zinc acetate solid but the relative amount of the zinc-based compounds depends on the nature of the hydrolytic catalyst, hydrolysis ratio, and of synthesis temperature. According to the proportion of the three zinc-based compounds, three families of powders could be distinguished. The amount of ZnO nanoparticles (1.6 +/- 0.6 nm) decreases as the synthesis temperature increases, as the hydrolysis ratio decreases, or by changing from basic to acid catalysis. This finding suggests that the formation of zinc compounds is controlled by the equilibrium between hydrolysis-condensation and complexation-reprecipitation reactions.

High-efficient microwave synthesis and characterisation of SrSnO3

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Lead-free BaBi4Ti4O15 ceramics: Effect of synthesis methods on phase formation and electrical properties

The processing of ferroelectric BaBi4Ti4O15 (BBT) ceramics from powders prepared by conventional solid state reaction (SSR) and mechanochemical activation (MA) has been investigated. It was shown that MA synthesis reduces the synthesis temperature of BBT powders, leading to smaller particles with reduced anisotropy and consequently to smaller grain size of ceramics. Dielectric properties were investigated in a wide range of temperatures (20-800 degrees C) and frequencies (1.21 kHz to 1 MHz). The relative dielectric permittivity at Curie temperature was higher for solid state obtained ceramics than for the mechanically treated ones. The conductivity of sintered samples was studied, suggesting decreasing of conductivity of BBT-MA in comparison with BBT-SS ceramics. The influence of the grain and the grain boundaries contribution to the dielectric behavior in both ceramics was analyzed through impedance spectroscopy. A well-defined ferroelectric hysteresis loop was obtained for both samples. (C) 2014 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Synthesis and Thermoelectric Properties of Bi2Se3 Nanostructures

Bismuth selenide (Bi2Se3) nanostructures were synthesized via solvothermal method. The crystallinity of the as-synthesized sample has been analyzed by X-ray diffraction, which shows the formation of rhombohedral Bi2Se3. Electron microscopy examination indicates that the Bi2Se3 nanoparticles have hexagonal flake-like shape. The effect of the synthesis temperature on the morphology of the Bi2Se3 nanostructures has also been investigated. It is found that the particle size increases with the synthesis temperature. Thermoelectric properties of the Bi2Se3 nanostructures were also measured, and the maximum value of dimensionless figure of merit (ZT) of 0.096 was obtained at 523 K.

Si3N4 single-crystal nanowires grown from silicon micro- and nanoparticles near the threshold of passive oxidation

A simple and most promising oxide-assisted catalyst-free method is used to prepare silicon nitride nanowires that give rise to high yield in a short time. After a brief analysis of the state of the art, we reveal the crucial role played by the oxygen partial pressure: when oxygen partial pressure is slightly below the threshold of passive oxidation, a high yield inhibiting the formation of any silica layer covering the nanowires occurs and thanks to the synthesis temperature one can control nanowire dimensions

Si3N4 single-crystal nanowires grown from silicon micro- and nanoparticles near the threshold of passive oxidation

A simple and most promising oxide-assisted catalyst-free method is used to prepare silicon nitride nanowires that give rise to high yield in a short time. After a brief analysis of the state of the art, we reveal the crucial role played by the oxygen partial pressure: when oxygen partial pressure is slightly below the threshold of passive oxidation, a high yield inhibiting the formation of any silica layer covering the nanowires occurs and thanks to the synthesis temperature one can control nanowire dimensions

Band gap control via tuning of inversion degree in CdIn2S4 spinel

Based on theoretical arguments we propose a possible route for controlling the band-gap in the promising photovoltaic material CdIn2S4. Our ab initio calculations show that the experimental degree of inversion in this spinel (fraction of tetrahedral sites occupied by In) corresponds approximately to the equilibrium value given by the minimum of the theoretical inversion free energy at a typical synthesis temperature. Modification of this temperature, or of the cooling rate after synthesis, is then expected to change the inversion degree, which in turn sensitively tunes the electronic band-gap of the solid, as shown here by Heyd-Scuseria-Ernzerhof screened hybrid functional calculations.

Síntese de nanopartículas de magnetita via decomposição térmica em meio não-aquoso

This work aims at obtaining nanoparticles of iron oxide, the magnetite one (Fe3O4), via synthesis by thermal decomposition through polyol. Thus, two routes were evaluated: a simple decomposition route assisted by reflux and a hydrothermal route both without synthetic air atmosphere using a synthesis temperature of 260ºC. In this work observed the influence of the observe of surfactants which are generally applied in the synthesis of iron oxide nanoparticles decreasing cluster areas. Further, was observed pure magnetite phase without secondary phases generally found in the iron oxide synthesis, a better control of crystallite size, morphology, crystal structure and magnetic behavior. Finally, the introduction of hydroxyl groups on the nanoparticles surface was analyzed besides its employment in the polymer production with OH radicals. The obtained materials were characterized by XRD, DLS, VSM, TEM, TG and DSC analyses. The results for the magnetite obtainment with a particle size greater than 5 nm and smaller than 11 nm, well defined morphology and good magnetic properties with superparamagnetic behavior. The reflux synthesis was more efficient in the deposition of the hydroxyl groups on the nanoparticles surface