First crystal structures of lanthanide-hydrocinnamate complexes: Hydrothermal synthesis and photophysical studies

Five new lanthanide(III) complexes of hydrocinnamic acid (Hcin), [Ln(cin)3(H2O)3]·3Hcin (Ln = Tb(III) (1), Dy(III) (2), Er(III) (3), Eu(III) (4) and Gd(III) (5)) have been synthesized and characterized. The X-ray structures of 1-5 reveal that all compounds are isostructural and that each lanthanide ion is nine-coordinated by oxygen atoms in an overall distorted tricapped trigonal-prismatic geometry. Six oxygen atoms are provided by carboxylate moieties, and the other three by water molecules. The supramolecular architectures of 1-5 show the presence of uncoordinated hydrocinnamic acid molecules which induce the formation of numerous hydrogen bonds. The photophysical properties of these complexes in the solid state at room temperature were studied using diffuse reflectance (DR), fluorescence excitation and emission spectra. An energy level diagram was used to establish the most relevant channels involved in the ligand-to-metal energy transfer, indicating that cin- ligands can act as intramolecular energy donors for Tb(III), Dy(III) and Eu(III) ions. © 2012 Elsevier B.V.

Microwave hydrothermal synthesis, characterisation, and catalytic performance of Zn1-xMnxO in cellulose conversion

Wurtzite-type Zn1-xMnxO (x = 0, 0.03, 0.05, 0.07) nanostructures were successfully synthesised using a simple microwave-assisted hydrothermal route and their catalytic properties were investigated in the cellulose conversion. The morphology of the nanocatalysts is dopant-dependent. Pure ZnO presented multi-plate morphology with a flower-like shape of nanometric sizes, while the Zn0.97Mn0.03O sample is formed by nanoplates with the presence of spherical nanoparticles; the Zn0.95Mn0.05O and Zn0.93Mn0.07O samples are mainly formed by nanorods with the presence of a small quantity of spherical nanoparticles. The catalyst without Mn did not show any catalytic activity in the cellulose conversion. The Mn doping promoted an increase in the density of weak acid sites which, according to the catalytic results, favoured promotion of the reaction. © 2013 Institute of Chemistry, Slovak Academy of Sciences.

Microwave-hydrothermal synthesis of single-crystalline Co3O 4 spinel nanocubes

An efficient microwave-hydrothermal (MAH) method has been developed for the synthesis of highly crystalline Co3O4 spinel nanocubes via β-Co(OH)2 without any surfactant assistance. The structure and surface chemical composition along the growth process are studied. The effects as well as the merits of the MAH method on the processing and characteristics of obtained Co3O4 spinel nanocubes are highlighted. © 2013 The Royal Society of Chemistry.

Microwave-assisted hydrothermal synthesis of magnetite nanoparticles with potential use as anode in lithium ion batteries

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

Titanate nanotubes produced from microwave-assisted hydrothermal synthesis: Photocatalytic and structural properties

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Long-range and short-range structures of cube-like shape SrTiO3 powders: microwave-assisted hydrothermal synthesis and photocatalytic activity

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Microwave-assisted hydrothermal synthesis of NiO-Ce1-XEuxO2-δ powders for fuel cell catalytic anodes

CeO2-based materials doped with rare earth (TR +3) can be used as alternative to traditional NiO-YSZ anodes in solid oxide fuel cells as they have higher ionic conductivity and lower ohmic losses compared to YSZ. Moreover, they allow fuel cell operation at lower temperatures (500-800°C). In the anode composition, the concentration of NiO acting as catalyst in YSZ provides high electrical conductivity and high electrochemical activity of reactions, promoting internal reform in the cell. In this work, NiO - Ce1-xEuxO2-δ compounds (x = 0.1, 0.2 and 0.3) have been synthesized by microwave-assisted hydrothermal method. The materials were characterized by TG, XRD, TPR and SEM-FEG techniques. The refinement of data obtained by X-ray diffraction showed the presence of ceria doped with europium crystallized in a cubic phase with fluorite structure, in addition to the presence of NiO. The microwave-assisted hydrothermal method showed significant reduction in the average particle size and good mass control of phase compositions compared to other chemical synthesis techniques.

Synthesis of KNbO3 nanostructures by a microwave assisted hydrothermal method

One-dimensional nanostructures of KNbO3 have attracted a great interest in the scientific community, mainly because of their promising application as nanoelectromechanical systems (NEMS). However, the synthesis of KNbO3 structures becomes complex due to the natural tendency to form non-stoichiometric potassium niobates. In this context, we report on the crystallization of one-dimensional KNbO3 nanostructures through the reaction between Nb2O5 and KOH under microwave-assisted hydrothermal synthesis (M-H). The use of this synthesis method made possible a very fast synthesis of singlecrystalline powders. Based on SEM, TEM and XRD characterizations, the influence of the synthesis time and the reactants concentration in the structure and morphology of the resultant KNbO3 was established. The conditions that favor the crystallization of nanofingers were determined to be small amounts of Nb2O5 and short reaction times. (C) 2008 Elsevier B.V. All rights reserved.

Photoluminescence properties and synthesis of a PZT mesostructure obtained by the microwave-assisted hydrothermal method

Micro-cube-shaped lead zirconate titanate was synthesized using the microwave-assisted hydrothermal method. Photoluminescence and field emission scanning electron microscopy were used for monitoring the formation of mesocrystals. Based on these results, a growth mechanism was then proposed which involved nanoparticle aggregation, nanoplate self-assembly on specific architecture and the final formation of mesoscopic micro-cube-shaped lead zirconate titanate. (C) 2011 Elsevier B. V. All rights reserved.

Photoluminescence properties of PZT 52/48 synthesized by microwave hydrothermal method using PVA with template

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

Synthesis and characterization of mesoporous TiO2 nanostructured films prepared by a modified sol-gel method for application in dye solar cells

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

Thermogravimetric investigations during the synthesis of silica-based MCM-41

MCM-41 material was synthesized starting from hydrogel containing colloidal fumed silica, sodium silicate, cetyltetramethylammonium bromide (CTMABr) as surfactant, and distilled water as solvent. These reactants were mixed to obtain a gel with the following composition: 4SiO(2):1Na(2)O:1CTMABr:200H(2)O. The hydrogel with pH=14 was hydrothermally treated at 100 degreesC, for 4 days. Each day, the pH was measured, and then adjusted to 9.5-10 by using 30% acetic acid solution. Thermogravimetry was the main technique, which was used to monitor the participation of the surfactant on the MCM-41 nanophase, being possible to determine the temperature ranges relative to water desorption as well as the surfactant decomposition and silanol condensation.

A study of the precursors and photoactivity of nanostructures of Ti oxides synthesized by the alkaline hydrothermal method

The present study describes the synthesis, characterization and photocatalytic potential of Ti oxide nanostructures of various morphologies and crystalline phases that were synthesized from 4 different precursors by the alkaline hydrothermal method. The materials were characterized by mainly X-ray diffraction (XRD), Raman spectroscopy, scanning and transmission electron microscopy (SEM and TEM), thermogravimetric analysis (TGA) and X-ray absorption spectroscopy (XAS). Also, photocatalytic potential was assessed by rhodamine B photodegradation. The materials obtained from peroxytitanium complexes (PTCs) exhibited a strong dependence on the concentration of KOH ([KOH]) used for synthesis. The pre-formed sheets of the PTCs were critical to the formation of nanostructures such as nanoribbons, and they were also compatible with the rolling up process, which can be utilized to form structures such as nanorods, nanowires or nanotubes. In the rhodamine photodegradation tests, TiO2 anatase nanostructures with six-coor inated Ti were more effective than the titanate ones (five-coordinated), despite having a smaller surface area and fewer OH groups. The lower photoactivity of the titanates was attributed to the presence of five-coordinated titanium species (TiO5), which may act as electron-hole recombination centers. Furthermore, the material with a mixture of TiO2/titanate was shown to be promising for photocatalytic applications. © 2013 by American Scientific Publishers.

Porous silica matrix obtained from pyrex class by hydrothermal treatment: Characterization and nature of the porosity

A novel porous silica matrix has been prepared from Pyrex glass, using hydrothermal treatment under saturated-steam condition. This process makes it possible to obtain, in one step, a silica support formed of a homogeneously distributed and interconnected macropore microstructure. The new matrix contains silanol groups that can be used in reactions of surface modification to provide a hybrid material and a selective macrofiltration membrane, and also it can improve chemical inertness. The porous matrix is noncrystalline as obtained and, after thermal treatment at temperatures higher than 950degreesC, exhibits an X-ray pattern characteristic of alpha-cristobalite and low volume contraction. The present samples were characterized by scanning electron microscopy, mercury intrusion porosimetry, nitrogen adsorption-desorption isotherms, infrared spectroscopy, X-ray powder diffractometry, atomic absorption, and high-resolution solid-state nuclear magnetic resonance. The results present a new way of producing a macroporous silica matrix.

Toward an understanding of intermediate- and short-range defects in ZnO single crystals. A combined experimental and theoretical study

A joint use of experimental and theoretical techniques allows us to understand the key role of intermediate- and short-range defects in the structural and electronic properties of ZnO single crystals obtained by means of both conventional hydrothermal and microwave-hydrothermal synthesis methods. X-ray diffraction, Raman spectra, photoluminescence, scanning electronic and transmission electron microscopies were used to characterize the thermal properties, crystalline and optical features of the obtained nano and microwires ZnO structures. In addition, these properties were further investigated by means of two periodic models, crystalline and disordered ZnO wurtzite structure, and first principles calculations based on density functional theory at the B3LYP level. The theoretical results indicate that the key factor controlling the electronic behavior can be associated with a symmetry breaking process, creating localized electronic levels above the valence band.