Microwave synthesis and spectroscopic characterization of manganese oxalate nanocrystals

The microwave synthesis of MnC2O4·2H2O nanoparticles was performed through the thermal double decomposition of oxalic acid dihydrate (C2H2O4·2H2O) and Mn(OAc)2·4H2O solutions using a CATA-2R microwave reactor. Structural characterization was performed using X-ray diffraction (XRD), particle size and shape were analyzed using transmission electron microscopy (TEM). The chemical in the structures was investigated using electron paramagnetic resonance (EPR) as well as optical absorption spectra and near-infrared (NIR) spectroscopies. The nanocrystals produced with this method were pure and had a distorted rhombic octahedral structure.

Extraordinary supercapacitor performance of heavily nitrogenated graphene oxide obtained by microwave synthesis

Heavily nitrogenated graphene oxide containing similar to 18 wt% nitrogen, prepared by microwave synthesis with urea as the nitrogen source, shows outstanding performance as a supercapacitor electrode material, with the specific capacitance going up to 461 F g(-1).

Microwave synthesis of fluorescent carbon nanoparticles with electrochemiluminescence properties

We present a facile, economical microwave pyrolysis approach to synthesize fluorescent carbon nanoparticles with electrochemiluminescence properties.

Microwave synthesis of YAG : Eu by sol-gel methodology

Yttrium-aluminum oxides are interesting compounds and they have been extensively used as host for lasers and phosphors, due to their stable physical and chemical properties. The fabrication of yttrium-aluminum garnet (YAG) has been investigated thoroughly. Single-crystal YAG is expensive and to produce it a new way has been investigated. This process consists of modifying the methodology of reagents mixture and the process of heating them. The microwave irradiation is used to heat-treat the oxide mixture. The traditional synthesis of YAG powders occurs through the reaction of aluminum and yttrium powders at high temperatures. With this work we investigated the preparation of YAG by non-hydrolytic sol-gel route as an alternative methodology to obtain yttrium-aluminum matrix from inorganic precursors (yttrium and aluminum chloride). The preparation of the gel was carried out in an oven-dried glassware. The AlCl3, YCl3 and ethanol were reacted in reflux under argon atmosphere. Europium III chloride was added as a structural probe. The powder was dried and heat-treated in modified microwaves. The samples were pre-treated at 50 and 800 C during I h and then heated in microwaves for 30 s, 2 and 4 min. The formation process and structure of the powders were studied by means of X-ray diffraction (XRD), photoluminescence (PL) and transmission electronic microscopy (TEM). XRD presents only picks corresponding to the YAG phase and confirmed by TEM. PL date showed that the YAG phase was formed in 2 min with the samples pre-treated at 50 C. For the samples pretreated at 800 degrees C, the YAG phase appears in 30s. The excitation spectra present a maximum of 394 nm corresponding to the L-5(6) level and emission spectra of Eu III ion present bands characteristic transitions arising from the D-5(0) -> F-7(J) (J= 1, 2, 3, 4) monifolds excited at their maximum. The magnetic dipole D-5(0) -> F-7(1) transition presents more intensity than the electric dipole D-5(0) -> F-7(2) transition. This methodology showed efficiency in obtaining YAG phase. (c) 2006 Elsevier B.V. All rights reserved.

Microwave synthesis of calcium bismuth niobate thin films obtained by the polymeric precursor method

The crystal structure, surface morphology and electrical properties of layered perovskite calcium bismuth niobate thin films (CaBi2Nb2O9-CBN) deposited on platinum coated silicon substrates by the polymeric precursor method have been investigated. The films were crystallized in a domestic microwave and in a conventional furnace. X-ray diffraction and atomic force microscopy analysis confirms that the crystallinity and morphology of the films are affected by the different annealing routes. Ferroelectric properties of the films were determined with remanent polarization P-r and a drive voltage V-c of 4.2 mu C/cm(2) and 1.7 V for the film annealed in the conventional furnace and 1.0 mu C/cm(2) and 4.0 V for the film annealed in microwave furnace, respectively. A slight decay after 10(8) polarization cycles was observed for the films annealed in the microwave furnace indicating a reduction of the domain wall mobility after interaction of the microwave energy with the bottom electrode. (C) 2006 Elsevier Ltd. All rights reserved.

High-efficient microwave synthesis and characterisation of SrSnO3

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Microwave Synthesis of Short-Chained Fluorinated Ionic Liquids and Their Surface Properties

Microwave synthesis is shown to be a valuable route to novel fluorinated ionic liquid surfactants. 1-Methyl-3-(3,3,4,4,5,5,6,6,6-nonafluorohexyl)imidazolium iodide was prepared by treatment of 1-methylimidazole with 1-iodo-1H,1H,2H,2H-perfluorohexane in a microwave reactor, and this product underwent anion exchange to yield 1-methyl-3-(3,3,4,4,5,5,6,6,6-nonafluorohexyl)imidazolium nonafluoro-1-butanesulfonate. This catanionic surfactant showed intriguing phase behavior and low surface tension.

Efficient microwave-assisted hydrothermal synthesis of CuO sea urchin-like architectures via a mesoscale self-assembly

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

Synthesis of inorganic solids using microwaves

Use of microwaves in the synthesis of materials is gaining importance. Microwave-assisted synthesis is generally much faster, cleaner, and more economical than the conventional methods. A variety of materials such as carbides, nitrides, complex oxides, silicides, zeolites, apatite, etc. have been synthesized using microwaves. Many of these are of industrial and technological importance. An understanding of the microwave interaction with materials has been based on concepts of dielectric heating and of the resonance absorption due to rotational excitation. This review presents a summary of recent reports of microwave synthesis of inorganic materials. Various observations regarding microwave interaction with materials are also briefly discussed.

Immobilization of glucose oxidase enzyme (GOD) in large pore ordered mesoporous cage-like FDU-1 silica

Large pore ordered mesoporous silica FDU-1 with three-dimensional (3D) face-centered cubic, Fm3m arrangement of rnesopores, was synthesized under strong acid media using B-50-6600 poly(ethylene oxide)-poly(butylene oxide)-poly(ethylene oxide) triblock copolymer (EO(39)BO(47)EO(39)), tetraethyl orthosilicate (TEOS) and trimethyl-benzene (TMB). Large pore FDU-1 silica was obtained by using the following gel composition 1TEOS:0.00735B50-6600:0.00735TMB:6HCl:155H(2)O. The pristine material exhibited a BET specific surface area of 684 m(2) g(-1), total pore volume of 0.89 cm(3) g(-1), external surface area of 49 m(2) g(-1) and microporous volume of 0.09 cm(3) g(-1). The enzyme activity was determined by the Flow Injection Analysis-Chemiluminescence (FIA-CL) method. For GOD immobilized on the FDU-1 silica, GOD supernatant and GOD solution, the FIA-CL results were 9.0, 18.6 and 34.0 U, respectively. The value obtained for the activity of the GOD solution with FIA-CL method is in agreement with the 35 U, obtained by spectrophotometry. (C) 2011 Elsevier B.V. All rights reserved.

Adsorption of Pb(2+), Cu(2+) and Cd(2+) in FDU-1 silica and FDU-1 silica modified with humic acid

Ordered mesoporous silica with cubic structure, type FDU-1, was synthesized under strong acid media using B-50-6600 poly(ethylene oxide)-poly(butilene oxide)-poly(ethylene oxide) triblock copolymer (EO(39)BO(47)EO(39)) and tetraethyl orthosilicate (TEOS). Humic acid (HA) was modified to the synthesis process at a concentration of 1.5 mmol per gram of SiO(2). Thermogravimetry, small angle X-ray diffraction, nitrogen adsorption and high resolution transmission electron microscopy were used to characterize the samples. The pristine FDU-1 and FDU-1 with incorporated 1.5 mmol of HA were tested for adsorption of Pb(2+), Cu(2+) and Cd(2+) in aqueous solution. Incorporation of humic acid into the FDU-1 silica afforded an adsorbent with strong affinity for Cd(2+), Cu(2+) and Pb(2+) from single ion solutions. Adsorption of Cu(2+) was significantly enhanced after incorporation of humic acid, a fact that can be explained by the formation of complexes with carboxylic and phenolic groups at low concentrations of the metal cation. The results demonstrated the potential applicability of FDU-1 with incorporated HA in the removal of low concentrations of heavy metal cations from aqueous solution, such as wastewaters, after usual precipitation of metal hydroxides in alkaline medium and proper pH conditioning in the range between 6 and 7. (C) 2007 Elsevier Inc. All rights reserved.

Caracterização dos eletrocatalisadores LaMnO3, LaFeO3, LaFe0,2Mn0,8O3 E La0,5Fe0,5MnO3 preparados por autocombustão assistida por microondas para cátodos de células a combustível do tipo SOFC

Materials consisting of perovskite-type oxides (ABO3) have been developed in this work for applications in fuel cell cathodes of solid oxide type (SOFC). These ceramic materials are widely studied for this type of application because they have excellent electrical properties, conductivity and electrocatalytic. The oxides LaMnO3, LaFeO3, LaFe0.2Mn0.8O3 e La0.5Fe0.5MnO3 were synthesized by the method of microwave assisted combustion and after sintering at 800°C in order to obtain the desired phases. The powders were characterized by thermogravimetry (TG), X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM) and voltammetric analysis (cyclic voltammetry and polarization curves). The results obtained by XRF technique showed that the microwave synthesis method was effective in obtaining doping oxides with values near stoichiometric. In general, powders were obtained with particle size less than 0.5 μm, having a porous structure and uniform particle size distribution. The particles showed spherical form, irregular and crowded of varying sizes, according to the analysis of SEM. The behavior of the oxides opposite the thermal stability was monitored by thermogravimetric curves (TG), which showed low weight loss values for all samples, especially those of manganese had its structure. By means of Xray diffraction of the samples sintered at 800°C was possible to observe the formation of powders having high levels of crystallinity. Furthermore, undesirable phases such as La2O3 and MnOx were not identified in the diffractograms. These phases block the transport of oxygen ions in the electrode/electrolyte interface, affecting the electrochemical activity of the system. The voltammetric analysis of the electrocatalysts LF-800, LM-800, LF2M8-800 e L5F5M-800 revealed that these materials are excellent electrical conductors, because it increased the passage of electrical current of the working electrode significantly. Best performance for the oxygen reduction reaction was observed with iron-rich structures, considering that the materials obtained have characteristics suitable for use in fuel cell cathodes of solid oxide type

Síntese de nanocatalisador cerâmico a base de SnO2 pelo método hidrotermal assistido por micro-ondas aplicado a reação de transesterificação do óleo de babaçu

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

Electrocatalytic performance of environmentally friendly synthesized gold nanoparticles towards the borohydride electro-oxidation reaction

In this paper we report a simple and environmentally friendly synthesis of gold nanoparticles (AuNps) and their electrocatalytic activity for borohydride oxidation reaction (BOR). Ultraviolet spectroscopy (UV- vis) and transmission electron microscopy (TEM) confirmed the formation of poly(vinyl pyrrolidone)protected colloidal AuNps through direct reduction of Au3+ by glycerol in alkaline medium at room temperature. For the BOR tests the AuNps were directly produced onto carbon to yield the Au/C catalyst. Levich plots revealed that the process occured via 7.2 electrons, therefore near the theoretical value of 8 electrons. When compared to bulk Au, the gold nanoparticles presented enhanced catalytic properties since the onset potential for BOR was shifted 200 mV towards negative potentials. (C) 2012 Elsevier B.V. All rights reserved.