Structural and electrochemical properties of LiCoO2 prepared by combustion synthesis

LiCoO2 powders were prepared by combustion synthesis, using metallic nitrates as the oxidant and metal sources and urea as fuel. A small amount of the LiCoO2 phase was obtained directly from the combustion reaction, however, a heat treatment was necessary for the phase crystallization. The heat treatment was performed at the temperature range from 400 up to 700 degreesC for 12 h. The powders were characterized by X-ray diffraction (XRD), X ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and specific surface area values were obtained by BET isotherms. Composite electrodes were prepared using a mixture of LiCoO2, carbon black and poly(vinylidene fluoride) (PVDF) in the 85:10:5% w/w ratio. The electrochemical behavior of these composites was evaluated in ethylene carbonate/dimethylcarbonate solution, using lithium perchlorate as supporting electrolyte. Cyclic voltammograms showed one reversible redox process at 4.0/3.85 V and one irreversible redox process at 3.3 V for the LiCoO2 obtained after a post-heat treatment at 400 and 500 degreesC.Raman spectroscopy showed the possible presence of LiCoO2 with cubic structure for the material obtained at 400 and 500 degreesC. This result is in agreement with X-ray data with structural refinement for the LiCoO2 powders obtained at different temperatures using the Rietveld method. Data from this method showed the coexistence of cubic LiCoO2 (spinel) and rhombohedral (layered) structures when LiCoO2 was obtained at lower temperatures (400 and 500 degreesC). The single rhombohedral structure for LiCoO2 was obtained after post-heat treatment at 600 degreesC. The maximum energy capacity in the first discharge was 136 mA g(-1) for the composite electrode based on LiCoO2 obtained after heat treatment at 700 degreesC. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Immobilization and electrochemical properties of anionic complexes on a V2O5/surfactant nanocomposite

in this work, we report a new way of modifying an electrode by combining the intrinsic conductivity property of vanadium pentoxide xerogel with its water insolubility in the presence of the cationic surfactant N-cetyl-N,N,N,trimethyl-ammonium bromide (CTA(+)Br(-)). The obtained hybrid compound enables the immobilization of electroactive anions such as hexacyanoferrate (III) ([Fe(CN)(6)](3-)) and its analogue pentacyanonitrosylferrate (II) ([Fe(CN)(5)NO](2-)), rather than cations. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Electrochemical Properties of Oxo-Manganese Complex Biomimicking Enzyme Active Sites and Its Electrocatalytic Application for Dopamine Determination

This work describes the characterization of the [Mn2 IV,IVO2(terpy)2(H2O)2]4+ complex in aqueous solution by UV-vis spectrophotometry, cyclic voltammetry, and linear sweep voltammetry with a rotating disk electrode. The pH effect, potential scan rate, effect of perfluorosulfonate polymer, and anion of supporting electrode on the electrochemical behavior of the modified electrode for better performance were investigated. The potential peak of the modified electrode was linearly dependent upon the ratio [ionic charge]/[ionic radius]. The modified electrode exerted an electrocatalytic effect on dopamine oxidation in aqueous solution with a decrease in the overpotential compared with the unmodified glassy carbon electrode. This way, the modified electrode showed an enzymatic biomimicking behavior. Tafel plot analyses were used to elucidate the kinetics and mechanism of dopamine oxidation. © 2013 Springer Science+Business Media New York.

Electrochemical Properties of the Oxo-Manganese-Phenanthroline Complex Immobilized on Ion-Exchange Polymeric Film and Its Application as Biomimetic Sensor for Sulfite Ions

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

Structural and Electrochemical Properties of Lutetium Bis-Octachloro-Phthalocyaninate Nanostructured Films. Application as Voltammetric Sensors

Thin films of the bis[2,3,9,10,16,17,23,24-octachlorophthalocyaninate] lutetium(III) complex (LuPc2Cl32) have been prepared by the Langmuir-Blodgett and the Langmuir-Schaefer (LS) techniques. The influence of the chlorine substituents in the structure of the films and in their spectroscopic, electrochemical and sensing properties has been evaluated. The pi-A isotherms exhibit a monolayer stability greater than the observed in the unsubstituted analogue (LuPc2), being easily transferred to solid substrates, also in contrast to LuPc2. The LB and LS films present a linear growth forming stratified layers, monitored by UV-VIS absorption spectroscopy. The latter also revealed the presence of LuPc2Cl32 in the form of monomers and aggregates in both films. The FTIR data showed that the LuPc2Cl32 molecules present a non-preferential arrangement in both films. Monolayers of LB and LS were deposited onto 6 nm Ag island films to record surface-enhanced resonance Raman scattering (SERRS), leading to enhancement factors close to 2 x 10(3). Finally, LB and LS films deposited onto ITO glass have been successfully used as voltammetric sensors for the detection of catechol. The improved electroactivity of the LB and LS films has been confirmed by the reduction of the overpotential of the oxidation of catechol. The enhancement of the electrocatalytic effect observed in LB and LS films is the result of the nanostructured arrangement of the surface which increases the number of active sites. The sensors show a limit of detection in the range of 10(-5) mol/L.

Complementary study on the electrical and structural properties of poly(3-alkylthiophene) and its copolymers synthesized on ITO by electrochemical impedance and Raman spectroscopy

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Microstructural and electrochemical study of La0.5Li0.5TiO3

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

Effect of cerium on structure modifications of a hybrid sol-gel coating, its mechanical properties and anti-corrosion behavior

An organic-inorganic hybrid coating was developed to improve the corrosion resistance of the aluminum alloy AA 2024-T3. Organic and inorganic coatings derived from glycidoxypropyltrimethoxysilane (GPTMS) and aluminum tri-sec-butoxide Al((OBu)-Bu-s)(3), with different cerium contents, were deposited onto aluminum by dip-coating process. Corrosion resistance and mechanical properties were investigated by electrochemical impedance measurements and nano-indentation respectively. An optimal cerium concentration of 0.01 M was evidenced. To correlate and explain the hybrid coating performances in relation to the cerium content, NMR experiments were performed. It has been shown that when the cerium concentration in the hybrid is higher than 0.01 M there are important modifications in the hybrid structure that account for the mechanical properties and anti-corrosion behavior of the sol-gel coating. (C) 2012 Elsevier Ltd. All rights reserved.

Spectroscopic and electrochemical characterization of polyaniline and a ruthenium complex, mer-[RuCl3(dppb)(py)], in the form of Langmuir-Blodgett films

Langmuir monolayers and Langmuir-Blodgett (LB) films have been produced from polyaniline and a biphosphinic ruthenium complex, referred to as Rupy. Strong, repulsive interaction between the two components led to a nonlinear change in area per molecule and surface potential with the concentration of Rupy in the mixed film. Molecular interaction was also denoted in the spectroscopic and electrochemical properties of the Y-type LB transferred films. The Raman spectra of mixed PANI-Rupy films indicated that the degree of oxidation of PANI increased linearly with the concentration of Ropy. With PANI being increasingly oxidized by presence of Rupy, the electroactivity of the mixed films decreased with the amount of Rupy, to become undetectable when the mixed LB film is 501 mol in Rupy. The presence of Rupy caused the electrical properties of the mixed LB films to be less sensitive to environmental changes. The electrical capacitance of a mixed film changed only by 15% when the sample was taken from vacuum to air, whereas the change was 215% for a pure PANI LB film.

The relation between structural features and electrochemical activity of MnO2 nanoparticles synthesized from a polyol-made Mn 3O4 precursor

A simple hybrid synthesis processing method was developed to synthesize γ-MnO2 nanocrystalline particles. The polyol method was modified by the addition of nitric acid in order to allow the synthesizing of single-phase Mn3O4 in a large scale. In the sequence, the acid digestion technique was used to transform Mn3O4 into γ-MnO2. Structural and morphological characterization was carried out by X-ray diffractometry, Infrared and Raman spectroscopy, thermogravimetric analysis, nitrogen adsorption isotherm, scanning electron microscopy, and transmission electron microscopy. The electrochemical properties were investigated by cyclic voltammetry and galvanostatic charge-discharge measurements. The synthesized material exhibits a specific capacitance of 125.1 F g-1 at a mass loading of 0.98 mg cm-2. The relation between structural features and electrochemical activity is discussed by comparing the synthesized material with commercial electrolytic manganese dioxide. © 2013 Springer-Verlag Berlin Heidelberg.

Rapid preparation of alpha-FeOOH and alpha-Fe2O3 nanostructures by microwave heating and their application in electrochemical sensors

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Study of the potentiometric response of the doped spinel Li1.05Al0.02Mn1.98O4 for the optimization of a selective lithium ion sensor

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Iron phthalocyanine in non-aqueous medium forming layer-by-layer films: growth mechanism, molecular architecture and applications

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

Deposition and characterization of BiVO4 thin films and evaluation as photoanodes for methylene blue degradation

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Electrocatalysis on noble metal and noble metal alloys dispersed on high surface area carbon

In this work, a simple route to prepare carbon supported Pt/C, Pt:Ru/C, Pt:Mo/C and Pt:Ru:Mo/C catalysts is reported. The electrochemical properties of the several carbon materials used as substrates in the absence and in the presence of supported platinum and platinum alloys catalysts were investigated using cyclic voltammetry and employing the thin porous coating electrode technique. The activity of the dispersed catalysts composed of Pt/C with respect to the oxygen reduction and of alloy/C with respect to methanol oxidation was investigated using steady state polarization measurements. The performance with respect to the oxygen reduction reaction of the Pt/C catalyst prepared on heat-treated Vulcan carbon substrate is equivalent to that reported in the literature for the state-of-the-art electrocatysts. Pt:Ru:Mo/C samples prepared in this work presented the higher catalytic effect for methanol electro-oxidation.