18 resultados para Nanostructured film
em Repositório Institucional UNESP - Universidade Estadual Paulista "Julio de Mesquita Filho"
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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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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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The electrochemical preparation described herein involved the electrocatalytic oxidation of sulfite on a platinum electrode modified with nanostructured copper salen (salen=N,N'-ethylenebis(salicylideneiminato)) polymer films. The complex was prepared and electropolymerized at a platinum electrode in a 0.1 mol L-1 solution of tetrabutylammonium perchlorate in acetonitrile by cyclic voltammetry between 0 and 1.4V vs. SCE. After cycling the modified electrode in a 0.50 mol L-1 KCI solution, the estimated surface concentration was found to be equal to 2.2 x 10(-9) Mol cm(-2). This is a typical behavior of an electrode surface immobilized with a redox couple that can usually be considered as a reversible single-electron reduction/oxidation of the copper(II)/copper(III) couple. The potential peaks of the modified electrode in the electrolyte solution (aqueous) containing the different anions increase with the decrease of the ionic radius, demonstrating that the counter-ions influence the voltammetric behavior of the sensor. The potential peak was found to be linearly dependent upon the ratio [ionic charge]/[ionic radius]. The oxidation of the sulfite anion was performed at the platinum electrode at +0.9V vs. SCE. However, a significant decrease in the overpotential (+0.45V) was obtained while using the sensor, which minimized the effect of oxidizable interferences. A plot of the anodic current vs. the sulfite concentration for chronoamperometry (potential fixed = +0.45V) at the sensor was linear in the 4.0 x 10(-6) to 6.9 x 10(-5) mol L-1 concentration range and the concentration limit was 1.2 x 10(-6) mol L-1. The reaction order with respect to sulfite was determined by the slope of the logarithm of the current vs. the logarithm of the sulfite concentration. (C) 2009 Elsevier Ltd. All rights reserved.
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An amperometric oxygen sensor based on a polymeric nickel-salen (salen = N,N '-ethylenebis(salicydeneiminato)) film coated platinum electrode was developed. The sensor was constructed by electropolymerization of nickel-salen complex at a platinum electrode in acetonitrile/tetrabuthylamonium perchlorate by cyclic voltammetry. The voltammetric behavior of the modified electrode was investigated in 0.5 mol L-1 KCl solution in the absence and presende of molecular oxygen. A significant increased of cathodic peak current (at -0.20 vs. SCE) of the modified electrode with addition of oxygen to the solution was observed. This result shows that the nickel-salen film on the surface of the electrode promotes the reduction of oxygen. The reaction can be brought about electrochemically where in the nickel(II) complex is first reduced to a nickel(I) complex at the electrode surface. The nickel(I) complex then undergoes a catalytic oxidation by the oxygen molecular in solution back to the nickel(II) complex, which can then be electrochemically re-reduced to produce an enhancement of the cathodic current. The plot of the cathodic current versus the dissolved oxygen concentration for chronoamperometry (potential fixed = -0.20 V) at the sensor was linear in the concentration range of 3.95 to 9.20 mg L-1 with concentration limit of 0.17 mg L-1 O-2. The modified electrode proposed is useful for the quality control and routine analysis of dissolved oxygen in commercial water and environmental water samples. The results obtained for the levels of dissolved oxygen are in agreement with the results obtained with an O-2 commercial sensor. (C) 2011 Published by Elsevier Ltd.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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The effect of the Sb addition on the microstructural and electrical conductivity of the SnO2 thin film was studied in this work. Experimental results show that the Sb addition allowed to control the grain size and electrical conductivity of the SnO2 thin film, resulting in a nanostructured material. The nanostructured Sb-doped SnO2 thin films present high electrical conductivity, even in the presence of high porosity, supporting the hypothesis that nanostructured material must possess strong electrical conductivity. This work involves important aspects that can be applied to the development of high performance transparent conducting thin film. (C) 2003 Elsevier B.V. All rights reserved.
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dThe detection of aromatic compounds from pesticides and industrial wastewater has become of great interest, since these compounds withstand chemical oxidation and biological degradation, accumulating in the environment. In this work, a highly sensitive biosensor for detecting catechol was obtained with the immobilization of Cl-catechol 1,2-dioxygenase (CCD) in nanostructured films. CCD layers were alternated with poly(amidoamine) generation 4 (PAMAM G4) dendrimer using the electrostatic layer-by-layer (LbL) technique. Circular dichroism (CD) measurements indicated that the immobilized CCD preserved the same conformation as in solution. The thickness of the very first CCD layers in the LbL films was estimated at ca. 3.6 nm, as revealed by surface plasmon resonance (SPR). PAMAM/CCD 10-bilayer films were employed in detecting diluted catechol solutions using either an optical or electrical approach. Due to the mild immobilization conditions employed, especially regarding the pH and ionic strength of the dipping solutions, CCD remained active in the films for periods longer than 3 weeks. The optical detection comprised absorption experiments in which the formation of cis-cis muconic acid, resulting from the reaction between CCD and catechol, was monitored by measuring the absorbance at 260 nm after film immersion in catechol solutions. The electrical detection was carried out using LbL films deposited onto gold-interdigitated electrodes immersed in aqueous solutions at different catechol concentrations. Using impedance spectroscopy in a broad frequency range (1Hz-1kHz), we could detect catechol in solutions at concentrations as low as 10(-10) M. (c) 2005 Elsevier B.V. All rights reserved.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Chemical sensors made from nanostructured films of poly(o-ethoxyaniline) POEA and poly(sodium 4-styrene sulfonate) PSS are produced and used to detect and distinguish 4 chemicals in solution at 20 mM, including sucrose, NaCl, HCl, and caffeine. These substances are used in order to mimic the 4 basic tastes recognized by humans, namely sweet, salty, sour, and bitter, respectively. The sensors are produced by the deposition of POEA/PSS films at the top of interdigitated microelectrodes via the layer-by-layer technique, using POEA solutions containing different dopant acids. Besides the different characteristics of the POEA/PSS films investigated by UV-Vis and Raman spectroscopies, and by atomic force microscopy.. it is observed that their electrical response to the different chemicals in liquid media is very fast, in the order of seconds, systematical, reproducible, and extremely dependent on the type of acid used for film fabrication. The responses of the as-prepared sensors are reproducible and repetitive after many cycles of operation. Furthermore, the use of an "electronic tongue" composed by an array of these sensors and principal component analysis as pattern recognition tool allows one to reasonably distinguish test solutions according to their chemical composition. (c) 2007 Published by Elsevier B.V.
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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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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Four lignin samples were extracted from sugar cane bagasse using four different alcohols (methanol, ethanol, n-propanol, and 1-butanol) via the organosolv-CO2 supercritical pulping process. Langmuir films were characterized by surface pressure vs mean molecular area (Pi-A) isotherms to exploit information at the molecular level carrying out stability tests, cycles of compression/expansion (hysteresis), subphase temperature variations, and metallic ions dissolved into the water subphase at different concentrations. Briefly, it was observed that these lignins are relatively stable on the water surface when compared to those obtained via different extraction processes. Besides, the Pi-A isotherms are shifted to smaller molecular areas at higher subphase temperatures and to larger molecular areas when the metallic ions are dissolved into the subphase. The results are related to the formation of stable aggregates (domains) onto the water subphase by these lignins, as shown in the Pi-A isotherms. It was found as well that the most stable lignin monolayer onto the water subphase is that extracted with 1-butanol. Homogeneous Langmuir-Blodgett (LB) films of this lignin could be produced as confirmed by UV-vis absorption spectroscopy and the cumulative transfer parameter. In addition, FTIR analysis showed that this lignin LB film is structured in a way that the phenyl groups are organized preferentially parallel to the substrate surface. Further, these LB films were deposited onto gold interdigitated electrodes and ITO and applied in studies involving the detection of Cd+2 ions in aqueous solutions at low concentration levels throughimpedance spectroscopy and electrochemical measurements. FTIR spectroscopy was carried out before and after soaking the thin films into Cd+2 aqueous solutions, revealing a possible physical interaction between the lignin phenyl groups and the heavy metal ions. The importance of using nanostructured systems is demonstrated as well by comparing both LB and cast films.
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Tin oxide thin films doped with 7 mol% antimony oxide multilayer were prepared by the polymeric precursor method. Morphological characterization revealed films with round-shaped grains, nanometric size (similar to 13 nm), and low roughness. These films display high transmittance (similar to 80%) in the visible range of transmittance spectra, which is desirable for transparent conductive oxide films. Analysis on electrical resistivity versus temperature data showed two different conduction mechanisms toward the temperature range. The gas sensor properties measurement of the thicker thin film revealed good sensibility for the NOx. (c) 2006 Elsevier B.V. All rights reserved.