Electric measurements with constant current: A practical method for characterizing dielectric films

This article assesses the use of the constant current (CC) method for characterizing dielectric films. The method is based on charging the sample with a constant current (current stress) and measuring the corresponding voltage rise under the closed circuit condition. Our article shows that the CC method is an alternative to the constant voltage stressing method to study the electric properties of nonpolar, ferroelectric, and polar polymers. The method was tested by determining the dielectric constant of polytetrafluoroethylene, and investigating the electric conduction in poly(ethylene terephthalate). For the ferroelectric polymer poly(vinylidene fluoride), it is shown that hysteresis loops and the dependence of the ferroelectric polarization on the electric field can be obtained. (C) 2001 American Institute of Physics.

Doping of polyaniline by corona discharge

In the present article it is shown that a corona discharge can be employed to dope thin films of polyaniline (PANI) coated on poly(ethylene terephthalate) films, allowing the electrical conductivity to be tuned within the range 10(-10) to 0.3 S cm(-1). A study of the effect of different corona conditions, namely corona treatment for positive and negative polarities, air humidity, treatment time, corona current, and the geometry of the corona triode, on the electrical conductivity of the polyaniline is presented. The results indicate that the corona discharge leads to protonic doping of polyaniline similar to that which occurs in conventional protonic acid solution doping. Atomic force microscopic analysis shows that, as the PANI is exposed to the corona discharge, its globular morphology is disrupted leading to the appearance of droplet-like features and a significant decrease in the average height and surface roughness. Doping by corona discharge presents several advantages over the conventional solution method namely that it is a dry process which does not require use of chemicals reagents, and which is both rapid and avoids dopant migration. The latter can be important for applications of PANI in microelectronic devices. (C) 2000 American Institute of Physics. [S0021-8979(00)01608-X].

Mechanical properties, hydrophilicity and water activity of starch-gum film: effect of additives and deacetylated xanthan gum

The effect of deacetylated xanthan gum, additives (sucrose, soybean oil, sodium phosphate and propylene glycol) and pH modifications on mechanical properties, hydrophilicity and water activity of cassava starch-xanthan gum films has been studied. Sucrose addition resulted in the highest effect observed on cassava starch films elongation at break. The deacetylated xanthan gum had higher effect on elongation at break when comparing to the acetylated gum, although both gums presented an inferior effect in relation to the obtained with sucrose. However, when comparing to the control and PVC films, lower tensile strength resistance values were observed when adding sucrose. Increased water activity was observed for films added with sucrose, thus, increasing the material biodegradation. Sucrose and deacetylated xanthan gum addition resulted in a slight hydrophilicity increase. (C) 2004 Elsevier Ltd. All rights reserved.

Cracks developed during SrTiO3 thin-film preparation from polymeric precursors

Strontium titanate (SrTiO3) thin films were prepared by dip-coating Si(111) single-crystal substrates in citrate solutions of ethylene glycol, considering several citric acid/ethylene glycol (CA/EG) ratios. Measurements of intrinsic viscosity indicate that increasing the amount of EG increases the precursors' polymeric chains and increases the weight loss. After deposition the substrates were dried on a hotplate (approximate to 150 degrees C); this was followed by heat treatment at temperatures ranging from 500 to 700 degrees C using heating and cooling rates of 1 degrees C min(-1). SEM and optical microscopy investigations of the sintered films obtained from different CA/EG ratios indicate that there is a critical thickness above which the films present cracks. This critical thickness for SrTiO3 films deposited on the Si(111) substrate is about 150 nm, Measurements of crack spacing as a function of film thickness indicate that the origin of cracks cannot be explained by the elastic behavior of the film but rather by the viscoelastic relaxation of the film during pyrolysis and sintering. Copyright (C) 1999 John Wiley & Sons, Ltd.

Indium tin oxide films prepared via wet chemical route

In this work, indium tin oxide (ITO) films were prepared using a wet chemical route, the Pechini method. This consists of a polyesterification reaction between an alpha-hydroxicarboxylate complex (indium citrate and tin citrate) with a polyalcohol (ethylene glycol) followed by a post annealing at 500 degrees C. A 10 at.% of doping of Sn4+ ions into an In2O3 matrix was successfully achieved through this method. In order to characterize the structure, the morphology as well as the optical and electrical properties of the produced ITO films, they were analyzed using different experimental techniques. The obtained films are highly transparent, exhibiting transmittance of about 85% at 550 nm. They are crystalline with a preferred orientation of [222]. Microscopy discloses that the films are composed of grains of 30 nm average size and 0.63 nm RMS roughness. The films' measured resistivity, mobility and charge carrier concentration were 5.8 x 10(-3) Omega cm, 2.9 cm(2)/V s and -3.5 x 10(20)/cm(3), respectively. While the low mobility value can be related to the small grain size, the charge carrier concentration value can be explained in terms of the high oxygen concentration level resulting from the thermal treatment process performed in air. The experimental conditions are being refined to improve the electrical characteristics of the films while good optical, chemical, structural and morphological qualities already achieved are maintained. (C) 2007 Elsevier B.V. All rights reserved.

Chemical vapor deposition of multi-walled carbon nanotubes from nickel/yttria-stabilized zirconia catalysts

Multi-walled carbon nanotubes (MWNT) were produced by chemical vapor deposition using yttria-stabilized zirconia/nickel (YSZ/Ni) catalysts. The catalysts were obtained by a liquid mixture technique that resulted in fine dispersed nanoparticles of NiO supported in the YSZ matrix. High quality MWNT having smooth walls, few defects, and low amounts of by-products such as amorphous carbon were obtained, even from catalysts with large Ni concentrations (> 50 wt.%). By adjusting the experimental parameters, such as flux of the carbon precursor (ethylene) and Ni concentration, both the MWNT morphology and the process yield could be controlled. The resulting YSZ/Ni/MWNT composites can be interesting due to their mixed ionic-electronic transport properties, which could be useful in electrochemical applications.

Thermal degradation of geomembranes after exposure to heat

HDPE and PVC geomembranes are sensitive to changes in their properties when in contact with high temperatures. The effects of hot temperature on polymeric geomembranes are assessed by the ASTM D794 and ASTM D5721.This paper brings an analysis of degradation of the Poly Vinyl Chloride (PVC) and High Density Poly Ethylene (HDPE) geomembranes when exposed to conventional and air oven after specific periods.. Mechanical and physical properties were evaluated. OIT tests were also performanced to evaluate the level of oxidation degradation occurred on the HDPE geomembranes. Geomembranes of two thicknesses were tested: 1.0, 2.0 nun (PVC) and 0.8, 2.5 mm, (HDPE). The results obtained show, for example, that after the last period of exposure, the PVC geomembranes (1.0, 2.0 mm) were more rigid and stiffer than fresh samples. The HDPE geomembranes, on the other hand, when exposed to heat presented increases in deformation. OIT tests showed efficient to detect some level of degradation on the HDPE geomembranes.

Room temperature co-precipitation of nanocrystalline CeO2 and Ce0.8Gd0.2O1.9-delta powder

This paper describes a simple method to co-precipitate CeO2 and Ce0.8Gd0.2O1.9-delta with ammonium hydroxide from solvents such as: water, ethylene glycol, ethyl alcohol and isopropyl alcohol. Characterization by Raman spectroscopy and XRD evidenced the formation of a solid solution of gadolinium-doped ceria at room temperature. Nanometric particles with crystallite size of 3.1 nm were obtained during synthesis using ethyl alcohol as solvent. This is a promising result compared with those mentioned in the literature, in which the smallest crystallite size reported was, 6.5 nm. (c) 2006 Elsevier B.V. All rights reserved.

Synthesis and some properties of hybrid gels of titanium oxide containing europium (III)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Synthesis and properties of branched polyethylene/high-density polyethylene blends using a homogeneous binary catalyst system composed of early and late transition metal complexes

Branched polyethylene/high-density polyethylene blends (BPE/HDPE) with a wide range of molecular weights, melt flow indexes (MFI), and intrinsic viscosity were prepared using the homogeneous binary catalyst system composed by Ni(alpha-diimine)Cl-2 (1) (alpha-diimine = 1,4-bis(2,6-diisopropylphenyl)-acenaphthenediimine) and {Tp(Ms*)} TiCl3 (2) (Tp(Ms*)=hydridobis(3-mesitylpyrazol-1-yl)(5-mesityl-pyrazol-1-yl)) activated with MAO and/or TIBA in hexane at two different polymerization temperatures (30 and 55 degreesC) and by varying the nickel loading molar fraction (x(Ni)). At all Temperatures, a non-linear correlation between the x(Ni) and the productivity was observed, suggesting the occurrence of a synergistic effect between the nickel and the titanium catalyst precursors, which is more pronounced at 55 degreesC. The molecular weight of the BPE/HDPE blends considerably decreases with increasing Al/M molar ratio. The melt flow indexes (MFI) and intrinsic viscosities (eta) are strongly affected by x(Ni), but the melting temperatures are nearly constant, 132 +/- 3 degreesC. Dynamic mechanical thermal analysis (DMTA) shows the formation of different polymeric materials where the stiffness vanes according, to the x(Ni) and temperature used in the polymerization reaction. The surface morphology of the BPE/HDPE blends studied by scanning electron microscopy (SEM) revealed a low miscibility between the PE phases resulting in the formation of a sandwich structure after etching with o-xylene.

Combination of nickel and titanium complexes containing nitrogen ligands as catalyst for polyethylene reactor blending

Ethylene was polymerized using a combination of Ni(diimine)Cl-2 (1) (diimine = 1,4-bis(2,6-di-isopropylphenyl)-acenaphthenediimine) and {Tp(Ms)*} TiCl3 (2) (Tp(Ms)* = hydridobis(3-mesitylpyrazol-1-yl)(5-mesityl-pyrazol-1-yl)) compounds in the presence of methyl-aluminoxane (MAO) at 30 degrees C. The productivity reaches a maximum at X-Ni = 0.75 (1400 kg of PE/mol[M] . h), and the produced polyethylene (PE) showed maximal melt flow index (0.13 g/10 min) and minimal intrinsic viscosity (2.24 dL/g) compared to polyethylenes obtained with different values of nickel loading fractions (X-Ni). Productivity intrinsic viscosity data, as well as melt flow index measurements markedly depend upon the content of the late transition metal, thus suggesting a synergic effect between nickel and titanium catalysts.

Characterization of an all sol-gel electrochromic device WO3/Ormolyte/CeO2-TiO2

Electrochemical lithium intercalation in thin films of CeO2-TiO2 and WO3, prepared by the sol-gel technique was investigated with cyclic voltammetry and spectroelectrochemical techniques in propylene carbonate solutions. A solid state system having the configuration WO3/Ormolyte/CeO2-TiO2 has been assembled. The solid electrolyte, an organically modified electrolyte (ormolyte), was prepared with different [O]/[Li] ratios. The transmittance variation of this system during a potentiostatic step from -0.7 V to 0.8 V was about 35% at 550 nm.

Kinetic parameters of polymer degradation by SAPO-37

High density poly(ethylene) has been submitted to thermal degradation alone, and in the presence of silicoaluminophosphate SAPO-37. The processes were carried out in a reactor connected on line to a gas chromatograph/mass spectrometer in order to analyze the evolved products. Polymer degradation was also evaluated by thermogravimetry, from room temperature until 800 degreesC, under nitrogen dynamic atmosphere, with multiple heating rates. From TG curves, the activation energy related to degradation process was calculated using the Flynn and Wall multiple heating rate kinetic model for pure polymer (PE) and for polymer in the presence of catalyst (PE/S37). SAPO-37 showed good selectivity for low molecular mass hydrocarbons in PE catalytic degradation.

Multi-scale structural description of siloxane-PPO hybrid ionic conductors doped by sodium salts

Alkaline metal doped organic - inorganic hybrids have potential applications in the field of portable energy sources. Attractive sol - gel derived urea cross-linked polyether, siloxane - PPO ( poly( propylene oxide)) hybrids doped with sodium salts ( NaClO4 and NaBF4) were examined by multi-spectroscopic approach that includes complex impedance, X-ray powder diffraction (XRPD), small angle X-ray scattering (SAXS), Si-29 and Na-23 magic-angle spinning nuclear magnetic resonance (NMR/MAS), Na K-edge X-ray absorption near edge structure (XANES) and Raman spectroscopies. The goals of this work were to determine which cation coordinating site of the host matrix ( ether oxygen atoms or carbonyl oxygen atoms) is active in each of the materials analyzed, its influence on the nanostructure of the samples and its relation with the thermal and electrical properties. The main conclusion derived from this study is that the NaBF4 salt has a much lower solubility in the hybrid matrix than the NaClO4 salt. Furthermore, the addition of a large amount of salt plays a major role in the hybrid nanostructure and electrical properties, modifying the PPO chain conformation, weakening or breaking the hydrogen bond of the polyether - urea associations and changing the polycondensation and aggregation processes involving the siloxane species.

Synthesis of nanocrystalline tetragonal zirconia by a polymeric organometallic method

A polymeric precursor method based on the Pechini process was successfully used to synthesize zirconia-12 mol% ceria ceramic powders, the influence of the main process variables (citric acid-ethylene glycol ratio, citric acid-total oxides ratio and calcination temperature) on phase formation and powder morphology (surface area and crystallite size) were investigated. The thermal decomposition behavior of the precursor is presented. X-ray diffraction (XRD) patterns of powders revealed a crystalline tetragonal zirconia single-phase, with crystallite diameter ranging from 6 to 15 nm. The BET surface areas were relatively high, reaching 95 m(2) g(-1) Nitrogen adsorption/desorption on the powders suggested that nonaggregated powders could be attained, depending on the synthesis conditions. Copyright (C) 1999 John Wiley & Sons, Ltd.