Sensor arrays to detect humic substances and Cu(II) in waters

The interaction between poly(o-ethoxyaniline) (POEA) adsorbed onto solid substrates and humic substances (HS) and Cu(2+) ions has been investigated using UV-vis spectroscopy and atomic force microscopy (AFM). Both HS and Cu(2+) are able to dope POEA and change film morphology. This interaction was exploited in a sensor array made with nanostructured films of POEA, sulfonated lignin and HS, which could detect small concentrations of HS and Cu(2+) in water. (C) 2009 Elsevier B.V. All rights reserved.

Modification of surface properties of Ti-16Si-4B powder alloy by plasma immersion ion implantation

Results of the surface modification of Ti-16Si-4B powder alloy by nitrogen ion implantation are presented, together with the experimental description of the preparation of that powder by high-energy ball milling and hot pressing. The phase structure, chemical composition and morphology of sample surfaces were observed by utilizing X-ray diffractometer (XRD), atomic force microscope (AFM) and scanning electron microscopy (SEM). A tribological characterization was carried out with a ball-on-disc tribometer and an SEM. Friction coefficient is compared with the one obtained for Ti-6Al-4V alloy and the wear scars characterized by SEM/EDS (energy dispersive spectroscopy). The concentration profile of the detected elements have been investigated using Auger electron spectroscopy (AES) depth profiling. Our results show that a shallow implanted layer of oxygen and nitrogen ions were obtained at the Ti-16Si -4B alloy surface, sufficient to modify slightly its tribological properties. Crown Copyright (C) 2011 Published by Elsevier Ltd. All rights reserved.

A comparison between neodymium doped alumina samples obtained by Pechini and sol-gel methods using thermo-stimulated luminescence and SEM

Neodymium doped and undoped aluminum oxide samples were obtained using two different techniques: Pechini and sol-gel. Fine grained powders were produced using both procedures, which were analyzed using Scanning Electron Microscopy (SEM) and Thermo-Stimulated Luminescence (TSL). Results showed that neodymium ions incorporation is responsible for the creation of two new TSL peaks (125 and 265 degrees C) and, also, for the enhancement of the intrinsic TSL peak at 190 degrees C. An explanation was proposed for these observations. SEM gave the dimensions of the clusters produced by each method, showing that those obtained by Pechini are smaller than the ones produced by sol-gel; it can also explain the higher emission supplied by the first one. (C) 2010 Elsevier B.V. All rights reserved.

Effects of interactions between algal densities and cadmium concentrations on Ceriodaphnia dubia fecundity and survival

The influence of different densities of the algae Pseudokirchneriella subcapitata on the chronic toxicity of cadmium to Ceriodaphnia dubia was investigated. The importance of algal cells as a source of metal to zooplankton was studied by exposing P. subcapitata cells to free cadmium ions and supplying the algae as food to C. dubia. The results of a bifactorial analysis (metal versus food levels) showed that metal toxicity to zooplankton was dependent on food level. Significant toxic effects on the fecundity and survival of C. dubia were observed at low metal concentrations with high algal density. Algae contaminated with Cd2+ were less toxic to cladoceran than was the Cd2+ in solution. Green algae retained cadmium and released low metal concentration in the test medium. We concluded that algal cells are an important route of exposure to metal and a factor that has an appreciable influence on the expression of metal toxicity to daphnids. (C) 2007 Elsevier Inc. All rights reserved.

Influence of chloride ion concentration and temperature on the electrochemical properties of passive films formed on a superduplex stainless steel

Polarization measurements were conducted to monitor the corrosion behavior of superduplex stainless steel ASTM A995M-Gr.SA/EN 10283-Mat#1.4469(GX2CrNiMo26-7-4) when exposed to a) an electrolyte containing 22,700 parts per million (ppm) of chloride ions at seven different temperatures and b) an electrolyte at 25 GC and different chloride ion concentrations (5800, 22,700, 58,000 and 80,000 ppm of Cl(-)). The polarization curves indicate that the passive films formed are only slightly affected by NaCl concentration, but the pitting potential decreases drastically increasing the temperature, in particular >60 degrees C. The image analysis of the microstructure after potentiodynamic polarization showed that the pitting number and size vary in function of the temperature of the tested medium. Nyquist diagrams were determined by electrochemical impedance spectroscopy to characterize the resistance of the passive layer. According to Nyquist plots, the arc polarization resistance decreases increasing the temperature due to a catalytic degradation of the oxide passive films. (C) 2009 Elsevier Inc. All rights reserved.

Microstructural characteristics and corrosion behavior of a super duplex stainless steel casting

The machining of super duplex stainless steel castings is usually complicated by the difficulty involved in maintaining the dimensional tolerances required for given applications. Internal stresses originating from the solidification process and from subsequent heat treatments reach levels that exceed the material`s yield strength, promoting plastic strain. Stress relief heat treatments at 520 degrees C for 2 h are an interesting option to solve this problem, but because these materials present a thermodynamically metastable condition, a few precautions should be taken. The main objective of this work was to demonstrate that, after solution annealing at 1130 degrees C and water quenching, stress relief at 520 degrees C for 2 h did not alter the duplex microstructure or impair the pitting corrosion resistance of ASTM A890/A890M Grade 6A steel. This finding was confirmed by microstructural characterization techniques, including light optical and scanning electron microscopy, and X-ray diffraction. Corrosion potential measurements in synthetic sea water containing 20,000 ppm of chloride ions were also conducted at three temperatures: 5 degrees C, 25 degrees C and 60 degrees C. (c) 2008 Elsevier Inc. All rights reserved.

Model to predict the chloride penetration in concrete with profile forming peak: verification of its precision

Chloride attack in marine environments or in structures where deicing salts are used will not always show profiles with concentrations that decrease from the external surface to the interior of the concrete. Some profiles show an increase in chloride concentrations from when a peak is formed. This type of profile must be analyzed in a different way from the traditional model of Fick`s second law to generate more precise service life models. A model for forecasting the penetration of chloride ions as a function of time for profiles having formed a peak. To confirm the efficiency of this model, it is necessary to observe the behavior of a chloride profile with peak in a specific structure over a period of time. To achieve this, two chloride profiles with different ages (22 and 27 years) were extracted from the same structure. The profile obtained from the 22-year sample was used to estimate the chloride profile at 27 years using three models: a) the traditional model using Fick`s second law and extrapolating the value of C(S)-external surface chloride concentration; b) the traditional model using Fick`s second law and shifting the x-axis to the peak depth; c) the previously proposed model. The results from these models were compared with the actual profile measured in the 27-year sample and the results were analyzed. The model was presented with good precision for this study of case, requiring to be tested with other structures in use.

Sand bioconsolidation through the precipitation of calcium carbonate by two ureolytic bacteria

Two ureolytic strains, B. sphaericus LMG 22257 and Bacillus sp (I-001), were tested for their ability to consolidate sand by submitting them to two days` treatment using 10(7) viable cell concentrations of inocula and medium precipitation with calcium ions. The results showed that B. sphaericus LMG 22257 induced greater calcium carbonate formation. Both strains produced calcite and were able to consolidate sand. Tensile strength of consolidated sand was not a function of the amount of precipitated CaCO(3) but a linear function of the ratio bioconsolidation index (BC) defined as the ratio of CaCO(3) volume to initial sand porosity. A simple model to estimate the engineering benefits of consolidation is proposed. (C) 2011 Elsevier B.V. All rights reserved.

Evidences of the evolution from solid solution to surface segregation in Ni-doped SnO(2) nanoparticles using Raman spectroscopy

Ni-doped SnO(2) nanoparticles, promising for gas-sensing applications, have been synthesized by a polymer precursor method. X-ray diffraction (XRD) and transmission electron microscopy (TEM) data analyses indicate the exclusive formation of nanosized particles with rutile-type phase (tetragonal SnO(2)) for Ni contents below 10 mol%. The mean crystallite size shows a progressive reduction with the Ni content. Room-temperature Raman spectra of Ni-doped SnO(2) nanoparticles show the presence of Raman active modes and modes activated by size effects. From the evolution of the A(1g) mode with the Ni content, a solubility limit at similar to 2 mol% was estimated. Below that content, Raman results are consistent with the occurrence of solid solution (ss) and surface segregation (seg.) of Ni ions. Above similar to 2 mol% Ni, the redshift of A(1g) mode suggests that the surface segregation of Ni ions takes place. Disorder-activated bands were determined and their integrated intensity evolution with the Ni content suggest that the solid-solution regime favors the increase of disorder; meanwhile, that disorder becomes weaker as the Ni content is increased. Copyright (C) 2010 John Wiley & Sons, Ltd.

Synthesis, characterization, and bactericidal properties of composites based on crosslinked resins containing silver

Two different commercial crosslinked resins (Amberlite GT73 and Amberlite IRC748) were employed for anchoring silver. The -SH and -N(CH2COOH)2 groups, respectively, present on these resins were used for Ag+ chelation from an aqueous solution. The Ag+ ions were reduced with three different reductants: hydrazine, hydroxylamine, and formaldehyde (under an alkaline pH). The produced composites were characterized with thermogravimetry/differential thermogravimetry and scanning electron microscopy combined with a backscattered scanning electron detector. Energy-dispersive X-ray spectroscopy coupled to scanning electron microscopy allowed the observation of submicrometer particles of silver, and chemical microanalysis of emitted X-rays revealed the presence of metal on the internal and external surfaces of the composite microspheres. The amount of incorporated silver was determined by titration. The antibacterial activity of the silver/resin composites was determined toward 10(3)-10(7) cells/mL dilutions of the auxotrophic AB1157 Escherichia coli strain; the networks containing anchored submicrometer silver particles were completely bactericidal within a few minutes because of the combined action of silver and functional groups of the resins. (c) 2007 Wiley Periodicals, Inc.

TiAlN coatings deposited by triode magnetron sputtering varying the bias voltage

TiAlN films were deposited on AISI O1 tool steel using a triode magnetron sputtering system. The bias voltage effect on the composition, thickness, crystallography, microstructure, hardness and adhesion strength was investigated. The coatings thickness and elemental composition analyses were carried out using scanning electron microscopy (SEM) together with energy dispersive X-ray (EDS). The re-sputtering effect due to the high-energy ions bombardment on the film surface influenced the coatings thickness. The films crystallography was investigated using X-ray diffraction characterization. The X-ray diffraction (XRD) data show that TiAlN coatings were crystallized in the cubic NaCl B1 structure, with orientations in the {111}, {200} {220} and {311} crystallographic planes. The surface morphology (roughness and grain size) of TiAlN coatings was investigated by atomic force microscopy (AFM). By increasing the substrate bias voltage from -40 to -150 V, hardness decreased from 32 GPa to 19 GPa. Scratch tester was used for measuring the critical loads and for measuring the adhesion. (C) 2011 Elsevier B. V. All rights reserved.

Quantification of MgO surface excess on the SnO(2) nanoparticles and relationship with nanostability and growth

In this work, we experimentally showed that the spontaneous segregation of MgO as surface excess in MgO doped SnO(2) nanoparticles plays an important role in the system`s energetics and stability. Using Xray fluorescence in specially treated samples, we quantitatively determined the fraction of MgO forming surface excess when doping SnO(2) with several different concentrations and established a relationship between this amount and the surface energy of the nanoparticles using the Gibbs approach. We concluded that the amount of Mg ions on the surface was directly related to the nanoparticles total free energy, in a sense that the dopant will always spontaneously distribute itself to minimize it if enough diffusion is provided. Because we were dealing with nanosized particles, the effect of MgO on the surface was particularly important and has a direct effect on the equilibrium particle size (nanoparticle stability), such that the lower the surface energy is, the smaller the particle sizes are, evidencing and quantifying the thermodynamic basis of using additives to control SnO(2) nanoparticles stability. (C) 2010 Elsevier B.V. All rights reserved.

Structural and magnetic properties of pure and nickel doped SnO(2) nanoparticles

Ni-doped SnO(2) nanoparticles prepared by a polymer precursor method have been characterized structurally and magnetically. Ni doping (up to 10 mol%) does not significantly affect the crystalline structure of SnO(2), but stabilizes smaller particles as the Ni content is increased. A notable solid solution regime up to similar to 3 mol% of Ni, and a Ni surface enrichment for the higher Ni contents are found. The room temperature ferromagnetism with saturation magnetization (MS) similar to 1.2 x 10(-3) emu g(-1) and coercive field (H(C)) similar to 40 Oe is determined for the undoped sample, which is associated with the exchange coupling of the spins of electrons trapped in oxygen vacancies, mainly located on the surface of the particles. This ferromagnetism is enhanced as the Ni content increases up to similar to 3 mol%, where the Ni ions are distributed in a solid solution. Above this Ni content, the ferromagnetism rapidly decays and a paramagnetic behavior is observed. This finding is assigned to the increasing segregation of Ni ions (likely formed by interstitials Ni ions and nearby substitutional sites) on the particle surface, which modifies the magnetic behavior by reducing the available oxygen vacancies and/or the free electrons and favoring paramagnetic behavior.

Microstructural Effects of Sn Addition to Fe(2)O(3) Thin Films

The influence of Sri in Fe(2)O(3) thin films is addressed. The presence of the tin ions decreases the Fe(2)O(3) particle sizes and surface roughness decreasing of the films` surface is observed as a consequence. X-ray diffraction and atomic force microscopy measurements together with literature results support this phenomenon to be related to the segregation of the additive onto the surface and consequently surface energy decrease, which constitutes the driving force for the microstructure modification, similarly to results previously obtained for powders with same compositions. The effect of the anions introduced in the system as counter-ions of the precursors is also discussed.

Chemical characterization and anticorrosion properties of corrosion products formed on pure copper in synthetic rainwater of Rio de Janeiro and Sao Paulo

This work aims to characterize corrosion products formed on copper samples exposed to synthetic rainwater of Rio Janeiro and Sao Paulo. XRD and XPS were employed to determine their composition, while electrochemical techniques were used to evaluate their protective properties. XRD and XPS indicated the thickening of the corrosion layer with time. Electrochemical results showed that the protectiveness of the corrosion layer depends on the solution composition. Based on our findings a corrosion mechanism for copper in simulated rainwater is proposed where the role of NH(4)(+) ions in the cuprite layer partial regeneration is taken into account. (C) 2009 Elsevier Ltd. All rights reserved.