Plasma-deposition of Ag-containing polyethyleneoxide-like coatings

Ag-containing polyethyleneoxide (FEO)-like thin films have been deposited in Radio Frequency Glow Discharges fed with vapors of diethyleneglycol-dimethyl-ether and argon. Proper experimental conditions have been utilized in order to fragment the monomer in the glow and, at the same time, sputter Ag from the silver RF cathode of the reactor, in a way that polyethyleneoxide(PEO)-like coatings with embedded Ag clusters have been deposited at the ground electrode. The composition of the coatings has been investigated by means of different techniques; the plasma process has been investigated by means of Actinometric Optical Emission Spectroscopy. A correlation has been found between the amount of silver embedded in the coatings and that sputtered in the discharge, monitored by actinometry, that could eventually be utilized to control in situ the deposition process.

Minimization of lead and copper interferences on spectrophotometric determination of cadmium using electrolytic deposition and ion-exchange in multi-commutation flow system

A new strategy for minimization of Cu2+ and Pb2+ interferences on the spectrophotometric determination of Cd2+ by the Malachite green (MG)-iodide reaction using electrolytic deposition of interfering species and solid phase extraction of Cd2+ in flow system is proposed. The electrolytic cell comprises two coiled Pt electrodes concentrically assembled. When the sample solution is electrolyzed in a mixed solution containing 5% (v/v) HNO3, 0.1% (v/v) H2SO4 and 0.5 M NaCl, Cu2+ is deposited as Cu on the cathode, Pb2+ is deposited as PbO2 on the anode while Cd2+ is kept in solution. After electrolysis, the remaining solution passes through an AG1-X8 resin (chloride form) packed minicolumn in which Cd2+ is extracted as CdCl4/2-. Electrolyte compositions, flow rates, timing, applied current, and electrolysis time was investigated. With 60 s electrolysis time, 0.25 A applied current, Pb2+ and Cu2+ levels up to 50 and 250 mg 1-1, respectively, can be tolerated without interference. For 90 s resin loading time, a linear relationship between absorbance and analyte concentration in the 5.00-50.0 μg Cd 1-1 range (r2 = 0.9996) is obtained. A throughput of 20 samples per h is achieved, corresponding to about 0.7 mg MG and 500 mg KI and 5 ml sample consumed per determination. The detection limit is 0.23 μg Cd 1-1. The accuracy was checked for cadmium determination in standard reference materials, vegetables and tap water. Results were in agreement with certified values of standard reference materials and with those obtained by graphite furnace atomic absorption spectrometry at 95% confidence level. The R.S.D. for plant digests and water containing 13.0 μg Cd 1-1 was 3.85% (n = 12). The recoveries of analyte spikes added to the water and vegetable samples ranged from 94 to 104%. (C) 2000 Elsevier Science B.V.

The improvement of thin polymer film properties through plasma immersion ion implantation and deposition technique

Thin polymer films were deposited from acetylene and argon mixtures by plasma immersion ion implantation and deposition. The effect of the pulse frequency, v, on molecular structure, optical gap, contact angle and hardness of the films was investigated. It was observed progressive dehydrogenation of the samples and increment in the concentration of unsaturated carbon bonds as the pulse frequency was increased. Film hardness and contact angle increased and optical gap decreased with v. These results are interpreted in terms of the chain unsaturation and crosslinking.

Calcium salts deposition in rat connective tissue after the implantation of calcium hydroxide-containing sealers

This study was conducted to observe the rat subcutaneous connective tissue reaction to implanted dentin tubes that were filled with mineral trioxide aggregate, Sealapex, Calciobiotic Root Canal Sealer (CRCS), Sealer 26, and the experimental material, Sealer Plus. The animals were sacrificed after 7 and 30 days, and the specimens were prepared for histological analysis after serial sections with a hard-tissue microtome. The undecalcified sections were examined with polarized light after staining according to the Von Kossa technique for calcium. At the tube openings, there were Von Kossa-positive granules that were birefringent to polarized light. Next to these granulations, there was irregular tissue, like a bridge, that was Von Kossa-positive. The dentin walls of the tubes exhibited a structure highly birefringent to polarized light, usually like a layer, in the tubules. These results were observed with all the studied materials, except the CRCS, which didn't exhibit any kind of mineralized structure. The results suggest that among the materials studied, the CRCS could have the least possibility of encouraging hard tissue deposition.

Dental implants: Surface modification of cp-Ti using plasma spraying and the deposition of hydroxyapatite

The commercial pure titanium (cp-Ti) is currently being used with great success in dental implants. In this work we investigate how the cp-Ti implants can be improved by modifying the metal surface morphology, on which a synthetic material with properties similar to that of the inorganic part of the bone, is deposited to facilitate the bone/implant bonding. This synthetic material is the hydroxyapatite, HA, a calcium-phosphate ceramic. The surface modification consists in the application of a titanium oxide (TiO2) layer, using the thermal aspersion - plasma spray technique, with posterior deposition of HA, using the biomimetic method. The X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) with Energy Dispersive X-ray (EDX) and Diffuse Reflectance Infrared Fourier Transform (DRIFT) techniques have been used for characterizing phases, microstructures and morphologies of the coatings. The TiO2 deposit shows a mixture of anatase, rutilo and TiO2-x phases, and a porous and laminar morphology, which facilitate the HA deposition. After the thermal treatment, the previously amorphous structured HA coating, shows a porous homogeneous morphology with particle size of about 2-2.5 μm, with crystallinity and composition similar to that of the biological HA.

Morphology changes induced by laser irradiation on disperse red 13 films prepared by physical vapor deposition

Surface morphology changes induced by argon laser irradiation (514 nm) on disperse red 13 (DR13) films prepared by physical vapor deposition (PVD) were investigated. Atomic force microscopy was used to characterize the irradiated sample for different periods of irradiation. Needle-shape structures are observed which are attributed to the symmetry of DR13 molecules. The film becomes increasingly closely packed with the irradiation, with lower root mean square roughness for long exposure times. This is due to photoisomerization of DR13 molecules and probably heating of the sample, which can provide the required mobility for the molecular rearrangement. The rearrangement is such that voids in the film are filled in upon irradiating the sample, thus decreasing the film roughness and increasing the packing.

Temperature and stoichiometry effect on microstructural and ferroelectric properties of Pb(Zr1-xTix)O3 thin films prepared by chemical soulution deposition

Lead zirconate titanate (PZT) solutions were prepared using a polymeric precursor method, Zr n-propoxide and Ti i-propoxide were used as starting materials with ethylene glycol and water as solvents. The PZT solution was spin-coated on Pt/Ti/SiO2/Si substrates, baked on a hot plate, and finally heat-treated in a tube furnace between 400 and 800°C. The surface morphology and grain size of the films were characterized by atomic force microscopy (AFM), using a tapping mode with amplitude modulation. The films, thermal annealed at temperatures higher than 500°C, exhibited a dense microstructure, without noticeable cracks or voids. Electrical properties were investigated as a function of composition and annealing temperature.

Deposition and leaching of tebuthiuron on sugar cane straw applied with and without alkyl polyglycoside adjuvant

A laboratory experiment was carried out aiming to study the effects of an alkyl polyglycoside adjuvant (APG) on deposition and leaching of the herbicide tebuthiuron applied on sugar cane straw. Tebuthiuron, at concentration of 1200 mg L-1, was applied separately and in tank mix with the APG adjuvant, at concentrations of 0.07 and 0.09% (wt v-1), using a spraying volume of 204 L ha-1. A precipitation equivalent to 20 mm of rain was simulated, 24 h after the applications, to evaluate the herbicide leaching. The quantification of tebuthiuron was carried out by the high performance liquid chromatography (HPLC). It was observed that the addition of APG adjuvant at 0.07% (wt v-1) provided an increase of 11.5% in the deposition of tebuthiuron on straw, reduction of 50.4% in the drift of the herbicide and it did not affect significantly the leached amount (68.5%), when compared with the treatment where tebuthiuron was applied alone (70.8%). At the concentration of 0.09% (wt v-1), the APG adjuvant caused an increase of 22.7% in the deposition; it reduced the drift of the herbicide by 99.9% and reduced the leached amount by 7.6% thereby increasing the retention of the herbicide by straw.

An ellipsometric study of manganese oxide films: In situ characterization of the deposition and electroreduction of MnO2

The electrodeposition of manganese oxide films onto a platinum substrate was investigated by means of in situ ellipsometry. In the thickness range from 0 to 150 nm, the anodic oxide behaves as an Isotropic single layer with optical constants that are independent of thickness. Deviations at higher thickness are explained in terms of anisotropic properties of the film. The electroreduction of thin films (up to ca. 150 nm) in an alkaline electrolyte leads to a decrease in both the refractive index and the extinction coefficient and is accompanied by a thickness increase of ca. 10%. The Mn(IV) to Mn(III) conversion takes place from the oxide/electrolyte interface inwards. © 2004 The Electrochemical Society. All rights reserved.

Hydrothermal synthesis and crystal structure of a copper(ii) coordination polymer with bridging dicarboxylate and diamine ligands

This work reports on the synthesis of a copper(II) coordination compound with 4,4-oxibis(benzoate) (obb) and trans-1,2- bis(4-pyridyl)ethene (bpe) ligands. The complex was characterized by single-crystal X-ray diffraction, which showed a 3D polymeric structure. Each copper center is surrounded by four oxygen atoms at the basal plane and one nitrogen atom and one copper atom at the axial positions, revealing a distorted octahedral geometry. Four carboxylic groups bridge two copper atoms, forming a cage-like structure, with the distance between the metallic centers being 2.656(1)Å. 2008 © The Japan Society for Analytical Chemistry.

Structural refinement and photoluminescence properties of cube-like (Ca 1-xCu x)TiO 3 crystals synthesized by the microwave-hydrothermal method

In this work, (Ca 1-xCu x)TiO 3 crystals with (x = 0, 0.01 and 0.02), labeled as CTO, CCTO1 and CCTO2, were synthesized by the microwave-hydrothermal method at 140°C for 32 min. XRD patterns (Fig. 1), Rietveld refinement and FT-Raman spectroscopy indicated that these crystals present orthorhombic structure Pbnm. Micro-Raman and XANES spectra suggested that the substitution of Ca by Cu in A-site promoted a displacement of the [TiO6]-[TiO6] clusters adjacent from its symmetric center, which leads distortions on the [CaO 12] clusters neighboring and consequently cause the strains into the CaTiO3 lattice. FE-SEM images showed that these crystals have an irregular shape as cube like probably indicating an Ostwald-ripening and self-assemble as dominant mechanisms to crystals growth. The powders presented an intense PL blue-emission.

CdMoO 4 synthesized by a microwave-assisted hydrothermal method and their photoluminescence and photocatality properties

In this work CdMoO 4 nanoparticles were obtained under hydrothermal conditions using microwave radiation (2.45 GHz) (MH) at 100°C for different times. These powders were analyzed by X-ray diffraction (XRD), Field-emisson gum scanning electron microscopy (FEG-SEM), Ultraviolet-visible (UV-vis) absorption spectroscopy and photoluminescence (PL) measurements. XRD pattern confirmed that the pure CdMoO 4 phases were obtained. FEG-SEM powders present large-scale and homogeneous particles with microspheres-like morphology. UV-vis results were employed to determine the optical band gap these materials. Also, it showed existence of photoluminescence (PL) emission in the green wavelength range of 540-546 nm. Photocatalytic activity of CdMoO 4 nanocrystals was examined by monitoring the degradation of rhodamine B dye.

Microwave-assisted hydrothermal synthesis of ZnO powders with different reagents

In this work, zinc oxide powders were synthesized by microwave-assisted hydrothermal method in basic medium. These powders were analyzed by X-ray diffraction (XRD), Field-emisson gum scanning electron microscopy (FEG-SEM), Ultraviolet-visible (UV-vis) absorption spectroscopy and photoluminescence (PL) measurements. XRD pattern confirmed that the pure ZnO phases were obtained after MH processing performed at 130°C/ 1h. FEG-SEM micrographs reveals that these nanostructures are made up of ZnO plates. UV-vis results were employed to determine the optical band gap these materials. Also, it showed existence of photoluminescence (PL) in the different zinc powders. An orange PL emission when excited by 350 nm wavelength at room temperature was observad in the different powders.

Electronic structure and magnetic properties of FeWO 4 nanocrystals synthesized by the microwave-hydrothermal method

This communication reports that FeWO 4 nanocrystals were successfully synthesized by the microwave-hydrothermal method at 443 K for 1 h. The structure and shape of these nanocrystals were characterized by X-ray diffraction, Rietveld refinement, and transmission electron microscopy. The experimental results and first principles calculations were combined to explain the electronic structure and magnetic properties. Experimental data were obtained by magnetization measurements for different applied magnetic fields. Theoretical calculations revealed that magnetic properties of FeWO 4 nanocrystals can be assigned to two magnetic orderings with parallel or antiparallel spins in adjacent chains. These factors are crucial to understanding of competition between ferro- and antiferromagnetic behavior. © 2012 Elsevier Inc.

Comparative in vivo study of commercially pure Ti implants with surfaces modified by laser with and without silicate deposition: Biomechanical and scanning electron microscopy analysis

The purpose of this study was to evaluate commercially pure titanium implant surfaces modified by laser beam (LS) and LS associated with sodium silicate (SS) deposition, and compare them with machined surface (MS) and dual acid-etching surfaces (AS) modified. Topographic characterization was performed by scanning electron microscopy-X-ray energy dispersive spectroscopy (SEM-EDX), and by mean roughness measurement before surgery. Thirty rabbits received 60 implants in their right and left tibias. One implant of each surface in each tibia. The implants were removed by reverse torque for vivo biomechanical analysis at 30, 60, and 90 days postoperative. In addition, the surface of the implants removed at 30 days postoperative was analyzed by SEM-EDX. The topographic characterization showed differences between the analyzed surfaces, and the mean roughness values of LS and SS were statistically higher than AS and MS. At 30 days, values removal torque LS and SS groups showed a statistically significant difference (p < 0.05) when compared with MS and AS. At 60 days, groups LS and SS showed statistically significant difference (p < 0.05) when compared with MS. At 90 days, only group SS presented statistically higher (p < 0.05) in comparison with MS. The authors can conclude that physical chemistry properties and topographical of LS and SS implants increases bone-implant interaction and provides higher degree of osseointegration when compared with MS and AS. © 2012 Wiley Periodicals, Inc.