949 resultados para thin-layer chromatography (TLC)
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In order to improve the chemical resistance of zirconium fluoride glass a protective transparent SnO2 layer was deposited by the solgel dip-coating process in the presence of Tiron (R) as particle surface modifier agent. After water immersion for different periods of time, both coated and non-coated fluoride glasses were analyzed by scanning electron microscopy, mass loss evaluation, infrared spectroscopy and X-ray photoelectron spectroscopy. In contrast to the effects occurring for non-coated glass, where the surface undergoes a rapid selective dissolution of the most soluble species, the results for the SnO2-coated glass showed that the filling of the film nanopores by dissolved glass material results in a hermetic barrier protecting the glass surface. The selective glass dissolution was confirmed by liquid chromatography measurements of the etching solution after each exposure time. (c) 2006 Elsevier B.V. All rights reserved.
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In this work we investigate the effect from the solution concentration on aggregation in layer-by-layer (LBL) films of poly(omethoxyaniline) (POMA) alternated with poly(vinyl sulfonic acid). Films are adsorbed on hydrophilized glass substrates and characterized with UV-Vis spectroscopy and atomic force microscopy. The formation of aggregates is favored in more concentrated solutions, leading to an increase in the diameter of the domains. This is caused by stronger polymer-polymer interactions under high concentrations. The size of POMA aggregates in solution is estimated to be larger than in LBL films, which is surprising because one should expect aggregates from solution to coalesce into larger aggregates in the deposited films. This unexpected result may be explained by a swelling effect of aggregates in the aqueous POMA solutions, consistent with other reports in the literature which consider the aggregates in solution to be made up of smaller aggregates. Upon adsorption on a solid substrate to form the LBL film, a molecular reorganization probably takes place, resulting in smaller aggregates. It is also found that the size distribution of the POMA domains in the LBL films is determined by the concentration of the solution. (C) 2002 Elsevier B.V. B.V. All rights reserved.
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The interactions governing adsorption of layer-by-layer (LBL) films from an azopolymer, PS-119(R), and poly(allylamine hydrochloride) (PAH) have been controlled by modifying the pH of the solutions used to form the films. The thickness per bilayer was varied by one order of magnitude, from 10 to 240 A, as the pH changed from 4 to 10. Thick layers were formed at higher pHs because in this case the PAH is only partially charged adopting a loopy conformation. This change in molecular conformation caused the kinetics of isomerization and mass transport to be much slower than at lower pHs. The writing time defined as the time to achieve 50% of maximum birefringence dropped from 110 to 18 min for films prepared from solutions with pH 10 and pH 4, respectively. This decrease is probably due to the higher free volume for isomerization in the films prepared at lower pHs, in which PAH molecules are less coiled than at higher pHs. For the same reason, the rate of inscription of surface-relief gratings with an interference pattern of p-polarized light was also much slower at higher pHs. (C) 2003 Elsevier B.V. All rights reserved.
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Multilayer thin films with perovskite structures were produced by the polymeric precursor method. SrTiO3/BaTiO3 (STO/BTO) multilayers were deposited on Pt(111)/Ti/SiO2/Si(100) substrates by the spin-coating technique and heated in air at 700 degreesC. The microstructure and crystalline phase of the multilayered thin films were examined by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), resolution-high transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and X-ray diffraction. The SrTiO3/BaTiO3 multilayer thin films consisted of grainy structures with an approximate grain size of 60 nm. The multilayered thin films showed a very clear interface between the components. The SrTiO3/BaTiO3 multilayer thin films revealed dielectric constants of approximately 527 and loss tangents of 0.03 at 100 kHz. The dielectric constant calculated for this multilayer film system is the value of the sum of each individual component of the film, i.e. The total value of the sum of each SrTiO3 (STO) and BaTiO3 (BTO) layer. The multilayer SrTiO3/BaTiO3 obtained by the polymeric precursor method, also showed a ferroelectric behavior with a remanent polarization of 2.5 muC/cm(2) and a coercive field of 30 kV/cm. The multilayer films displayed good fatigue characteristics under bipolar stressing after application of 10(10) switching cycles. (C) 2001 Published by Elsevier B.V. B.V. All rights reserved.
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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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We present photoluminescence and decay of photo excited conductivity data for sol-gel SnO(2) thin films doped with rare earth ions Eu(3+) and Er(3+), a material with nanoscopic crystallites. Photoluminescence spectra are obtained under excitation with several monochromatic light sources, such as Kr(+) and Ar(+) lasers, Xe lamp plus a selective monochromator with UV grating, and the fourth harmonic of a Nd: YAG laser (4.65eV), which assures band-to-band transition and energy transfer to the ion located at matrix sites, substitutional to Sn(4+). The luminescence structure is rather different depending on the location of the rare-earth doping, at lattice symmetric sites or segregated at grain boundary layer, where it is placed in asymmetric sites. The decay of photo-excited conductivity also shows different trapping rate depending on the rare-earth concentration. For Er-doped films, above the saturation limit, the evaluated capture energy is higher than for films with concentration below the limit, in good agreement with the different behaviour obtained from luminescence data. For Eu-doped films, the difference between capture energy and grain boundary barrier is not so evident, even though the luminescence spectra are rather distinct.
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Starting from aqueous colloidal suspensions, undoped and Nb5+ doped SnO2 thin films have been prepared by using the dip-coating sol gel process. X-ray diffraction results show that films are polycrystalline with crystallites of average size1-4nm. Decreasing the thickness of the films and increasing the Nb5+ concentration limits the crystallite size growth during firing. Complex impedance measurements reveal capacitive and resistive effects between adjacent crystallites or grains, characteristic of electrical potential barriers. The transfer of charge throughout these barriers determines the macroscopic electrical resistance of the layer. The analysis of the optical absorption spectra shows that the samples present more than 80% of their transmittance in the visible region and the value of the band gap energy increases with decreasing crystallite size. © 1997 Chapman & Hall.
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Polycrystalline SrBi2Nb2O9-layered ferroelectric thin films were synthesized on Pt/Ti/SiO2/Si substrate using the polymeric precursors solution. The dip-coated films were specular and crack-free and crystallized during firing at 700 °C. Single-, double-, and triple-layered films were obtained by several dips in the deposition solution, and the influence of crystallization between each dip was studied. Microstructure and morphological evaluation were followed by grazing incident x-ray diffraction (GIXRD), scanning electron microscopy (SEM), and atomic force microscopy (AFM). Multilayered films obtained using the intermediate-crystallized layer route present a dense microstructure with spherical grains, with a preferential orientation in the 〈215〉 direction; films obtained using the intermediate-amorphous layer route are polycrystalline and present elongated grains around 250 nm in size.
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We report on the properties of BaBi2Ta2O9 (BBT) thin films for dynamic random-access memory (DRAM) and integrated capacitor applications. Crystalline BBT thin films were successfully fabricated by the chemical solution deposition technique on Pt-coated Si substrates at a low annealing temperature of 650°C. The films were characterized in terms of structural, dielectric, and insulating properties. The electrical measurements were conducted on Pt/BBT/Pt capacitors. The typical measured small signal dielectric constant and dissipation factor, at 100 kHz, were 282 and 0.023, respectively, for films annealed at 700°C for 60 min. The leakage current density of the films was lower than 10-9 A/cm2 at an applied electric field of 300 kV/cm. A large storage density of 38.4 fC/μm2 was obtained at an applied electric field of 200 kV/cm. The high dielectric constant, low dielectric loss and low leakage current density suggest the suitability of BBT thin films as dielectric layer for DRAM and integrated capacitor applications.
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The methacrylic copolymer functionalized with the azo chromophore 4-[N-ethyl-N-(2-hydroxiethyl)]-amino-2′-chloro-4-nitroazobenzene (MMADR13), in its polyelectrolyte form, can be used to fabricate thin films by the layer-by-layer (LbL) technique just if one alternates this anionic polyelectrolyte with a cationic polyelectrolyte such as poly(allylamine hydrochloride) (PAH). Since PAH does not present any particular optical functionality, the main final film feature will came from the side chain DR13 azo-chromophore group due to its large nonlinear optical properties and photoisomerization capabilities. This work reports the electrooptic activity of MMADR13/DR13 LBL films, which arises from the high hiperpolarizability about the azo side chain group.
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The protection efficiency against water corrosion of fluorozirconate glass, ZBLAN, dip-coated by nanocrystalline tin oxide film containing the organic molecule Tiron® was investigated by X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). The chemical bonding structure of the surface region and morphology were studied before and after two water exposure periods of 5 and 30 min. The results of the analysis for the as-grown sample revealed a SnO1.6 phase containing carbon and sulfur, related to Tiron®, and traces of elements related to ZBLAN (Zr, F, Ba). This fact and the clear evidence of the presence of tin oxifluoride specie (SnOxF y) indicates a diffusion of the glass components into the porous coating. After water exposure, the increase of the oxygen concentration accompanied by a strong increase of Zr, F, Ba and Na content is interpreted as filling of the nanopores of the film by glass compounds. The formation of a compact protective layer is supported by the morphological changes observed by AFM. © 2005 Elsevier B.V. All rights reserved.
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Influence of cutting instruments and The aim of this study was to analyze the hybrid layer in noncarious dentin prepared by different cutting instruments and restored with composite resin. The cavities were randomly prepared in 40 specimens using a high-speed diamond bur (KG Sorensen 1013) and an ultrasonic tip (CVDentus C22). The cavities were restored with composite resin by varying the adhesive system between the Adper™ Single Bond (2 x 1 system, primer+adhesive) and the Prompt L-Pop™ (3 x 1 system, self-etching). The restorations were hemisected longitudinally and analyzed in the SEM (Scanning electron microscopy) in order to evaluate the hybrid layer and resinous tags characteristics, using scores ranging from 1 to 6. The Pearson test revealed a high correlation coefficient and good significance levels for both intra- and inter-raters values (r=0.90). The data were statistically analyzed using the Mann-Whitney test (P≤0.05). A larger proportion of regular hybrid layers with numerous tags were observed in the dentin prepared using the high-speed diamond burs and restored with a 2 × 1 adhesive system. Alternatively, the 3 × 1 adhesive system promoted the generation of a thin hybrid layer with few tags. After preparation using an ultrasonic tip revealed few or no tags after the preparation and 2 × 1 or 3 × 1 adhesive system application. The high-speed diamond burs produced a dentin surface that was more favorable to restorative material adhesion than the ultrasonic tips, regardless of the adhesive system used.
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Eumelanin pigments show hydration-dependent conductivity, broad-band UV-vis absorption, and chelation of metal ions. Solution-processing of synthetic eumelanins opens new possibilities for the characterization of eumelanin in thin film form and its integration into bioelectronic devices. We investigate the effect of different synthesis routes and processing solvents on the growth, the morphology, and the chemical composition of eumelanin thin films using atomic force microscopy and X-ray photoelectron spectroscopy. We further characterize the films by transient electrical current measurements obtained at 50% to 90% relative humidity, relevant for bioelectronic applications. We show that the use of dimethyl sulfoxide is preferable over ammonia solution as processing solvent, yielding homogeneous films with surface roughnesses below 0.5 nm and a chemical composition in agreement with the eumelanin molecular structure. These eumelanin films grow in a quasi layer-by-layer mode, each layer being composed of nanoaggregates, 1-2 nm high, 10-30 nm large. The transient electrical measurements using a planar two-electrode device suggest that there are two contributions to the current, electronic and ionic, the latter being increasingly dominant at higher hydration, and point to the importance of time-dependent electrical characterization of eumelanin films. This journal is © 2013 The Royal Society of Chemistry.
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Alumina thin films have been obtained by resistive evaporation of Al layer, followed by thermal oxidation by means of annealing in appropriate atmosphere (air or O2-rich), with variation of annealing time and temperature. Optical and structural properties of the investigated films reveal that the temperature of 550 °C is responsible for reasonable oxidation, which is accelerated up to 8 times for O2-rich atmosphere. Results of surface electrical resistivity and Raman spectroscopy are in good agreement with these findings. Surprisingly, X-ray and Raman data suggest also the crystallization of Si nuclei at glass substrate-alumina interface, which would come from the soda-lime glass used as substrate. © 2013 Elsevier Ltd and Techna Group S.r.l.