65 resultados para CHEMICAL ROUTE
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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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.
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A polymeric precursor method was used to synthesis PbTiO3 amorphous thin film processed at low temperature. The luminescence spectra of PbTiO3 amorphous thin films at room temperature revealed an intense single-emission band in the visible region, the visible emission band was found to be dependent on the thermal treatment history, Photoluminescence properties Versus different annealing temperatures were investigated. The experimental results (XRD, AFM, FL) indicate that the nature of photoluminescence (PL) must be related to the disordered structure of PbTiO3 amorphous thin films, Copyright (C) 2000 John Wiley & Sons, Ltd.
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Polycrystalline BaWO4 and PbWO4 thin films having a tetragonal scheelite structure were prepared at different temperatures. Soluble precursors such as barium carbonate, lead acetate trihydrate and tungstic acid, as starting materials, were mixed in aqueous solution. The thin films were deposited on silicon, platinum-coated silicon and quartz substrates by means of the spinning technique. The surface morphology and crystal structure of the thin films were investigated using scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray diffraction, and specular reflectance infrared Fourier transform spectroscopy, respectively. Nucleation stages and surface morphology evolution of thin films on silicon substrates have been studied by atomic force microscopy. XRD characterization of these films showed that BaWO4 and PbWO4 phase crystallize at 500 degreesC from an inorganic amorphous phase. FTIR spectra revealed the complete decomposition of the organic ligands at 500 degreesC and the appearance of two sharp and intense bands between 1000 and 600 cm(-1) assigned to vibrations of the antisymmetric stretches resulting from the high crystallinity of both thin films. The optical properties were also studied. It was found that BaWO4 and PbWO4 thin films have Eg = 5.78 eV and 4.20 eV, respectively, of a direct transition nature. The excellent microstructural quality and chemical homogeneity results confirmed that soft solution processing provides an inexpensive and environmentally friendly route for the preparation of BaWO4 and PbWO4 thin films. (C) 2003 Elsevier Ltd. All rights reserved.
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Lead zirconate titanate, Pb(Zr0.3Ti0.7)O-3 (PZT) thin films were prepared with success by the polymeric precursor method. Differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FT-IR), Micro-Raman spectroscopy and X-ray diffraction (XRD) were used to investigate the formation of the PZT perovskite phase. X-ray diffraction revealed that the film showed good crystallinity and no presence of secondary phases was identified. This indicates that the PZT thin films were crystallized in a single phase. PZT thin films showed a well-developed dense grain structure with uniform distribution, without the presence of rosette structure. The Raman spectra undoubtedly revealed these thin films in the tetragonal phase. For the thin films annealed at the 500-700 degreesC range, the vibration modes of the oxygen sublattice of the PZT perovskite phase were confirmed by FT-IR. The room temperature dielectric constant and dielectric loss of the PZT films, measured at 1 kHz were 646 and 0.090, respectively, for thin film with 365 nm thickness annealed at 700 degreesC for 2 h. A typical P-E hysteresis loop was observed and the measured values of P-s, P-r and E-c were 68 muC/cm(2), 44 muC/cm(2) and 123 kV/cm, respectively. The leakage current density was about 4.8 x 10(-7) A/cm(2) at 1.5 V. (C) 2003 Elsevier Ltd. All rights reserved.
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Polycrystalline SrTiO3 thin films having a cubic perovskite structure were prepared at different temperatures by the polymeric precursor method on platinum-coated silicon substrate. Crystalline films with uniform composition and thickness were prepared by spin-coating and the post-deposition heat treatment was carried out at different temperatures. The film showed good structural, dielectric, and insulating properties, Scanning electron microscopy (SEM) micrographs showed no occurrence of interdiffusion between the bottom electrode (platinum) and the film during post-annealing, indicating a stable interface between the SrTiO3 and the bottom electrode. The dielectric constant and dissipation factor at a frequency of 100 kHz were 250 and 0.01, respectively, for a 360 nm thick film annealed at 600 degreesC. The capacitance versus applied voltage characteristics showed that the capacitance was almost independent of the applied voltage. The I-V characteristics were ohmic in low fields and a Schottky emission and/or Poole-Frenkel emission were postulated in high fields. Room temperature leakage current density was found to be in the order of 10(-7) A/cm(2) for a 360 nm thick film in an applied electric field of about 100 kV/cm. The charge storage density of 36 fC/mum(2) was obtained in an applied electric field of about 100 kV/cm. (C) 2001 Published by Elsevier B.V. Ltd. 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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Detailed room temperature micro-Raman scattering, X-ray diffraction, atomic force microscopy and specular reflectance infrared Fourier transform spectroscopy studies were carried out on soft chemical by processed Pb1-xBaxTiO3 thin films. The micro-Raman spectra pointed the existence of a stable tetragonal ferroelectric phase in the entire composition range (0 < x <= 1). The infrared reflectance spectra showed that the frequency of several peaks decreases as the Ba2+ concentration increases. These features are correlated to a decrease in the tetragonal distortion of the TiO6 octahedra as the Ba2+ concentration increases. Furthermore, as x increases from 0.70 to 1.0, the Raman spectrum shows an evolution towards the well-known Raman spectrum of the tetragonal BaTiO3. Therefore, we demonstrated that the combination of solid solution PbTiO3-BaTiO3 with a grain size in the order of 30-40 nm supports the tetragonal ferroelectric phase at room temperature. (C) 2007 Elsevier B.V. All rights reserved.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Bi0.92La0.08FeO3 (BLFO) thin films were grown on platine substrates by the soft chemical route. Ferroelectric and dielectric behaviors of BLFO films deposited by spin-coating technique and annealed at 773 K for 2 h in air atmosphere were explained. BLFO thin films obtained presents a rhombohedral structure. The BLFO films present dielectric and ferroelectric behaviors with dielectric permittivity and dielectric loss of approximately 81 and 0.0144 at 1 kHz. The Au/BLFO/Pt capacitor shows a hysteresis loop with remnant polarization of 20.6 mu C/cm(2) and coercive field of 53.88 kV/cm. The polarization switching and the fatigue behavior of the BLFO films were significantly enhanced.
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Glass ionomer cements (GICs) are glass and polymer composite materials. These materials currently find use in the dental field. The purpose of this work is to obtain systems based on composition 4.5SiO(2)-3Al(2)O(3)-XNb2O5-2CaO to be used in Dentistry. The systems were prepared by chemical route at 700 degrees C. The results obtained by XRD and DTA showed that all systems prepared are glasses. The structures of the obtained glasses were compared to commercial material using Al-27 and Si-29 MAS NMR. The analysis of MAS NMR spectra indicated that the systems developed and commercial material are formed by SiO4 and AlO4 linked tetrahedra. The properties of glass ionomer cements based on the glasses prepared with several niobium contents were studied. Setting and working times of the cement pastes, microhardness and diametral tensile strength were evaluated for the experimental GICs and commercial luting cements. It was concluded that setting time of the cement pastes increased with increasing niobium content of the glasses (X). The properties to the GICs such as setting time and microhardness were influenced by niobium content. (c) 2005 Elsevier B.V. All rights reserved.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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The use of chemical methods in the synthesis of high-quality and small-size polycrystalline samples has been increased in recent years. In this work, a chemical route based on an aqueous precursor solution of metals followed by the addition of a water-soluble polymer formed by ethylenediaminetetraacetic acid (EDTA) and ethylene glycol (EG) was tested to produce superconducting mesoscopic YBa(2)Cu(3)O(7-gamma) samples. Different conditions of heat treatments and the effects of argon and oxygen atmospheres during the calcination steps were traced using X-ray diffraction (XRD), scanning electron microscopy (SEM) and magnetic measurements. (C) 2008 Elsevier B. V. All rights reserved.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)