Low temperature synthesis and electrical properties of PbTiO3 thin films prepared by the polymeric precursor method

Ferroelectric PbTiO3 thin films were successfully prepared on a Pt(111)Ti/SiO2/Si(100) substrate for the first time by spin coating, using the polymeric precursor method. X-ray diffraction patterns of the films indicate that they are polycrystalline in nature. This method allows low temperature (500 degrees C) synthesis and high electrical properties. The multilayer PbTiO3 thin films were granular in structure with a grain size of approximately 110-120 nm. A 380-nm-thick film was obtained by carrying out four cycles of the spin-coating/heating process. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) analyses showed the surface of these thin films to be smooth, dense and crack-free with low surface roughness (=3.4 nm). At room temperature and at a frequency of 100 kHz, the dielectric constant and the dissipation factor were, respectively, 570 and 0.016. The C-V characteristics of perovskite thin film prepared at low temperature show normal ferrolectric behavior. The remanent polarization and coercive field for the films deposited were 13.62 mu C/cm(2) and 121.43 kV/cm, respectively. The high electrical property values are attributed to the excellent microstrutural quality and chemical homogeneity of thin films obtained by the polymeric precursor method. (C) 2000 Elsevier B.V. S.A. All rights reserved.

Preparation, microstructural and electrical characterization of SrTiO3 thin films prepared by chemical route

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.

PREPARATION AND CHARACTERIZATION OF TI(IV) OXIDE GRAFTED ONTO SILICA ON A SILICA-GEL SURFACE

Silica gel with a surface area of 500 m2g-1 and an average pore diameter of 60 angstrom was chemically modified with Ti(IV) oxide using the grafting method. The amount of metal oxide attached to the surface was 1.8.10(-3) mol g-1. The X-ray photoelectron spectra showed that the metal ion species on the surface are Ti(IV) in TiO2 and MTiO3 (M = Ca2+, Sr2+, Ba2+ and Pb2+), i.e. they have the binding energy of Ti2p3/2 = 458.7 eV. The dehydration of the solid at higher temperature increased the O(II)/Ti (O(II) = oxygen bound to titanium atom) ratio, presumably due to a reticulation of the hydrous Ti(IV) oxide on the silica surface at higher temperatures. Migration of Ti(IV) into the silica gel matrix was observed but the specific surface area was not significantly changed.

Low-temperature synthesis of single-phase Co7Sb2O12

Polycrystalline Co7Sb2O12 compounds have been synthesized by a chemical route, which is based on a modified polymeric precursor method. In order to study the physical properties of the samples, X-ray diffraction (XRD), thermal analyses (TG and DSC), infrared spectroscopy (IR), specific surface area (BET), and magnetization measurements were performed on these materials. Characterization through XRD revealed that the samples are single-phase after a heat-treatment at 1100degreesC for 2h, while the X-ray patterns of the samples heat-treated at lower temperatures revealed the presence of additional Bragg reflections belonging to the Co6Sb2O6 phase. These data were analyzed by means of Rietveld refinement and further analyze showed that Co7Sb2O12 displays an inverse spinel crystalline structure. In this structure, the Co2+ ions occupy the eight tetrahedral positions, and the sixteen octahedral positions are randomly occupied by the Sb5+ and Co2+ ions. IR studies disclosed two strong absorption bands, v(1) and v(2), in the expected spectral range for a spinel-type binary oxide with space group Fd3m. Exploratory studies concerning the magnetic properties indicated that this sample presents a spin-glass transition at T-f similar to 64 K. (C) 2004 Elsevier B.V. All rights reserved.

Structural and ferroelectric properties of Pb1-xSrxTiO3 thin films

Strontium-modified lead titanate (PST) thin films with composition Pb1-xSrxTiO3 (0.10 < x &LE; 0.60) were grown on Pt/Ti/SiO2/Si substrates using a soft chemical process. The crystallization of the PST thin films was achieved by heat treatment at 600&DEG;C. The structural and microstructural modifications in the films were studied using X-ray diffraction (XRD) and atomic force microscopy, respectively. The XRD study shows that the lattice parameters of polycrystalline PST thin films calculated from X-ray data indicate a decrease in lattice tetragonality with the increase in strontium content in these films. This indicates a gradual change from tetragonal to cubic structure. By atomic force microscopy analysis, the average grain size of the thin films was systematically reduced with the increase in Sr content. The dielectric property of the thin films was found to be strongly dependent on the Sr concentration. With 60 at.% Sr content, a ferroelectric to paraelectric phase transition was observed at room temperature.

Pyrosol preparation and structural characterization of SnO2 thin films

Polycrystalline tin oxide thin films were prepared from ethanol solution of SnCl2.H2O (concentrations: 0.05, 0.1, 0.2 and 0.4 mol/dm(3)) at different substrate temperatures ranging from 300 to 450 degreesC. The kinetic deposition processes were studied in terms of various process parameters. The crystal phases, crystalline structure, grain size and surface morphology are revealed in accordance to X-ray diffractometry and scanning electron microscopy (SEM). Texture coefficients (TCs) for (110), (2 0 0), (2 11) and (3 0 1) reflections of the tetragonal SnO2 were calculated. Structural characteristics of deposited films with respect to varying precursor chemistry and substrate temperature are presented and discussed. (C) 2003 Published by Elsevier B.V.

Photoelectrocatalytic oxidation of remazol turquoise blue and toxicological assessment of its oxidation products

The ability of photoelectrocatalytic oxidation to degrade the commercially important copper-plitalocyanine dye, remazol turquoise blue 15 (RTB) was investigated. The best experimental condition was optimized, evaluating the performance of Ti/TiO2 thin-film electrodes prepared by sol-gel method in the decolourization of 32 mg L-1 RTB dye in 0.5 mol L-1 Na2SO4 pH 8 and applied potential of +1.5 V versus SCE under UV irradiation. Spectrophotometric measurements, high performance liquid chromatography, dissolved organic carbon (TOC) evaluation and stripping analysis of yielding solution obtained after 3 h of photoelectrolysis leads to 100% of absorbance removal from wavelength of 250-800 nm, 79.6% of TOC reduction and the releasing of up to 54.6% dye-bound copper (0.85 mg L-1) into the solution. Both, original and oxidized dye solution did not presented mutagenic activity with the strains TA98 and WOO of Salmonella in the presence and absence of S9 mix at the tested doses. Nevertheless, the yielding photoelectrocatalytic oxidized solution showed an increase in the acute toxicity for Vibrio fischeri bacteria, explained by copper liberation during treatment. (c) 2006 Elsevier B.V. All rights reserved.

Electron field emission from boron doped microcrystalline diamond

Field emission properties of hot filament chemical vapor deposited boron doped polycrystalline diamond have been studied. Doping level (N-B) of different samples has been varied by the B/C concentration in the gas feed during the growth process and doping saturation has been observed for high B/C ratios. Threshold field (E-th) for electron emission as function of B/C concentration has been measured, and the influences of grain boundaries, doping level and surface morphology on field emission properties have been investigated. Carrier transport through conductive grains and local emission properties of surface sites have been figured out to be two independent limiting effects in respect of field emission. Emitter current densities of 500 nA cm(-2) were obtained using electric fields less than 8 V/mu m. (c) 2007 Elsevier B.V. All rights reserved.

Preparation of 9/65/35 PLZT thin films deposited by a dip-coating process

Crack-free polycrystalline PLZT (Pb,a)(Zr,Ti)O-3 thin films with the perovskite structure were prepared by dir-coating using the Pechinis process. Lead acetate, hydrated lanthanum carbonate, zirconium n-propoxide and titanium isopropoxide were used as raw materials. The viscosity of the solution was adjusted in the range of 20 to 56 cP and the films were deposited by a dip-coating process on silicon (100) as substrate. Solutions with ionic concentration of 0.1 and 0.2 M were used. Thin film deposition was accomplished by dipping the substrates in the solution with control of withdrawal speed from 5 to 20 mm/min. The thin films were thermally treated in two steps: at 300 degreesC amid 650 degreesC. The influence of withdrawal speed. viscosity, heating rate and ionic concentration on the morphology of PLZT thin film was discussed. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

Microstructure and electrical properties of perovskite (Pb, La)TiO3 thin film deposited at low temperature by the polymeric precursor method

High-quality (Pb, La)TiO3 ferroelectric thin films were successfully prepared on a Pt(111)/Ti/SiO2/Si(100) substrate for the first time by spin coating, using the polymeric precursor method. The X-ray diffraction patterns show that the films are polycrystalline in nature. This method allows for low temperature (500 degrees C) synthesis, a high quality microstructure and superior dielectric properties. The effects on the microstructure and electrical properties were studied by changing the La content. The films annealed at 500 degreesC have a single perovskite phase with only a tetragonal or pseudocubic structure. As the La content is increased, the dielectric constant of PLT thin films increases from 570 up to 1138 at room temperature. The C-V and P-E characteristics of perovskite thin films prepared at a low temperature show normal ferroelectric behavior, representing the ferroelectric switching property. The remanent polarization and coercive field of the films deposited decreased due to the transformation from the ferroelectric to the paraelectric phase with an increased La content. (C) 2001 Kluwer Academic Publishers.

Film formation and surface growth on tin electrodes in bicarbonate solutions: an impedance spectroscopy study

The electrochemical behaviour of potentiodynamically formed thin anodic films of polycrystalline tin in aqueous sodium bicarbonate solutions (pH approximate to 8.3) were studied using cyclic voltammetry and electrochemical impedance spectroscopy. Different equivalent circuits corresponding to various potential regions were employed to account for the electrochemical processes taking place under each condition. (C) 2004 Elsevier Ltd. All rights reserved.

Stress-induced ordering due heavy interstitial atoms in Nb-0.3 wt.% Ti alloys

The mechanical properties of metals with bee structure, such as niobium and their alloys, are changed of a significant way by the introduction of heavy interstitial elements. These interstitial elements (oxygen, for example) present in the metallic matrix occupy octahedral sites and constitute an elastic dipole of tetragonal symmetry and might produce anelastic relaxation. Polycrystalline samples of Nb-0.3 wt.% Ti (Nb-Ti) alloy with oxygen in solid solution were analysed. The anelastic spectroscopy measurements had been made in a torsion pendulum, with frequencies in the Hz range, in a temperature range between 300 and 700 K. The results showed thermally activated relaxation structures were identified four relaxation process attributed to stress-induced ordering of single oxygen, nitrogen and carbon atoms around niobium and stress-induced ordering of single oxygen atoms around titanium atoms. (c) 2005 Elsevier B.V. All rights reserved.

Degradation of metallophtalocyanine dye by combined processes of electrochemistry and photoelectrochemistry

Photoelectrocatalytic degradation of metallophtalocyanine reactive dye (turquoise blue 15) was performed using a Ti/TiO2 thin film photoanode prepared by sol-get method. Hundred percent of color removal and almost complete mineralization (95% at pH 2 and 85% at pH 8) where achieved after 6 h of photolectrocatalytic oxidation of 2.5 x 10(-5) mol L-1 AT15 dye in Na2SO4 mol L-1 under E = +1.2 V versus SCE. The method limitation occurs at dye concentration higher than 4 x 10-5 mol L-1, where the degradation rate becomes markedly slower. An important improvement in color removal and TOC reduction for 1 x 10(-3) mol L-1 metallophtalocyanine dye was achieved using a combined process. After 4 h of potential controlled electrolysis at -1.2 V on a cathode of platinum followed by 6 h of photoelectrocatalytic oxidation leads to 100% of color removal and 83% of TOC decay and eletrodeposition of 69% of the released copper originally presented as copperphtalocyanine complex, by electrodeposition on the cathode without any other treatment. (C) 2005 Elsevier Ltd. All rights reserved.

Influence of the morphology and microstructure on the photocatalytic properties of titanium oxide films obtained by sparking anodization in H3PO4

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Ceramic materials in dentistry: historical evolution and current practice

Dental ceramics are presented within a simplifying framework allowing for facile understanding of their development, composition and indications. Engineering assessments of clinical function are dealt with and literature is reviewed on the clinical behaviour of all-ceramic systems. Practical aspects are presented regarding the choice and use of dental ceramics to maximize aesthetics and durability, emphasizing what we know and how we know it.