Synthesis and electrical characterization of tungsten doped Pb(Zr0.53Ti0.47)O-3 ceramics obtained from a hybrid process

Pure and W-doped PZT ceramics (PZT and PZTW) were prepared by a hybrid process consisting in the association of polymeric precursor and partial oxalate methods. The phase formation was investigated by simultaneous thermal analysis (TG/DSC) and X-ray diffraction (XRD). The effect of W doping PZT and their electrical properties was evaluated. Substitution of W by Ti leads to an increase of Curie temperature and broadening of dielectric constant. A typical hysteresis loop was observed at room temperature and the remnant polarization was increased with the content of W. (c) 2007 Elsevier B.V. All rights reserved.

X-ray powder data and bond valence of La0.65Sr0.35MnO3 after Rietveld refinement

Powder X-ray diffraction (XRD) data were collected for La0.65Sr0.35MnO3 prepared through an alternative method from a stoichiometric mixture of Mn2O3, La2O3, and SrO2, fired at 1300 degreesC for 16 h. XRD analysis using the Rietveld method was carried out and it was found that manganite has rhombohedral symmetry (space group R(3) over bar c). The lattice parameters are found to be a=5.5032 Angstrom and c=13.3674 Angstrom. The bond valence computation indicates that the initial inclusion of Sr occurs at higher temperature. (C) 2002 International Centre for Diffraction Data.

Properties and in vivo investigation of nanocrystalline hydroxyapatite obtained by mechanical alloying

Mechanical alloying has been used successfully to produce nanocrystalline powders of hydroxyapatite (HA) using three different procedures. The milled HA was studied by X-ray diffraction, Infrared, Raman scattering spectroscopy and Scanning Electron Microscopy (SEM). We obtained HA with different degrees of crystallinity and time of milling. The grain size analysis through SEM and XRD shows particles with dimensions of 36.9, 14.3 and 35.5 nm (for (R1), (R2) and (R3), respectively) forming bigger units with dimensions given by 117.2, 110.8 and 154.4 nm (for (R1), (R2) and (R3), respectively). The Energy-Dispersive Spectroscopy (EDS) analysis showed that an atomic ratio of Ca/P= 1.67, 1.83 and 1.50 for reactions (R1), (R2) and (R3), respectively. These results suggest that the R1 nanocrystalline ceramic is closer to the expected value for the ratio Ca/P for hydroxyapatite, which is 513 congruent to 1.67. The bioactivity analysis shows that all the samples implanted into the rabbits can be considered biocompatible, since they had been considered not toxic, bad not caused inflammation and reject on the part of the organisms of the animals, during the period of implantation. The samples implanted in rabbits had presented new osseous tissue formation with the presence of osteoblasts cells. (C) 2004 Elsevier B.V. All rights reserved.

Synthesis by the polymeric precursor method and characterization of undoped and Sn, Cr and V-doped ZrTiO4

In this work, zirconium titanate doped with 0. 1, 0.2, and 0.4 mole% of tin, chromium and vanadium was synthesized by the polymeric precursors method and characterized by thermal analysis (TG/DTA), X-ray diffraction (XRD), nitrogen adsorption and scanning electronic microscopy (SEM). The powder presented two mass losses attributed to the exit of water and to the pyrolysis of the organic material. The surface area reduction observed from 500 degrees C indicates the beginning of the sintering process. All the dopants led to changes in the lattice parameters and to the decrease of both crystallite size and particle size. (c) 2005 Elsevier B.V. All rights reserved.

Effect of thermal treatment temperature on the crystallinity and morphology of LiTaO3 thin films prepared from polymeric precursor method

Lithium tantalate thin films (LiTaO3) with (50:50) stoichiometry were prepared by spin coating method using a polymeric organic solution. The films were deposited on silicon (100) substrates with 4 layers. The substrates were previously cleaned and then the solution of lithium tantalate was deposited by adjusting the speed at 5000 rpm. The thin films deposited were thermally treated from 350 to 600degreesC for 3 hours in order to study the influence of the thermal treatment temperature on the crystallinity, microstructure, grain size and roughness of the final film. X-ray diffraction (XRD) results showed that the films are polycrystalline and secondary phases free. The thickness of films was observed by scanning electron microscopy (SEM). The atomic force microscopy (AFM) studies showed that the grain size and roughness are strongly influenced by thermal treatment.

Effect of the bath pH on the electrodeposition of nanocrystalline Pd-Co alloys and their magnetic properties

The effect of the bath pH on the electrodeposition of nanocrystalline Pd-Co alloys and on their magnetic properties was studied. The pH practically did not affect the alloy composition. Conversely, the pH showed a significant influence on the shape and size of crystallites. Two different crystallites morphology were observed depending on the bath pH. A crystallite size ranging from 18.2 to 30 nm was obtained from X-ray diffractometry (XRD) patterns using the Scherrer's method. Also from the XRD patterns the lattice strain percentage was calculated and correlated with the residual stress, which probably originated during the film electrodeposition on the substrate. Some alloy magnetic properties showed small variations. In contrast, high and unexpected coercivities were obtained reaching a maximum of 1.69 kOe at pH 5.5. The high coercivity values were attributed to the presence of residual stress at the film-substrate interface, which increased as the bath pH and crystallite size decrease, both of them contributing simultaneously to increase in coercivity. (C) 2006 Elsevier B.V. All rights reserved.

The influence of residual stress and crystallite size on the magnetic properties of electrodepo sited nanocrystalline Pd-Co alloys

Nanocrystalline Pd-Co alloys were obtained by electrodeposition from an ammoniacal chloride bath. The influence of the crystallite size and the residual stress on the magnetic properties of the alloys was investigated. The residual stress increased as the applied current density was increased. It was associated to the high nucleation rate during electrodeposition and correlated to the lattice strain, estimated from the XRD patterns. Also from the XRD patterns the average crystallite size and the lattice constant were determined by Scherrer's and Rietveld's methods, respectively. Both parameters were directly influenced by the applied current density. Magnetic properties such as coercivity, remanence, saturation magnetization and squareness showed strong dependence on the residual stress and crystallite size. Coercivity higher than 1 kOe was achieved when a high current density was applied. High coercivity was attributed to the presence of residual stress and to the small crystallite size of deposits. (C) 2007 Elsevier B.V. All rights reserved.

Growth and characterization of BaBi2Nb2O9 thin films made by RF-magnetron sputtering

The RF-magnetron sputtering technique has been used to deposit polycrystalline thin films of layered-structured ferroelectric BaBi2Nb2O9 (BBN). The XRD patterns for the films annealed at 700degreesC for 1 hour show the presence of the BBN phase as well as the BaNb2O6 secondary phase. A better crystallization of the BBN phase and an inhibition of the secondary phase is obtained with the increase of temperature. The surface of the prepared films was rather dense and smooth with no cracks. The 300 nm thick BBN thin films exhibited a room-temperature dielectric constant of about 779 with a dissipation factor of 0.09 at a frequency of 100 kHz.

Development of Ti-Mo alloys for biomedical applications: Microstructure and electrochemical characterization

Ti-Mo alloys from 4 to 20 Mo wt.% were arc-melted. Their compositions and surfaces were analyzed by EDX, XRF and SEM. The Mo mapping shows a homogeneous distribution for all alloys. The XRD analysis showed that the crystal structure of the alloys is sensitive to the Mo concentration; a mixture of the hexagonal alpha' and orthorhombic alpha '' phases was observed for the Ti-4Mo alloy, and the alpha '' phase is observed almost exclusively when the concentration of Mo added to the Ti reaches 6%. A significant retention of the beta phase is observed for the alloy containing 10% Mo, while at higher Mo concentrations (15% and 20%), retention of phase beta is only verified. Preliminary electrochemical studies have indicated a valve-metal behavior and good corrosion resistance in aerated Ringer solution for all alloys. (c) 2006 Published by Elsevier B.V.

Microstructural and morphological analysis of pure and Ce-doped tin dioxide nanoparticles

Structural morphological studies in pure and Ce-doped tin dioxide nanoparticles with high stability against particle growth were performed in samples, obtained using the polymeric precursor method and prepared at different annealing temperatures. A Ce-rich surface layer was used to control the particle size and stabilize SnO2 against particle growth. The formation of this segregated layer can contribute to a decreased surface energy, acting in the driving force, or reducing the surface mobility. Only the cassiterite SnO2 phase was observed below 1000 degreesC and a secondary phase (CeO2) was observed for the Ce-doped SnO2 at temperatures higher than 1000 degreesC, when de-mixing process occurs. The evolution of crystallite size, microstrain and morphology of the nanoparticles with annealing temperatures was investigated by X-ray diffraction (XRD), associated to Rietveld refinements, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). (C) 2002 Elsevier B.V. Ltd. All rights reserved.

New X-ray powder diffraction data and Rietveld refinement for Gd2O3 monodispersed fine spherical particles

Nominally pure Gd2O3 C-form structure from basic carbonate fine spherical particles and its differences concerning the XRD data among literature patterns using Rietveld method is reported. Gd2O3: Eu3+ from basic carbonate and Gd2O3 from oxalate were also investigated. All samples, except the one from oxalate precursor, are narrow sized, 100-200 nm. Only non-doped Gd2O3 from basic carbonate presents XRD data with smaller d(hkl) values than the literature ones. From Rietveld refinement, non-doped Gd2O3 from basic carbonate has the smallest crystallite size and from oxalate shows the greatest one. Also, the unit cell parameters indicate a plan contraction of the Gd2O3 from basic carbonate. The presence of Eu3+ increases crystallite size when basic carbonate precursor is used to prepare Gd2O3 and avoids plan contraction. The structural differences observed among Gd2O3 samples obtained are related to the type of precursor and to the presence or not of doping ion. (C) 2003 Elsevier B.V. (USA). All rights reserved.

Preparation and characterization of nanosized SrBi2Nb2O9 powder by the combustion synthesis

This work presents the preparation of SrBi2Nb2O9 (SBN) directly by the combustion synthesis. Strontium nitrate, niobium ammonium oxalate (NH4H2[NbO-(C2O4)(3)].3H(2)O) and bismuth oxide were used as oxidant reactants and urea as fuel. The influence of the fuel was evaluated by the addition of different fuel amounts (50%, 100%, 200% and 300%), 100% being the stoichiometric proportion. The XRD patterns showed that the SBN perovskite crystallized as the majority phase. The as-synthesized stoichiometric powder presented a specific surface area of around 13 m(2)/g and a mean grain size of around 16 nm. Dilatometric measurements showed that the maximum sintering rate occurs at 1275degreesC. The determination of the ferroparaelectric transition showed a Curie temperature (T-c) of 429degreesC. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Microstructural and optical characterization of CaWO4 and SrWO4 thin films prepared by a chemical solution method

Stoichiometric CaWO4 and SrWO4 thin films were synthesized using a chemical solution processing, the so-called polymeric precursor method. In this soft chemical method, soluble precursors such as strontium carbonate, calcium carbonate and tungstic acid, as starting materials, were mixed in an aqueous solution. The thin films were deposited on glass substrates by means of the spinning technique. The surface morphology and crystal structure of the thin films were investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), and atomic force microscopy (AFM). Nucleation stages and surface morphology evolution of the thin films on glass substrates were studied by atomic force microscopy. The films nucleate at 300 degreesC, after the coalescence of small nuclei into larger grains yielding a homogeneous dense surface. XRD characterization of these films showed that the CaWO4 and SrWO4 phases crystallize at 400 degreesC from an inorganic amorphous phase. No intermediate crystalline phase was identified. The optical properties were also studied. It was found that CaWO4 and SrWO4 thin films have an optical band gap, E-gap=5.27 and 5.78 eV, respectively, of a direct transition nature. The excellent microstructural quality and chemical homogeneity confirmed that this soft solution processing provides an inexpensive and environmentally friendly route for the preparation of CaWO4 and SrWO4 thin films. (C) 2003 Elsevier B.V. All rights reserved.

beta-ZnMoO4 microcrystals synthesized by the surfactant-assisted hydrothermal method: Growth process and photoluminescence properties

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Structural Refinement and Photoluminescence Properties of MnWO4 Nanorods Obtained by Microwave-Hydrothermal Synthesis

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)