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.

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.

Barium strontium titanate nanocrystalline thin films prepared by soft chemical method

Barium strontium titanate (Ba0.65Sr0.35TiO3) nanocrystalline thin films, which were produced by the soft chemical method, were crystallized at low temperature using a domestic microwave oven. A SiC susceptor were used to absorb the microwave energy and rapidly transfer the heat to the film. Low microwave power and short time have been used. The films obtained are crack-free, well-adhered, and fully crystallized. The microstructure displayed a polycrystalline nature with nanograin size. The metal-BST-metal structure of the thin films treated at 700 degrees C show food electric properties. The ferroelectric nature of the BST35 thin film was indicated by buttertly- shaped C-V curves. The capacitance-frequency curves reveal that the dielectric constant may reach a value up to 800 at 100kHz. The dissipation factor was 0.01 at 100kHz. The charge storage density as function of applied voltage graph showed that the charge storage densities are suitable for use in trench type 64 Mb ( 1-5 mu C/cm(2) and 265 Mb (2-11 mu C/cm(2)) DRAMs. (C) 2007 Elsevier Ltd. All rights reserved.

Synthesis of nanocrystalline tetragonal zirconia by a polymeric organometallic method

A polymeric precursor method based on the Pechini process was successfully used to synthesize zirconia-12 mol% ceria ceramic powders, the influence of the main process variables (citric acid-ethylene glycol ratio, citric acid-total oxides ratio and calcination temperature) on phase formation and powder morphology (surface area and crystallite size) were investigated. The thermal decomposition behavior of the precursor is presented. X-ray diffraction (XRD) patterns of powders revealed a crystalline tetragonal zirconia single-phase, with crystallite diameter ranging from 6 to 15 nm. The BET surface areas were relatively high, reaching 95 m(2) g(-1) Nitrogen adsorption/desorption on the powders suggested that nonaggregated powders could be attained, depending on the synthesis conditions. Copyright (C) 1999 John Wiley & Sons, Ltd.

Titania-based organic-inorganic hybrid planar waveguides

Eu3+ -doped titania-silica planar waveguides were prepared from tetraethylorthotitanate (TEOT) and modified silane 3-amino-propyltriethoxysilane (APTS). Films were deposited on borosilicate glass substrates by a dip-coating technique. The refractive index, the thickness and the total attenuation coefficient of the waveguides were measured at 632.8 and 1550 nm by prism coupling technique. Starting from pure titania films, the addition of modified silane leads to a decrease in the refractive index and an increase in thickness. Squared electric field simulation has shown that the light confinement in the waveguide increases with the silane content of the so]. Emission spectra present a broad emission band due to the modified silane and EU emission transitions arising mainly from the D-5(0) level to the F-7(J) (J = 0-4) manifolds. The dependence of transition intensities and excited state lifetimes on the initial composition and also on the heat treatment performed was interpreted in terms of structural changes occurring during the preparation process. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Nanocrystalline Ga1-xMnxN films grown by reactive sputtering

The growth of nanocrystalline Ga1-zMnxN (0.00 <= x <= 0.18) films grown by reactive RF-magnetron sputtering is focused here for the first time. The films were grown in a N-2 atmosphere by co-sputtering technique using a Ga target covered with small pieces of Mn onto c-GaAs (10 0), c-Si (10 0) and amorphous SiO2 substrates maintained at 500 K. Scanning electron microscopy and X-ray diffraction (XRD) experiments did not show any evidence for Mn segregation within the studied composition range. EDX measurements show that the Mn concentration is increased monotonically with the fraction of the target area covered by Mn. The XRD characterization show that the films are nanocrystalline, the crystallites having mean grain sizes in the 15-19 nm range and wurtzite structure with preferential growth orientation along the c-axis direction. The lattice parameters of alpha-GaN (a and c) increase practically linearly with the increase of Mn incorporation. The changes in the structural properties of our films due to the Mn incorporation are similar to those that occur in ferromagnetic GaMnN single-crystal films. (c) 2006 Elsevier B.V. All rights reserved.

Determination of the local site occupancy of Eu3+ ions in ZnAl2O4 nanocrystalline powders

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Phase Transformation in Titania Nanocrystals by the Oriented Attachment Mechanism: The Role of the pH Value

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

Structural and properties of nanocrystalline WO3/TiO2-based humidity sensors elements prepared by high energy activation

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

Morphology and topography analysis of mesoporous titania templated by micrometric latex sphere arrays

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

Microwave-assisted hydrothermal synthesis of nanocrystalline SnO powders

Tin oxide (SnO) powders were obtained by the microwave-assisted hydrothermal synthesis technique using SnCl2 center dot 2H(2)O as a precursor. By changing the hydrothermal processing time, temperature, the type of mineralizing agent (NaOH, KOH or NH4 OH) and its concentration, SnO crystals having different sizes and morphologies could be achieved. The powders were characterized by X-ray diffraction (X-ray), Field Emission Scanning Electron Microscopy (FE-SEM), High Resolution Transmission Electron Microscopy (HR-TEM) and Selected Area Electron Diffraction (SAED). The results showed that plate-like form is the characteristic morphology of growth and the TEM analyses indicate the growth direction as (200). (c) 2007 Elsevier B.V. All rights reserved.

Photoelectrocatalytic production of active chlorine on nanocrystalline titanium dioxide thin-film electrodes

The production of chlorine and hypochlorite is of great economical and technological interest due to their large-scale use in many kinds of commercial applications. Yet, the current processes are not without problems such as inevitable side reactions and the high cost of production. This work reports the photoelectrocatalytic oxidation of chloride ions to free chlorine as it has been investigated by using titanium dioxide (TiO2) and several metal-doped titanium dioxide (M-TiO2) material electrodes. An average concentration of 800 mg L-1 of free chlorine was obtained in an open-air reactor using a TiO2 thin-film electrode biased at +1.0 V (SCE) and illuminated by UV light. The M-doped electrodes have performed poorly compared with the pure TiO2 counterpart. Test solutions containing 0.05 mol L-1 NaCl pH 2.0-4.0 were found to be the best conditions for fast production of free chlorine. A complete investigation of all parameters that influence the global process of chlorine production by the photoelectrocatalytic method such as applied potential, concentration of NaCl, pH solution, and time is presented in detail. In addition, photocurrent vs potential curves and the reaction order are also discussed.

Nucleation and crystallization of titania nanoparticles in silica titania planar waveguides: A study by low frequency Raman scattering

SiO2 (1-x) - TiO2 (x) waveguides, with the mole fraction x in the range 0.07 - 0.20 and thickness of about 0.4 μm, were deposited on silica substrates by a dip-coating technique. The thermal treatments at 700-900°C, used to fully densify the xerogels, produce nucleation of TiO2 nanocrystals even for the lowest TiO2 content. The nucleation of TiO2 nanocrystals and their growth by thermal annealing up to 1300°C were studied by waveguide Raman spectroscopy, for the SiO2 (0.8) - TiO2 (0.2) composition. By increasing the annealing temperature, the Raman spectrum evolves from that typical of the silica-titania glass to that of anatase, but brookite phase is dominant at intermediate temperatures. In the low. frequency region (5-50 cm-1) of the Raman spectra, acoustic vibrations of the nanocrystals are observed. From the measured line shapes, we can deduce the size distribution of the particles. The results are compared with those obtained from the line widths in the X-ray diffraction patterns. Nanocrystals with a mean size in the range 4-20 nm are obtained, by thermal annealing in a corresponding range of 800-1300°C.