National Institute Of Materials Physics - Romania

Hydroxyapatite (HAp) films, widely used as a biocompatible material for hard tissues repairing. are studied in this paper for a better control and understanding of the crystallization and densification of sol-gel deposited layers. Calcium nitrate and triethyl phosphite diluted in alcohols were used as calcium and phosphorus precursors. HAp coatings were obtained by spinning method, followed by drying and annealing in the range 130-750 degrees C. Specific temperatures of the chemical reactions of HAp formation have been revealed by thermogravimetric analysis (TG-DTA). Structural. chemical and optical characterizations of the films were performed by Scanning Electron Microscopy (SEM) with Energy Dispersive X-ray Analysis (EDX) facilities, X-ray diffraction (XRD). Fourier Transform Infrared Spectroscopy (FTIR) and Spectral Ellipsometry (SE). The film crystallinity increases with file annealing temperature above 550 degrees C. XRD lines of HAp crystallographic planes become narrow at 750 degrees. and correspond to a single crystallographic phase. The Film morphology depends not only on annealing history but also on the synthesis parameters. Thus. layers with large grains of well sinterized HAp nano-crystals can be obtained. Using EDX measurements, the Ca/P ratio was found close to the stoichiometric value in the well sinterized HAp grain regions and slightly increased 1.82 for boundary regions between grains. The density of pores usually observed in sol-gel derived films was estimated for different samples using modeling of SE data.

In this communication, we study the production of defects by energetic ions in silicon and germanium, at very low temperatures, as dependencies of non-ionizing energy loss and number of displacements on the ion kinetic energy, and also the partition of the energy deposited between ionization, creation of defects and phonons, short time after the interaction.

ZnO is a wide band-gap (ca. 3.4 eV) semiconductor, piezoelectric, pyroelectric, biocompatible, transparent in the visible spectrum and UV light emitting material. The fabrication in 2001 of the first nanobelts of semiconductor oxide materials lead to a rapid expansion of researches concerning one dimensional nanostructures (nanotubes, nanowires, nanobelts), given their possible application in optics, optoelectronics, piezoelectricity, catalysis. Researches carried on up to date evidenced the possibility to obtain an extraordinary variety of ZnO nanostructures, in function of the experimental parameters and the used growth methods. In this work we present morphostructural results on nanostructured ZnO layers obtained by electrochemical deposition. The films have been grown on gold covered glass plates and Si wafers, in various experimental conditions such as: nature of the wetting agents, electrical polarization of the substrate (continuous, pulsed). The influence of the growth conditions on the crystalline structure and morphology of the films is revealed by scanning and transmission electron microscopy studies. The films show a variety of growth morphologies, from entangled-wires-like to honeycomb-like layers. These large-specific-surface layers will be tested as nanostructured substrates for photovoltaic cells with improved efficiency.

Iron- and europium-doped (<= 1 at.%)TiO2 nanoparticles powders have been synthesized by a hydrothermal route at 200 degrees C, starting with TiCl4, FeCl3 center dot 6H(2)O and EuCl3 center dot 6H(2)O. The structure, morphology and optical peculiarities were investigated by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), extended X-ray absorption fine structure (EXAFS), Mossbauer spectroscopy and UV-vis measurements. The photocatalytic performance was analysed in the photodegradation reaction of phenol. Rietveld refinements of XRD patterns reveal that the as-prepared samples consist in iron- and europium-doped TiO2 in the tetragonal anatase structural shape, with particle size as low as 15 nm. By means of Mossbauer spectroscopy on both Fe-57 and Eu-151 isotopes as well as by EXAFS analyses, the presence of Fe3+ and/or Eu3+ ions in the nanosized powders has been evidenced. It was found that iron and europium ions can substitute for titanium in the anatase structure. From the UV-vis reflection spectra, by using the transformed Kubelka-Munk functions, the band gap energy (E-g) of the hydrothermal samples has been determined in comparison with that of Degussa P-25 photocatalyst. A decrease of E-g from 2.9eV found for Degussa photocatalyst to 2.8 eV for the titania doped with 1 at.% Fe has been evidenced, indicating a valuable absorption shift (similar to 20 nm) towards visible light region. However, the best photocatalytic activity in the photodegradation reaction of phenol was evidenced for the hydrothermal sample, TiO2: 1 at.% Fe, 0.5 at.% Eu, in both UV and visible light regions. The photocatalytic activities of iron-doped and iron-europium-codoped samples are high and practically the same only in visible light. The photocatalytic properties in Correlation with the structural and optical peculiarities of the hydrothermal samples are discussed. (C) 2008 Elsevier B.V. All rights reserved.

The nanostructure of Si-x(SiO2)(1-x) films deposited on quartz substrate, where x varies from 0 to 1, was determined by high-resolution transmission electron microscopy in the sample regions with x approximate to 0.1, 0.2. 0.5. and 0.75. In the Si-0.5(SiO2)(0.5) region, the formation of a Si nanocrystallite network was established. At high concentrations of Si nanocrystallites, nanotwins and stacking faults occurred in the crystallites. Large Si crystallites appeared at x >= 0.5 in the quartz Substrate under the interface, while the film presented nanopores over the interface. The mechanisms for the formation of the nanocrystallites were discussed and correlated with the film properties.

Despite many investigations already performed with respect to sintering stability and grain growth vs. annealing conditions in low yttrium doped alpha- Al2O3 (150 ppm) - some fundamental questions are still open. These questions concern mainly the influence of small level of impurities at grain boundary in the sintering behavior and grains growth of the materials, i.e. the microstructure function of the annealing time at annealing temperature of 1650 degrees C. The low yttrium doped alpha- Al2O3 (150 ppm) samples were sintered and annealed at high temperatures. Besides conventional micro structural studies, such as grain diameter and grain size functions of distribution of the annealing temperature were studied by electron microscopy investigations and statistical measurement. The implications of the different microstructures with respect to micro structural stability have discussed and compared to observations described in the literature.

N-doping is often used to improve the photocatalytic properties of TiO2, films in order to achieve visible light response. In this work, we study the effect of annealing treatment (temperature and atmosphere) on the structural and optical properties of undoped and N-doped TiO2, films by means of X-ray diffraction (XRD), Atomic Force Microscopy (AFM), Rutherford backscattering (RBS), X-ray photoelectron spectroscopy (XPS), spectroscopic ellipsometry (SE) and UV-VIS optical transmission spectroscopy. Porous five-layer TiO2, films were deposited by sol-gel method on quartz substrate and thermally treated in oxygen or NH3 flow at 500 and 600 degrees C. Significant doping effect was achieved after annealing at 600 degrees C in NH3 and a shift in optical bandgap value down to visible range (2.69 eV) was observed. (C) 2008 Elsevier B.V. All rights reserved.

Hydroxyapatite (HA) biocoatings were obtained using two different deposition methods: sol-gel and sputtering. A direct comparison of films obtained using different techniques is necessary because of possible formation of multi-phases and components in HA films. HA films were investigated using spectroscopic ellipsometry (SE) as a powerful method to evaluate composition and structural properties of the films. For both types of films, sputtering and sol-gel, a weak dispersion of the refractive index within the wavelength range 0.4-0.7 pm was found. This corresponds to a high energy bandgap and a high optical transparency in the UV-VIS range. The internal porosity varying in a wide range in the sol-gel films was evaluated using a modeling of SE data. Additionally to SE Studies, structural, chemical and optical characterizations of the Films were performed using Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). Two absorption bands observed in the wavelength ranges 550-600 cm(-1) and 1000-1200 cm(-1) can be attributed to the major absorption modes associated with HA in agreement with published data. Prom XPS analysis, the atom ratio Ca/P was found for sol-gel films close to the stoichiometric value 1.67. For sputtering films, a higher Ca/P ratio of about 2.1 was estimated. However, similar FTIR spectra have been recorded for both sputtering and sol-gel films. XRD Studies show also similar crystallization conditions by annealing at temperatures higher than 500 degrees C. (C) 2008 Elsevier B.V. All rights reserved.

Nano-scale ordering may be revealed in transmission electron microscopy (TEM) by at least three techniques that will be presented in this work: selected area electron diffraction, conventional TEM and high-resolution TEM. Digital image processing is used to extract additional information from the high-resolution micrographs. The described methods are illustrated in a microstructural and compositional study of a 90%Pb(Mg1/3Nb2/3)O-3-10%PbTiO2 ceramic sample. High-resolution images reveal the presence of ordered compositional nano-domains, observable in two specific crystallographic orientations. Antiphase boundaries lying in the (111) planes separate them, while (100) and (111) facets separate the ordered domains from the disordered matrix.