National Institute Of Materials Physics - Romania

A new HA/Y2O3:alpha Al2O3 system was obtained by the deposition of a hydroxyapatite thin layer (similar to 150 nm), by magnetron sputtering, onto sintered substrates of low yttria (150 ppm) doped alumina. The yttria doped alumina was synthesized from very pure nanopowders, by mechanical homogenization, followed of pressing, sintering and different annealing regimes, in order to obtain bodies with various degree of nano-micro-structuration. TEM/HRTEM, SEM and EDS morpho-compositional analysis techniques were used to characterize the yttria doped alumina substrate and the hydroxyapatite superficial layer. The interfacial bonding strength between the sintered substrate and the hydroxyapatite thin film was analyzed by SEM. The evolution of the grains growth of the Y2O3:alpha Al2O3 substrate samples, with and without the hydroxyapatite covering layer is observed and discussed. A strong structural interdependence between the covering layer and the sintered substrate was emphasized. The grains' growth behaviour of the studied samples showed a linear evolution. A mathematical model for the grain growth process description was built, the grain size being interpreted as a random variable having a log-normal or Weibull probability density function.

We report on the synthesis of electrode layers by Pulsed Laser Deposition technique. We selected Nickel Oxide-8Yttria-Stabilized Zirconia as anode, La0.6Sr0.4Co0.2Fe0.8O3-delta perovskite material as cathode, and Yttria doped (Ceria-alpha Alumina) as electrolyte. We studied electrode structure (average grain size, porosity, and grain shape), the deposition uniformity and electrode-electrolyte interfaces. The electrodes were investigated in terms of morphology (Scanning Electron Microscopy) and composition (Energy Dispersive X-ray Spectroscopy). The initial powder and the synthesized cathodes have been investigated superficially and in bulk by Mossbauer spectroscopy, in order to detect and analyse local properties. We identified the conditions for electrode layer synthesis in respect with porosity, composition, and mean grain size.

N-type P-doped silicon single crystals with resistivity higher than 8000 Omega cm were irradiated with I-127(6+) ions of 28 MeV kinetic energy. The penetration of the ions through the target and the processes of energy loss were simulated using the CTRIM Monte Carlo code, and point defect production was calculated in the frame of our diffusion-reaction model. Trapping phenomena were investigated using the method of thermally stimulated currents without applied bias. The modeling of the current-temperature curves takes into consideration both point defects and stress-type trapping centers, produced by the ions stopped into the crystal.

This paper reports on the conduction mechanisms in amorphous SiO2 films with embedded Ge nanoparticles. For this, measurements of current-temperature and current-voltage were employed and correlated with the microstructure results obtained from transmission electron microscopy (TEM). TEM images reveal that our films contain big Ge nanoparticles with low density and small Ge nanoparticles with high density, the last ones being the only responsible for the electrical transport. Two transport mechanisms were found at low and high temperature respectively, namely hopping on localized states in a band near Fermi level and charge excitation to the extended states at mobility edge.

In this paper we continue the previous investigations on nanostructured GexSi1-x films. The films were deposited by magnetron sputtering and annealed in N-2 atmosphere at 700 degrees C. Their structure was investigated and correlated with the electrical behavior. For this, conventional and high-resolution transmission electron microscopy together with selected area electron diffraction was used. Electrical measurements of current-voltage and current-temperature curves were made. The majority of crystallites that forms the films have the composition Ge50Si50 and 15 - 30 nm size. The I - T characteristics have Arrhenius dependence, with two activation energies interpreted as transitions between quantum confinement levels.

In this paper the electrochemical analysis of new materials, designed to be used as solid electrolytes for intermediate temperature fuel cells (IT-SOFC) was made. The materials are two different composites based on ceria 10YDC + (10%) 150ppm YA and 10ScDC + (10%) 150ppm YA, obtained by sol-gel method and sintered at temperature of 1500 degrees C. The electrochemical investigation was performed by Electrochemical Impedance Spectroscopy technique. According of these analyses the composite 10YDC + (10%) 150ppm YA presents better conductivity than 10ScDC + (10%) 150ppm YA. These results were related with morphological investigation, realized by SEM.

The hydrogen storage material lithium borohydride was infiltrated from solvent solution into the pores of the carbon replica of MSU-H mesoporous silica by the incipient wetness method. Different amounts of lithium borohydride up to 40 % from the weight of the high surface area carbonic material were used. By this method was achieved a good dispersion of the hydride into the carbonaceous support. The hydrogen desorption starts at temperatures as low as 150 degrees C for the sample with 8 wt% LiBH4 dispersed onto the MSU-H carbon replica while pure LiBH4 does not release hydrogen below 300 degrees C. After rehydrogenation, a lower amount of hydrogen is desorbed due to the fact that increasing temperature up to 400 degrees C a part of hydride segregates outside the pores of the carbonaceous support.

In this paper we present electron paramagnetic resonance (EPR) and Mossbauer (transmission method, TMS and measurements in the scattering method, CEMS) experiments on Fe-57 (0.11at.%) doped nanocrystalline anatase-type TiO2, synthesized by a hydrothermal method. Different Fe3+ and Fe2+ ions positions, with various hyperfine interactions evidenced in Mossbauer spectra (MS), confirm a partial magnetic ordering at room temperature. The magnetic hyperfine fields in the TMS spectra, better resolved at lower temperatures, do not change essentially with temperature. The first CEMS measurements, carried out on iron-doped TiO2 nanoparticles, reveal a larger disorder in the surface particles layer. The temperature dependence of the double integral EPR spectral intensity, proportional with the sample susceptibility, shows an anomalous behaviour. It suggests the bound magnetic polaron (BMP) mechanism for the magnetic ordering.

The formation and crystallization of disordered nanosized ZnO resulting from the thermal decomposition of nanocrystalline hydrozincite [Zn-5(CO3)(2)(OH)(6)] has been Observed and investigated during pulse annealing experiments Up to 625 degrees C in air or vacuum by electron paramagnetic resonance of trace amounts of substitutional Mn2+ impurity ions, in correlation with X-ray diffraction and transmission electron microscopy measurements. The mesoporous structure of the disordered ZnO, which initially forms in air and vacuum at 225 and 175 degrees C, respectively, further transforms into nanocrystalline ZnO of increasing particle size and improved lattice quality at higher annealing temperatures. The crystallization process, which does not affect the concentration of the substitutional impurity ions, as well as the simultaneous presence of both disordered and crystalline phases, should be considered in further applications of the resulting nanosized ZnO.

A mesoporous structure of self-assembled nanocrystals of cubic ZnS doped with Mn2+ ions with a homogeneous distribution of pores of similar size was synthesized at room temperature by a surfactant-assisted liquid-liquid reaction. The component nanocrystals exhibit a high crystallinity and a tight size distribution centered at 2 nm, as well as the narrowest Electron Paramagnetic Resonance (EPA) spectra linewidth and the best resolution reported so-far, effects attributed to self-assembling. The observed EPA spectra consist of lines from the substitutional Mn2+(I) and surface Mn2+(II) and Mn2+(III) centers. Here we show that, in contrast with previous reports, our EPA spectra are highly sensitive to structural changes during pulse annealing in vacuum up to 500 degrees C. The changes are related to the transformation of the surface Mn2+ centers in new Mn2+ centers, attributed to an oxidation process in which the thermal decomposition of the Tween 20 additive, also observed by EPA, seems to be involved. We have also been able to observe, for the first time by EPR spectroscopy, the formation of the ZnO phase and the nanocrystals size increase, which occur during annealing up to 500 degrees C, structural changes confirmed by XRD and TEM observations on the samples previously investigated by EPR.