National Institute Of Materials Physics - Romania

The EPR, radioluminescence, and photoluminescence of cubic ZnS (cZnS) nanocrystals (NCs) with a narrow size distribution centered at 2 nm, doped with 0.1, 0.2, and 0.5 at.% Mn2+ ions were investigated. Besides the main lines from substitutional Mn2+ ions localized in the core of the NCs next to a stacking defect, the EPR spectra exhibited two broader hyperfine sextets, attributed to the so-called Mn(II)and Mn(III) surface centers, which could be separated by adequate thermal treatments. The contribution to the photoluminescence from the Mn2+ ions at various sites was further determined from the analysis of the steady-state and time-resolved photoluminescence data from cZnS: Mn NCs subjected to thermal treatments and from cZnS: Mn single crystals. Thus, the main emission consisting of two intense overlapping bands peaking at 596 and 630 nm was attributed to the T-4(1)-(6)A(1) transition of the substitutional Mn2+ ions in the core of the cZnS nanocrystals and to residual aggregated Mn2+ ions, respectively, the last ones being responsible for a broad EPR line observed in the X-band spectrum. The Mn(II) and Mn(III) centers, consisting of Mn2+ ions in the oxidized and hydrolyzed surface layer of the NCs, respectively, are only indirectly involved in the energy transfer to the substitutional Mn2+ centers, very likely through pairs interaction.

The trap parameters of defects in Si/CaF2 multilayered structures were determined from the analysis of optical charging spectroscopy measurements. Two kinds of maxima were observed. Some of them were rather broad, corresponding to "normal" traps, while the others, very sharp, were attributed to stress-induced traps. A procedure of optimal linear smoothing the noisy experimental data has been developed and applied. This procedure is based on finding the minimal value of the relative error with respect to the value of the smoothing window. In order to obtain a better accuracy for the description of the trapping-detrapping process, a Gaussian temperature dependence of the capture cross-sections characterizing the stress-induced traps was introduced. Both the normal and the stress-induced traps have been characterized, including some previously considered as only noise features. (C) 2011 American Institute of Physics. [doi: 10.1063/1.3525582]

Transmission electron microscopy and X-ray photoelectron spectroscopy analyses are performed to investigate Ge nanoparticles embedded in an amorphous SiO2 matrix. GeSiO thin films are prepared by two methods, sol-gel and radio frequency magnetron sputtering. After the deposition, the sol-gel films are annealed in either N-2 (at 1 atm and 800 A degrees C) or H-2 (at 2 atm and 500 A degrees C), and the sputtered films in H-2 (at 2 atm and 500 A degrees C), to allow Ge segregation. Amorphous Ge-rich nanoparticles (3-7 nm size) are observed in sol-gel films. Crystalline Ge nanoparticles in the high pressure tetragonal phase (10-50 nm size) are identified in the sputtered films. The size of the nanoparticles increases with Ge concentration in the volume of the film. At the film surface, the Ge concentration is much larger that in the volume for both sol-gel and sputtered films. At the same time, at the film surface, only oxidized Ge is observed.

The electronic structure of metallofullerene Ce@C-82 is probed by resonant x-ray emission spectroscopy at the Ce L-3 absorption edge. We observed a satellite structure in x-ray absorption and resonant emission spectra for Ce@C-82, which, we show, corresponds to the charge transfer induced by the core-hole potential in the final state, similarly to Pr@C-82. This charge-transfer satellite may be a common feature in metallofullerenes. The temperature dependence of the electronic structure is also investigated.

The attractive properties of ceria, particularly the conductivity and chemical stability, have led to vast research efforts to investigate, characterize and develop such materials. One of the main applications of this ceramic is in the solid oxides fuel cells for intermediate temperatures IT-SOFC. The aim of this work is the preparation and characterization of cubic ceria nanopowders doped with 10 mol % yttria or Scandia. A thermal treatment (calcinations) was applied on the obtained nanopowders, which were consequently investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM) and selected aria electron diffraction (SAED).

Yttria doped ceria reinforced with yttria doped alumina compound for IT-SOFC applications has been prepared by sol-gel method and sintered at 1300 degrees C, 1400 degrees C, 1500 degrees C. XRD, and SEM show the presence of a needle-like cerium-magnetoplumbite (CeAl11O17) phase in the compound; the oxygen deficient phase grows from the alumina phase by using ceria from the surrounding matrix and releasing oxygen ions As the sintering temperature is increased, the alumina phase is gradually transformed into CeAl11O17. Compared to the yttria doped ceria without reinforcement, the obtained compounds with ceria-magnetoplumbite show only a slight decrease of the Young elasticity modulus. However, the samples become brittle after backing in oxygen atmosphere (1000 degrees C, and 1500 degrees C).

Replacing the graphite with carbides in the mixture with Fe powder may be an alternative technological process, by the fact that as carbides decompose when heated, the carbon is set free and diffuses into the Fe network ensuring chemical and structural homogeneity corresponding to sintered steels. Using cementite nanopowder mix with Fe powder is to ensure a better compaction by pressing, less time to decompose and C diffusion into the Fe network in a remarkably chemical homogeneity. The obtaining procedure for Fe3C consists in direct carburation of Fe powder in a special chamber.

The optical band gaps of the nanocomposite TiO2-Ge thin films deposited by reactive co-sputtering method onto quartz and silicon substrates at different oxygen partial pressures have been investigated by the optical characterization method. Using 2%, 4% and 6% oxygen dilution in argon, an atomic content of 3%, 22% and 35% germanium in the TiO2 oxide matrix was obtained. Structural characterization of layers was performed by X-ray diffraction and the result revealed that no crystallization phenomena have occurred after the annealing at 700 degrees C. When increasing the annealing temperature, at 750 degrees C the TiO2 anatase phase crystallizes and subsequently it partially convert to the rutile polymorph (at 800 degrees C). The optical band gaps were analyzed using Tauc plot formula for direct and indirect transitions gap. Intermediate energy levels appear in the TiO2 energy gap and a slight increasing of the indirect transitions gap with germanium content was noticed.

Nano-hydroxyapatite bio-ceramics were synthesized by sol-gel method. The gel was dried at 80 degrees C for 96 h. The dried gels were individually heated at a rate of 5 degrees C/min up to 600 degrees C, 800 degrees C, and 1000 degrees C. X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were used for to characterize the composition, morphology and particle size of samples. At 800 degrees C a small amount of CaO (about 0.3 wt%) was detected in which increased after annealing at 1000 degrees C (about 1.1 wt%). The crystallites are elongated along the c crystallographic axis, but the size anisotropy decreases with increasing temperature above 800 degrees C. The size along the elongation axis increased from 43 nm at 80 degrees C to about 143 nm at 1000 degrees C, as determined by XRD, and from 120 to 280 nm, as measured by TEM. The functional groups were analyzed using Fourier transform infrared (FTIR) and Raman spectroscopies confirming the presence of various and PO43 and OH- bands in the samples. After calcination at 1000 degrees C the bands are more intense which indicates an increase in the cristallynity. The photoluminescence (PL) of HAp treated at various temperatures (80, 600, 800, 1000 degrees C) was also studied. hFOB 1.19 osteoblats cells were used to determine cell proliferation, viability and citotoxicity after interaction with the prepared bioceramics. To evaluate cell proliferation rate quantitative by the hFOB 1.19 cells on HAp samples were cultured to 4 days. Cellular morphology was investigated using FESEM to obtain qualitative information of osteoblast cells on HAp samples. The number of hFOB 1.19 cells on control HAp_80, HAp_600, HAp_800 and HAp_1000 was 400 +/- 30, 360 +/- 25, 350 +/- 21, 320 +/- 16 and 300 +/- 10 after 4 days. Our results proved that the HAp sintered at 1000 degrees C promoted osteoblast cell attachment and adhesion.

The combined investigation techniques, electron probe microanalysis (EPMA), Mossbauer spectroscopy (NGR), transmission electron microscopy (TEM), selected area electron diffraction (SAED), X-ray diffraction (XRD),) evidenced the third level of the inclusions at nanosize scale for specific minerals of different Romanian metamorphic deposits. So, NGR technique reveals the contribution of the (Mn, Fe) oxides - small particles at standard (RT) and at very low temperature (LHeT) in the Fe-52 gamma - ray signal of manganoan-fayalites (Razoare deposit). The EM analysis techniques confirmed the presence of the nanometric Fe and Mn oxides inclusions in manganoan fayalites, as well as of pyroxferroite (Razoare deposit). On the other hand, an extensive investigation of the gold ores in the South Carpathians (Costesti, Valea lui Stan and Jidostita) has been performed by using a fruitful combination among the above mentioned complementary mineralogical and structural methods. The investigation of the representative sulfide samples by the structural techniques relieved new minerals in the gold ores, the presence of submicroscopic inclusions of uytenbogaardtite, cobaltite and loellingite as well as the "coral like" aggregates of nanometric gold.