Publications

We were successful in synthesizing non-linear YBa(2)Cu(3)Ox whiskers, i.e. half loops or kinked shapes, which are promising candidates for solid-state devices based on the intrinsic Josephson effect and with improved electrical connections. We report on a complete characterization of their structural properties via a synchrotron nanoprobe as well as laboratory single-crystal diffraction techniques. This investigation allowed us to fully disclose the growth mechanism, which leads to the formation of curved whiskers. The superconducting properties are evaluated in comparison with their straight counterpart, revealing a strong functional analogy and confirming their potential applicability in superconducting electronic devices.

Experiments at the European X-ray Free Electron Laser (XFEL) require silicon pixel sensors which can withstand X-ray doses up to 1 GGy. For the investigation of X-ray radiation damage up to these high doses, MOS capacitors and gate-controlled diodes built on high resistivity n-doped silicon with crystal orientations and produced by two vendors, CiS and Hamamatsu, have been irradiated with 12 keV X-rays at the DESY DORIS III synchrotron light source. Using capacitance/conductance-voltage, current-voltage and thermal dielectric relaxation current measurements, the surface densities of oxide charges and interface traps at the Si-SiO2 interface, and the surface-current densities have been determined as function of dose. Results indicate that the dose dependence of the surface density of oxide charges and the surface-current density depend on the crystal orientation and producer. In addition, the influence of the voltage applied to the gates of the MOS capacitor and the gate-controlled diode during X-ray irradiation on the surface density of oxide charges and the surface-current density has been investigated at doses of 100 kGy and 100MGy. It is found that both strongly depend on the gate voltage if the electric field in the oxide points from the surface of the SiO2 to the Si-SiO2 interface. Finally, annealing studies have been performed at 60 degrees C and 80 degrees C on MOS capacitors and gate-controlled diodes irradiated to 5MGy and the annealing kinetics of oxide charges and surface current determined.

As synthesized mer-Alq(3) powder, obtained by wet chemical synthesis, has been subjected to different new characterization techniques such as Energy Dispersive X-ray, Cathodoluminescence and Scanning Electron Microscopy in order to identify their structural and photophysical properties. Other common techniques like X-ray diffraction, Raman and Fourier Transform Infrared spectroscopy have been involved in order to prove the formation of mer-Alq(3) compound. The vibrational spectroscopic properties were interpreted by using the output files from Gaussian software with B3YLP functionals and 6-311(d) basic sets. The growth kinetic of mer-Alq(3) nanocrystals in the alpha-phase has been evaluated by using the finite-size effects based on the Raman position peaks and their linewidths, which confirms the semiconductor character of the mer-Alq(3) compound. The XRD results suggest that the isothermal annealing increases the mer-Alq(3) nanocrystals, which modify the regular shape of typical spectral parameters from Raman peaks. (C) 2012 Elsevier B.V. All rights reserved.

Amination of bromobenzene with aniline was carried out on heterogeneous Au-TiO2 catalysts prepared using the deposition-precipitation method. The deposition of gold in loadings in the range 0.1-0.9 wt.% on titania occurred with the formation of gold particles with controlled size and oxidation state as demonstrated from TEM and XPS measurements. In addition, Raman and DR-UV-Vis investigation of these catalysts showed that the interaction of Au particles with the support stabilized the metallic state of gold. Catalytic results demonstrated that the conversion and selectivity depended on the gold-particle size and dispersion, while the mechanism of reaction was in direct relation with the reaction medium. Working in DMC, the solvent was playing the role of base. The advantage of working in DMC was avoiding the formation of KBr which is very difficult to be separated from the reaction products. HBr resulted as a by-product formed adducts with the coupling product, which was separated as crystals at room temperature by a simple filtration. However, in DMC, the reaction occurred with low selectivities. In dioxane, the presence of potassium ethoxide as base was mandatory. The reaction occurred with very high selectivities for moderate conversions. The conversion was limited by KBr released from the reaction. However, the use of the heterogeneous catalyst has the advantage of scavenger, since KBr becomes chemisorbed on the surface and could be simple removed by percolation and the catalyst can be reused. (C) 2012 Elsevier Inc. All rights reserved.

Lignin isolated from Miscanthus x giganteus using acidic (FAL) and basic (AL) conditions was thereafter subjected to catalytic depolymerization under thermal or ultrasonic activation. The characterization of lignin samples was achieved by thermogravimetric analysis and FTIR. Three different classes of catalysts containing nickel as the active species have been prepared in this respect: (i) nano-Ni(0) by reduction of NiCl2 with NaBH4 under ultrasonication, (ii) Fe3O4-(NiMgAlO)(x) and (NiAlO)(x) by calcination of Mg(Ni)-Al hydrotalcite incorporating Fe3O4, followed by reduction with hydrogen, and (iii) NiO(1 1 1) nanosheets by reduction of Ni(NO3)(2) with urea using benzyl alcohol as a structure directing agent. The catalysts were characterized by XRD and XPS techniques. Reduced mixed oxides displayed a moderate activity while a significant increase in conversion (up to 90%) was observed with nano-Ni(0) and NiO(1 1 1) nanosheets catalysts. The conversion and the mass distribution of the reaction products were strongly related to the procedure used for the extraction of lignin. In all the reactions AL samples had a greater extent of depolymerization. The performance from the tested catalysts under ultrasonic conditions was inferior to those tested under conventional heating conditions. The nature of the solvent was also found to be very important to this process, with the ionic liquid, 1-butyl-3-methylimidazolium acetate ([BMIM]OAc) demonstrating the best results in autoclave conditions and methanol under ultrasonic conditions. (C) 2012 Elsevier B. V. All rights reserved.

N-doped ZnO (ZnO: N) thin films, intended to be used as one of the layers in solar cell applications were deposited by r.f. sputtering, using ZnN target (99.9% purity), on silicon and fused silica substrates. In the gas flow composition, Ar was kept constant (50%) and the O-2/N-2 ratio was varied as: 40%/10%, 25%/25% and 10%/40%. After deposition, rapid thermal annealing (RTA) at 400 and 550 degrees C for 1 min in N-2 ambient has been performed. The RTA impact on the optical and microstructural properties of ZnO: N thin films have been investigated by X-ray diffraction (XRD), atomic force microscopy (AFM), transmission electron microscopy (TEM) coupled with selected area electron diffraction (SAED) and energy dispersive X-ray spectroscopy (EDX), UV-vis-NIR spectroscopy, UV-vis-NIR spectroscopic ellipsometry (SE) and infrared ellipsometry (IR-SE). The as-deposited (ad) ZnO: N films are polycrystalline with preferentially oriented columnar crystals. After RTA we found ZnO: N films with improved crystallinity and fewer boundary defects. We report optical constants of ZnO: N from UV to IR spectral range as well as the infrared active phononic modes. (C) 2012 Elsevier B. V. All rights reserved.

The hysteretic properties of metal-ferroelectric-semiconductor (MFS) structures based on Pb(Zr0.2Ti0.8)O-3 (PZT) and ZnO films were studied with respect of the quality of the PZT-ZnO interface. The films were grown by pulsed laser deposition (PLD) on platinized silicon (Pt/Si) substrate and on single crystal, (001) oriented SrTiO3 (STO) substrates. The structural analysis has revealed that the PZT-ZnO stack grown on single crystal STO is epitaxial, while the structure grown on Pt/Si has columnar texture. The temperature change of the capacitance-voltage (C-V) hysteresis direction, from clockwise at low temperatures to counter clockwise at high temperatures, was observed at around 300K in the case of the MFS structure grown by PLD on Pt/Si substrate. This temperature is lower than the one reported for the case of the PZT-ZnO structure grown by sol-gel on Pt/Si substrate (Pintilie et al., Appl. Phys. Lett. 96, 012903 (2010)). In the fully epitaxial structures the C-V hysteresis is counter clockwise even at 100K. These findings strongly points out that the quality of the PZT-ZnO interface is essential for having a C-V hysteresis of ferroelectric nature, with negligible influence from the part of the interface states and with a memory window of about 5V at room temperature. (C) 2012 American Institute of Physics. [http://dx.doi.org/10.1063/1.4765723]

Gas sensing peculiarities of chromiumoxide (Cr2O3) nanoparticles, obtained by hydrothermal reaction at moderate temperature and subsequent thermal annealing, were studied. The structure and morphology of the obtained Cr2O3 samples were investigated by X-ray diffraction and transmission electron microscopy techniques. Gas sensing measurements revealed their selective sensitivity to nitrogen dioxide (NO2) at 200 degrees C relative to carbon monoxide (CO), both in dry and humid air. Higher selectivity towards NO2 is attributed to the material surface reactivity even at low operating temperatures. This property was experimentally highlighted by work function changes, as a complementary investigation method to basic electrical resistance. Thus, it was observed that the surface reactivity of Cr2O3 (calcinated at 1000 degrees C) towards NO2 is higher compared to CO and less influenced by the relative humidity of the surrounding atmosphere. The present study reveals possible applications in the selective detection of NO2 based on Cr2O3. (C) 2012 Elsevier B.V. All rights reserved.

Ba(Zn1/3Ta2/3)O-3 (BZT) thin films were grown on Pt-coated Si substrates at 500 degrees C substrate temperatures by pulsed electron beam deposition method and post-annealed at 600 and 650 degrees C for 1 h. The X-ray diffraction patterns indicate that the as-grown films are partially crystallized but single-phase cubic perovskite structure was formed in annealed films. The temperature dependence of the dielectric constant of the BZT films was recorded in the -100 to + 100 degrees C range. The annealing treatment induces a decrease of the temperature coefficient of the dielectric permittivity with an order of magnitude, from 2000 to 100 ppm/degrees C. The influence of the annealing treatments on the temperature behavior of the BZT films was evidenced; a dielectric constant of about 21 at room temperature was obtained for the films annealed at 650 degrees C. (C) 2012 Elsevier B. V. All rights reserved.

The influence of target-substrate distance during pulsed laser deposition of indium zinc oxide (IZO), indium tin oxide (ITO) and aluminium-doped zinc oxide (AZO) thin films grown on polyethylene terephthalate (PET) substrates was investigated. It was found that the properties of such flexible transparent conductive oxide (TCO)/PET electrodes critically depend on this parameter. The TCO films that were deposited at distances of 6 and 8 cm exhibited an optical transmittance higher than 90% in the visible range and electrical resistivities around 5 x 10(-4) Omega cm. In addition to these excellent electrical and optical characteristics the films grown at 8 cm distance were homogenous, smooth, adherent, and without cracks or any other extended defects, being suitable for opto-electronic device applications. (C) 2012 Elsevier B. V. All rights reserved.