National Institute Of Materials Physics - Romania

Bio-glass films were deposited by radio-frequency magnetron sputtering technique onto medical grade Ti6Al7Nb alloy substrates from prepared silica based bio-glass target. A low deposition temperature was used (150 degrees C) and three different working pressures, followed by annealing in air at 550 and 750 degrees C. A quasi-stoichiometric target to substrate atomic transfer was found for Si, Ca and P, along with strong enrichment in Na and depletion in K and Mg, as evidenced by the energy dispersive microanalysis. The best results, taking into account stoichiometry and surface roughness, were obtained for the BG layers deposited at 0.3 Pa argon working pressure. The infrared spectroscopy of the as-sputtered and of the annealed films evidenced the characteristic molecular vibrations of silicate, phosphate and carbonate functional groups. The as-deposited films are amorphous and became partly crystalline after annealing at 750 degrees C, as evidenced by X-ray diffraction. The pull-out measurements, performed with a certified pull-test machine, gave very strong film-substrate adhesion strength values. For the non-crystalline layers, the pull-out strength is higher than 85 MPa, and decreases after annealing at 750 degrees C to 72.9 +/- 7.1 MPa. The main objective of this work was to establish the influence of the working pressure upon the composition and morphology of the as-deposited films, and of the annealing temperature upon structure and film substrate adhesion. (C) 2009 Elsevier B. V. All rights reserved.

The aim of this paper was to study the influence of crystallization heat treatments up to 750 degrees C, upon the integrity and structure of hydroxylapatite thin films. Two different types of hydroxylapatite coatings were investigated: abrupt structures prepared by magnetron sputtering and respectively functional graded structures deposited by a co-sputtering technique. A clear dependence was noticed between adherence values and annealing temperature and was correlated with the SEM, XRD and FTIR results. X-ray diffraction and FTIR measurements showed that the hydroxylapatite coatings annealed at 400 degrees C were less crystalline, similar to biological apatites. Over 550 degrees C, the apatite coatings obtained were well crystallized and preferentially oriented on (002) HA crystal plane. The adherence of HA coating increased with annealing the temperature up to 550 degrees C due to diffusion phenomena. At 550 degrees C the adhesion test results indicated better adhesion values in case of functional graded structures (> 85 MPa) in comparison with abrupt ones (similar to 70 MPa). At 750 degrees C an adherence decreasing occurred for both types of structures. This is mainly due to the effect of a significant thermal stress owed to the mismatch of the thermal expansion coefficients between the crystallized HA and Ti substrate. The presence of rutile lines in XRD spectrum suggests an increasing of the diffusion phenomena and a strong substrate oxidation at the HAM interface with annealing temperature.

Epitaxial ferroelectric PbZr0.2Ti0.8O3 thin films were grown by pulsed laser deposition. PbZr0.2Ti0.8O3 was doped with Cr acting as acceptor ion. Microstructural characterization was performed by (high resolution) transmission electron microscopy. The voltage dependence of polarization, dielectric constant, and leakage current were measured with respect to the Cr content. To derive the electronic properties, PZT was considered as a wide-gap semiconductor which allows treating the metal-PZT interface as a Schottky contact. The Cr was found to facilitate the elastic relaxation of the film. Furthermore, the leakage current was increased through a reduction of the Schottky barrier. (C) 2009 American Institute of Physics. [DOI: 10.1063/1.3141733]

The leakage current in epitaxial BiFeO3 capacitors with bottom SrRuO3 and top Pt electrodes, grown by pulsed laser deposition on SrTiO3 (100), SrTiO3 (110), and SrTiO3 (111) substrates, is investigated by current-voltage (I-V) measurements in the 100-300 K temperature range. It is found that the leakage current is interface-limited and strongly dependent on the orientation of the substrate. The potential barriers at the electrode interfaces are estimated to about 0.6, 0.77, and 0.93 eV for the (100), (110), and (111) orientations, respectively.

The structural peculiarities of titanium oxide films formed by pulsed laser deposition have been investigated. A pure titanium target was irradiated by a Nd:YAG laser (355 and 532 nm). The work studied the influence of the beam wavelength, and oxygen pressure (20, 40, 80, and 160 mTorr) upon the layer structure. The films deposited at room temperature were partly crystalline. The crystalline fraction was a mixture of titanium sub-oxides. The 532 nm wavelength seems to favour the oxidation of titanium leading to TiO(2) formation even at room temperature. After annealing, crystalline TiO(2-) anatase formed at both irradiation wavelengths, but only at low oxygen pressures (20 and 40 mTorr). The best crystallization occurs in the layers deposited at the lowest oxygen pressure (20 mTorr), at both laser beam wavelengths; most anatase formed in the sample obtained at 20 mTorr, 532 nm. At 20 mTorr the films were compact, for both wavelengths, but also tilted or randomly distributed columnar grains were observed at higher pressure. The films deposited with 355 nm, were thinner than those with 532 nm; at 355 nm the thickness decreased at higher pressure, while at 532 nm the dependence was opposite.

The characteristics of carbonic materials obtained by downstream deposition in a low pressure argon plasma beam injected with acetylene are reported. The influence of substrate temperature, presence of Ni catalyst and hydrogen in gas composition on the material properties is described. By increasing the substrate temperature, an enhanced order in the material is revealed by Raman spectroscopy, while FTIR measurements show a decreasing of the hydrogen content and the disappearing of sp(1) hybridized carbon in the deposit. The SEM and Raman investigation show a clear tendency of crystalline phases formation when hydrogen is assisting the deposition. (C) 2008 Elsevier B. V. All rights reserved.

Thin films of complex oxides have been obtained by pulsed-laser deposition (PLD) from glass targets belonging to the system Li2O-Al2O3-P2O5-(RE)(2)O-3, with RE = Nd, Pr, Er. The films were deposited on quartz, silicon and ITO/glass substrates using a F-2 laser (lambda = 157 nm, iota approximate to 20 ns) for ablation in vacuum. The structural, morphological and optical properties of the oxide films were investigated through IR and UV-VIS spectroscopy, Atomic Force Microscopy (AFM), Scanning Electron Microscopy, Energy Dispersive X-ray Spectroscopy (SEM-EDX) and Spectroscopic Ellipsometry. The laser wavelength was found to be the key parameter to obtain thin films with very smooth surface. In this way new possibilities are opened to grow multilayer structures for photonic applications. (C) 2008 Elsevier B. V. All rights reserved.

Mixtures of transparent and conductive oxides such as ITO-ZnO have been grown by a combinatorial pulsed laser deposition technique from two targets that were located 15 mm apart. The films were deposited on (1 0 0) Si and quartz substrates that were heated at temperatures from 300 to 500 degrees C. Measurements of the In to Zn ratios along the transversal axis of the substrates, which passes through the maximum thickness points corresponding to each target position were performed using energy dispersive X-ray spectroscopy and spectroscopic ellipsometry. From simulations of the X-ray reflectivity spectra, collected with a 2 mm mask on different locations along the transversal axis of the samples, the density and thickness of the deposited films were calculated and then the In to Zn ratios. The crystalline structure and electrical properties of the deposited films were also investigated along the same axis. Changes in the ratio of In/Zn along this axis resulted in changes of the film lattice constant and texture. (C) 2008 Elsevier B. V. All rights reserved.

Ferroelectric materials in thin film form, largely used in a broad variety of high-tech applications, are characterized by performing electrical measurements on capacitor-like structures. A complete characterization should include hysteresis, capacitance, and current measurements performed at different bias voltages, frequencies and temperatures. The analysis of the experimental data should be made considering that the real test structure is metal-ferroelectric-metal, and taking care of the direct impact of the microstructure on the macroscopically measured quantities. Further on, the theoretical models developed to simulate the experimental results should be able to explain simultaneously the data obtained from different types of electrical measurements. The main type of electrical measurements performed on ferroelectric capacitors will be discussed in detail. A special attention will be given to some important problems such as: the electrode-ferroelectric interfaces; calculation of the dielectric constant; intrinsic-versus-extrinsic contributions to the value of the dielectric constant--fake hysteresis loops and the question "Is the presence of the hysteresis cycle solid evidence for the presence of ferroelectricity?"; non-conventional contributions to the polarization charge and their effect on the frequency dependence of the hysteresis loop; conduction mechanisms in different ferroelectric materials. Some "hot" topic will be also discussed, as for example the validity of the serial model in the case of ferroelectric multilayers, and the coexistence of ferroelectric and antiferroelectric behavior in some structures and multilayers. The presentation is supported by experimental material collected by the author in the last 7 years, especially during his extended stay at the Max Planck Institute from Halle, Germany. The author is very grateful to V. Stancu, I. Vrejoiu and K. Boldyreva for providing most part of the samples, and to M. Alexe, D. Hesse and U. Goesele for the useful discussions and funding during the stay in Halle. Part of the experimental work was made in the frame of the contract CEEX-44-DINAFER, financed by the Romanian Ministry of Education and Research.

Imaging experiments at the XFEL pose unprecedented requirements to the detectors in terms of radiation tolerance: Fluxes of up to 10(16) (12 keVphotons/cm(2)) corresponding to approximately 10(9) Gy in silicon, are expected. An irradiation station has been set up in the DORIS beam line F4, MOS test structures have been irradiated, and first results on the dose dependence of the CN-characteristics, surface current density, and interface trap density have been obtained.