National Institute Of Materials Physics - Romania

We studied the chemical growth of calcium phosphate nanostructured coatings onto silicon wafers pre-covered with carbonated polycrystalline hydroxyapatite films. Silicon wafers were covered with hydroxyapatite thin layers by radio frequency magnetron sputtering and then immersed in 370 degrees C simulated body fluids for up to 20 days. Immersed structures were extracted every 2 days for studies by Fourier transform IR spectrometry. The chemically grown layers were further analyzed by X-ray diffraction and scanning electron microscopy. The growth kinetics of calcium phosphate deposits was monitored by estimating the area of phosphate, carbonate and water stretching bands of the recorded infra-red vibrational spectra. Sequential annealing in vacuum up to 950 degrees C was applied to elucidate the nature of incorporated water. Our studies revealed that the layers growing in simulated body fluid are rougher than initial hydroxyapatite interlayers, contain carbonates, include water in interlayer's voids and have therefore an increased biological activity for promoting faster implants integration with human bone tissues.

The microwaves are used for both civilian and military applications for communication and detection. Due to the emerging applications and the need for more bandwidth as well as for high speed there is a strong competition for ultra high frequencies devices. As it is know the size of different kind of microwave components is in a certain relation with the wavelength divided by root square of the dielectric permittivity. So the size of microwave component can be decreased by increasing the dielectric permittivity. Dielectric materials based on TiO2 are recommended for applications in electromagnetism and optics due to their nonlinear properties, to high value of the dielectric permittivity and their temperature behavior. The paper describes very shortly the technology applied to manufacture high dielectric permittivity materials based on TiO2 and microwave devices designed with this. In addition, the experimental data measured for a dielectric antenna are presented.

Epitaxial antiferroelectric/ferroelectric PbZrO3/PbZr0.8Ti0.2O3 multilayers were grown on SrRuO3-electroded SrTiO3(100) substrates by pulsed laser deposition. Polarization-field and switching current-voltage curves show a mixed antiferroelectric-ferroelectric behavior of the multilayers with an individual layer thickness above 10 nm, whereas below 10 nm the multilayers show only ferroelectric behavior. Clearly the PbZrO3 layers thinner than 10 nm experienced a transition into the ferroelectric state. X-ray diffraction reciprocal space mapping showed a corresponding orthorhombic-to-rhombohedral transition of the PbZrO3 layers. The observations are discussed in terms of the influence of strain.

Pb(Zr1-xTix)O-3 (PZT) thin films were prepared by sol-gel method on stainless steel (SS) and on platinum-coated silicon substrate (Pt/Si). The structure revealed by X-ray diffraction shows strong crystallographic orientation: (110) and (100), respectively. A small amount of pyrochlore phases (Pb-2(Zr,Ti)(2)O6-delta is formed in the films deposited on SS substrate. The crystallite size shows significant differences: d((00l))((SS)) = 27.1 nm, d((h00))((Pt)) = 88 nm. The tetragonal splitting is (Delta c/c)((SS)) = 3.55 % and (Delta c/c)((Pt)) = 3.32 %.

Hydroxyapatite (HAP) thin films (0.2 pm, 0.3 pm and 1.2 mu m thickness) were grown by RF magnetron sputtering in argon atmosphere onto silicon substrates at high deposition rates (0.6 mu m/h). Crystalline HAP films were obtained using a low temperature (100 degrees C) followed by post-deposition annealing at 300 degrees C, 450 degrees C, 500 degrees C and 550 degrees C in environmental air for 1 hour. An important influence of the films thickness upon the crystallization degree was noticed at intermediate annealing temperatures, as obtained from XRD measurements. For low and high temperatures similar values were obtained with a better crystallization degree for the thinner films. FTIR absorption led to the same conclusion considering the shape of stretching and bending PO4 lines. This suggests that the crystallization process has a diffusion component besides usual thermal activation process.

Fluorinated hydroxyapatite [Ca-10(PO4)(6)(OH)(x)F1-x] implantologic structures could constitute an alternative to classic hydroxyapatite [Ca-10(PO4)6(OH)21 ones in medical applications due to their bioactivity and low solubility. Bioactive apatites are usually used as coatings onto surface of biocompatible metals, leading to implants which take advantage of the coating's bioactivity and good mechanical properties of metals. In this work, powders and apatite type films were prepared on Ti6Al4V medical grade alloy using three sol-gel chemical routes by mixing different calcium and phosphorous precursors Ca(NO3)2, P2O5 and C6H15PO3, and two fluoride reagents: HPF6 and NH4F. The resulting calcium phosphates and fluorapatite/hydroxyapatite solid solution (FHA) compounds were investigated by SEM, XRD and evaluated in vitro in SBF Kokubo solution. An efficient preparation algorithm was designed for the Ca(NO3)(2+) C6H15PO3+ NH4F chemical route which produced monophasic powders with a high crystallinity degree. This chemical route led to FHA sol-gel coatings with bioactive potential.

Barium strontium titanate (BST) bulk ceramic with composition Ba0.5Sr0.5TiO3 was produced by solid-state reaction and was used as target for PLD thin film deposition. A Nd-YAG laser, working at 5-10 Hz and different wavelengths has been used. Thin films of stoichiometric BST were deposited on alumina substrate with the thickness between 400 and 500 nm. An aditional annealing was carried out at 800 degrees C for 6 h. XRD and SEM were used for sample characterization. Capacity measurements were performed versus temperature at 100 kHz in a large temperature range. A diffuse ferroelectric-paraelectric phase transition with T-C = -72 degrees C for the BST thin film was determined. A 5% tunability was measured in the transition region. (c) 2007 Elsevier B.V. All rights reserved.

Ceramic based barium strontium titanate (BST) solid solutions with the formula Ba1-xSrxTiO3 are very important candidates for a wide range device applications. Several doped (Mn and Mg) and undoped samples were prepared by standard solid-state reaction. Special emphasis was put on compositions with x=0.35 and 0.60, with high potential for applications. The samples were sintered at temperatures in the 1200 divided by 1260 degrees C range. Structural X-ray diffraction analysis preformed confirms the perovskite structure. The dielectric parameters were investigated in a wide temperature range between - 150 and 150 degrees C. The temperature was cyclically changed in both directions, up and down, at a rate of less than 2 degrees C/ min. Both permittivity and dielectric loss were measured at low frequencies, 1 kHz. The peak values of the permittivity are increasing from 2000 to 4000 with the sintering temperature increase. Moreover the dielectric parameters were measured at room temperature in microwave domain (1 divided by 2 GHz). The Curie temperature of BST samples with x=0.35 and x=0.6 is in agreement with the Curie point dependence on Sr content, as we have previously reported. (C) 2007 Published by Elsevier B.V.

The sol-gel deposition method has been successfully applied to obtain Pb(Zr0.2Ti0.8)03 thin films on platinized silicon wafers. Addition of different amounts (7-15 wt.%) of organic macromolecular polyvinylpyrrolidone in the precursor solution prior to spin coating proves to be an excellent method for obtaining porous films. The crystal structure of as deposited films was analyzed by X-ray diffraction. The porous films show perovskite phase after annealing at 650 degrees C. The surface morphology has been studied by Atomic Force Microscopy and Scanning Electron Microscopy. The surface profile indicates a roughness of the film of 5 nm and no microcracks on the surface. The ferroelectric behavior was proved for each film, by hysteresis loops and by the "butterfly" shape of the capacitance-voltage characteristics. The remnant polarization and the coercive field decrease while the amount of added PVP increases. (C) 2006 Elsevier B.V. All rights reserved.