Catalysis and temperature dependence on the formation of ZnO nanoparticles and of zinc acetate derivatives prepared by the sol-gel route

The chemical and structural nature of powders prepared from the zinc acetate-derived precursor using the sol-gel route is discussed. The influence of the synthesis temperature and of the hydrolytic catalyst on the structural features of the powder is focused on the basis of X-ray powder diffraction (XRPD) and extended X-ray absorption fine structure (EXAFS) measurements and complemented with density and thermoanalysis (TG-DTA) results. EXAFS and XRPD results show that no-washed nanoparticulate powders are composed of a mixture of ZnO (wurtzite), zinc acetate, and zinc hydroxyacetate. The latter has a layered structure typical of hydroxy double salts (HDS). The main component of no-washed powders is always unreacted zinc acetate solid but the relative amount of the zinc-based compounds depends on the nature of the hydrolytic catalyst, hydrolysis ratio, and of synthesis temperature. According to the proportion of the three zinc-based compounds, three families of powders could be distinguished. The amount of ZnO nanoparticles (1.6 +/- 0.6 nm) decreases as the synthesis temperature increases, as the hydrolysis ratio decreases, or by changing from basic to acid catalysis. This finding suggests that the formation of zinc compounds is controlled by the equilibrium between hydrolysis-condensation and complexation-reprecipitation reactions.

Preparation of Pb(Zr,Ti)O-3 thin films by soft chemical route

Lead zirconate titanate, Pb(Zr0.3Ti0.7)O-3 (PZT) thin films were prepared with success by the polymeric precursor method. Differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FT-IR), Micro-Raman spectroscopy and X-ray diffraction (XRD) were used to investigate the formation of the PZT perovskite phase. X-ray diffraction revealed that the film showed good crystallinity and no presence of secondary phases was identified. This indicates that the PZT thin films were crystallized in a single phase. PZT thin films showed a well-developed dense grain structure with uniform distribution, without the presence of rosette structure. The Raman spectra undoubtedly revealed these thin films in the tetragonal phase. For the thin films annealed at the 500-700 degreesC range, the vibration modes of the oxygen sublattice of the PZT perovskite phase were confirmed by FT-IR. The room temperature dielectric constant and dielectric loss of the PZT films, measured at 1 kHz were 646 and 0.090, respectively, for thin film with 365 nm thickness annealed at 700 degreesC for 2 h. A typical P-E hysteresis loop was observed and the measured values of P-s, P-r and E-c were 68 muC/cm(2), 44 muC/cm(2) and 123 kV/cm, respectively. The leakage current density was about 4.8 x 10(-7) A/cm(2) at 1.5 V. (C) 2003 Elsevier Ltd. All rights reserved.

Preparation, microstructural and electrical characterization of SrTiO3 thin films prepared by chemical route

Polycrystalline SrTiO3 thin films having a cubic perovskite structure were prepared at different temperatures by the polymeric precursor method on platinum-coated silicon substrate. Crystalline films with uniform composition and thickness were prepared by spin-coating and the post-deposition heat treatment was carried out at different temperatures. The film showed good structural, dielectric, and insulating properties, Scanning electron microscopy (SEM) micrographs showed no occurrence of interdiffusion between the bottom electrode (platinum) and the film during post-annealing, indicating a stable interface between the SrTiO3 and the bottom electrode. The dielectric constant and dissipation factor at a frequency of 100 kHz were 250 and 0.01, respectively, for a 360 nm thick film annealed at 600 degreesC. The capacitance versus applied voltage characteristics showed that the capacitance was almost independent of the applied voltage. The I-V characteristics were ohmic in low fields and a Schottky emission and/or Poole-Frenkel emission were postulated in high fields. Room temperature leakage current density was found to be in the order of 10(-7) A/cm(2) for a 360 nm thick film in an applied electric field of about 100 kV/cm. The charge storage density of 36 fC/mum(2) was obtained in an applied electric field of about 100 kV/cm. (C) 2001 Published by Elsevier B.V. Ltd. All rights reserved.

SAXS study of monodispersed silica nanospheres obtained by an amino acid route

Spherical silica nanoparticles were prepared using a basic amino acid catalysis route and the kinetics of the particles growth was investigated by small angle X-ray scattering (SAXS). L-arginine was used in the polar aqueous phase as the basic catalyst whereas the tetraethylorthosilicate (TEOS) was dissolved in the cyclohexane oil phase as the silicate monomer source. The SAXS measurements were taken in the aqueous phase at different reaction times. A high degree of monodispersity was clearly evidenced for the spherical nanoparticles as a result of the pronounced high-order oscillations observed in the SAXS curves. The SAXS data show that the particles number density remains unchanged since both the particle size as well as the volume fraction gradually increase. This process was discussed based on a reaction-controlled addition of monomer species at the surface of the growing particles. Consequently, the monodispersed spherical nanoparticles radius can as such be finely tuned from 7 to 12 nm by varying the reaction time. (C) 2010 Elsevier B.V. All rights reserved.

Leakage current, ferroelectric and structural properties in Pb(1-x)Ba(x)TiO(3) thin films prepared by chemical route

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

The influence of the synthesis route on the final properties of SnO2-based varistors

A comparative study of two customary routes of ceramics processing applied to the synthesis of SnO2-based varistors is reported in this paper. Devices of equivalent composition were prepared through the Pechini method and through directly mixing the oxides without the addition of anti-agglomerants or binders. The microstructures of the sintered samples were characterised with X-ray diffraction and scanning and transmission electron microscopies. The electrical behaviour of the devices was studied on the basis of the current density versus electric field (J-E) characteristics and impedance spectroscopy measurements. The Pechini method ensures the homogeneity in the distribution of the additives in the tin oxide matrix but the formation of secondary phases seems to be independent of the synthesis route. Devices with similar non-linear coefficients of 18 and 21 were obtained through the mixed oxides route and the Pechini method, respectively. (C) 2007 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Cyclosporine-a and bone density around titanium implants: A histometric study in rabbits

Aim: Cyclosporine A (CsA) is an immunosuppressive agent commonly used to prevent organ transplantation rejection. It has been demonstrated that CsA may negatively affect osseointegration around dental implants. Therefore, the aim of this study was to evaluate the effect of CsA administration on bone density around titanium dental implants. Materials and Methods: Fourteen New Zealand rabbits were randomly divided into 2 groups with seven animals each. The test group (CsA) received daily subcutaneous injection of CsA (10mg/kg body weight) and the control group (CTL) received saline solution by the same route of administration. Three days after the beginning of immunosuppressive therapy, one machined dental implant (7.00 mm in lenght and 3.75 mm in diameter) was inserted bilaterally at the region of the tibial methaphysis. After 4 and 8 weeks the animals were sacrificed and the histometrical procedures were performed to analyse the bone density around the first four threads of the coronal part of the implant. Results: A significant increase in the bone density was observed from the 4- to the 8 week-period in the control group (37.41% + 14.85 versus 58.23% + 16.38 - p <0.01). In contrast, bone density consistently decreased in the test group overtime (46.31% + 17.38 versus 16.28 + 5.08 - p <0.05). In the 8-week period, there was a significant difference in bone density between the control and the test groups (58.23 + 16.38 eand16.28 + 5.08 - p= 0.001). Conclusion: Within the limits of this study, long-term CsA administration may reduce bone density around titanium dental implants during the osseointegration process.