Dynamical study of ZnO nanocrystal and Zn-HDS layered basic zinc acetate formation from sol-gel route

We have pointed out that zinc based particles obtained from ethanolic solution of a zinc acetate derivative (zinc oxy-acetate, Zn4O(Ac)(6)) are a mixture of nanometer sized ZnO, zinc oxy-acetate, and zinc hydroxide double salt (Zn-HDS). The knowledge of the mechanisms involved in the formation of ZnO and Zn-HDS phases, and the evolution of Zn species in reaction medium was monitored in situ during 14 h by simultaneous measurements of UV-vis absorption and extended X-ray absorption fine structures (EXAFS) spectra. This spectroscopic monitoring was initialized just after the addition of an ethanolic lithium hydroxide solution ([LiOH]/[Zn] = 0. 1) to the reaction medium kept under controlled temperature (40 degrees C). This study points out the first direct evidence of the reaction between ZnO nanoparticles and unreacted zinc oxy-acetate to form a Zn-HDS phase. The dissolution of ZnO and the reprecipitation of Zn-HDS are induced by the gradual release of water mainly produced by ethanol esterification well evidenced by gas chromatography coupled to mass spectroscopy and FT-IR measurements.

Oriented growth of Bi3.25La0.75Ti3O12 thin films on RuO2/SiO2/Si substrates by using the polymeric precursor method: Structural, microstructural and electrical properties

c-axis oriented Bi3.25La0.75Ti3O12 (BLT) thin films were grown on a RuO2 top electrode deposited on a (100) SiO2/Si substrate by the polymeric precursor method. X-ray diffraction and atomic force microscope investigations indicate that the films exhibit a dense, well crystallized microstructure having random orientations with a rather smooth surface morphology. The electrical properties of preferred oriented Bi3.25La0.75Ti3O12 (BLT) thin films deposited on RuO2 bottom electrode leaded to a large remnant polarization (P-r ) of 17.2 mu C/cm(2) and (V-c ) of 1.8 V, fatigue free characteristics up to 10(10) switching cycles and a current density of 2.2 mu A/cm(2) at 5 V. We found that the polarization loss is insignificant with nine write/read voltages at a waiting time of 10,000 s. Independently of the applied electric field the retained switchable polarization approached a nearly steady-state value after a retention time of 10 s.

SAXS study of the kinetics of formation of ZnO colloidal suspensions

We have investigated, by in situ small-angle X-ray scattering (SAXS), the kinetics of formation of zinc oxide colloidal suspensions obtained after refluxing alcoholic solution of zinc acetate and catalysed by lithium hydroxide. The experimental results demonstrate that the suspensions are composed of colloidal spheroidal particles with a multimodal size distribution. The average radius of the main mode, approximately 2 nm, is invariant but the number of these basic particles continuously increases for increasing hydrolysis reaction time. The other two modes correspond to particles with average radii close to 6 and 10 nm, respectively. The larger particles are formed by coagulation of the smaller ones. (C) 1999 Elsevier B.V. B.V. All rights reserved.

Thermal conductivity features of ZnO-based varistors using the laser-pulse method

The thermal conductivity of several commercial ZnO-based varistor systems was determined based on the laser-pulse method, a technique that proved extremely useful and easy to apply. Using this technique, the thermal conductivity was found to be dependent on the microstructural features of the devices, involving the mean grain size and phase composition. Among the phases existing in commercial ZnO-based varistors, ZniSb2O12 and Bi2O3 were found to contribute strongly to the thermal conductivity of the devices. (C) 2003 Elsevier B.V. All rights reserved.

Structural and microstructural behaviour of SnO2 dense ceramics doped with ZnO and WO3

SnO2-based varistors doped with ZnO and WO3 were prepared by mixed oxide method. Experimental evidence shows that the increase in ZnO amount increases the volume and microstrain of unit cell while the WO3 promotes a decrease. The effect of ZnO and WO3 additives could be explained by the substitution of Sn4+ by Zn2+ and W6+. The addition of WO3 inhibits the grain growth due to the segregation in the grain boundary without influence in the densification of the samples. Besides that, an increase in the electrical resistance of the SnO2-ZnO-WO3 system was observed independent of the WO3 concentration. (c) 2005 Elsevier B.V. All rights reserved.

Structural electrical and optical properties of undoped and indium doped ZnO thin films prepared by the pyrosol process at different temperatures

The influence of the substrate temperature on the structural features and opto-electrical properties of undoped and indium-doped ZnO thin films deposited by pyrosol process was investigated. The addition of indium induces a drastic decrease (by a factor approximate to 10(10) for samples deposited at 300 degreesC) in the electrical resistivity of films, the lowest electrical resistivity (6 mOmega-cm) being observed for the film deposited at 450 degreesC. Films are highly transparent (>80%) in the Vis-NIR ranges, and the optical band gap exhibits a blue shift (from 3.29 to 3.33 eV) for the In-doped films deposited at increasing temperature. Preferential orientation of the ZnO crystallites with the c-axis perpendicular to the substrate surface and an anisotropic morphology of the nanoporous structure was observed for films growth at 300 and 350 degreesC. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Electroluminescence of zinc oxide thin-films prepared via polymeric precursor and via sol-gel methods

Zinc oxide (ZnO) is an electroluminescent (EL) material that can emit light in different regions of electromagnetic spectrum when electrically excited. Since ZnO is chemically stable, inexpensive and environmentally friendly material, its EL property can be useful to construct solid-state lamps for illumination or as UV emitter. We present here two wet chemical methods to prepare ZnO thin-films: the Pechini method and the sol-gel method, with both methods resulting in crystalline and transparent films with transmittance > 85% at 550 nm. These films were used to make thin-film electroluminescent devices (TFELD) using two different insulator layers: lithium fluoride (LiF) or silica (SiO2). All the devices exhibit at least two wide emission bands in the visible range centered at 420 nm and at 380 nm attributed to the electronic defects in the ZnO optical band gap. Besides these two bands, the device using SiO2 and ZnO film obtained via sol-gel exhibits an additional band in the UV range centered at 350 nm which can be attributed to excitonic emission. These emission bands of ZnO can transfer their energy when a proper dopant is present. For the devices produced the voltage-current characteristics were measured in a specific range of applied voltage. (C) 2007 Elsevier B.V. All rights reserved.

Structural studies on TeO2-PbO glasses

Binary tellurite-based glasses in the TeO2-PbO system were prepared and its structure investigated by means of Raman Scattering and X-ray Absorption Spectroscopy. Both spectroscopies indicate strong modifications of the first coordination shell around tellurium atoms when the PbO content increases revealing for lead its glassy network modifier role. Also, Pb L-3-edge EXAFS measurements reveal this structural role played by lead atoms, but the presence of a medium range order contribution indicates that lead also participates to the glassy network formation. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

Effect of the addition of ZnO seeds on the electrical proprieties of ZnO-based varistors

ZnO has the characteristic of presenting an intermediate value for the effective 3 eV barrier at room temperature. ZnO ceramics are applied in high-voltage systems or circuits. Attempts were made to reduce the number of effective barriers in the system by adding large particles of ZnO to the varistor composition. This procedure reduced the breakdown field of the varistors by values up to 90% lower than those initially obtained, and produced nonlinear coefficients as low as 20. (C) 2003 Elsevier B.V. B.V. All rights reserved.

Blue cooperative luminescence properties in Yb3+ doped GeO2-PbO-Bi2O3 vitreous system for the production of thin films

Germanate glasses are of interest for optoelectronic applications because they combine high mechanical strength, high chemical durability and temperature stability with a large transmission window (400 to 4500 nm) and high refractive index (2.0). GeO2-PbO-Bi2O3 glasses doped with Y-b(3+) were fabricated by melting powders in a crucible and then pouring them in a brass mold. Energy Dispersive Spectroscopy showed that the glass composition has a high spatial uniformity and that the Yb concentration in the solid sample is proportional to the Yb concentration in the melt, what was confirmed by absorption measurements. Intense blue emission at 507 nm was observed, corresponding to half of the wavelength of the near infrared region (NIR) emission; besides, a decay lifetime of 0.25 ms was measured and this corresponds to half of the decay lifetime in the infrared region; these are very strong indications of the presence of blue cooperative luminescence. Larger targets have been produced to be sputtered, resulting in thin films for three dimensional (3D) display and waveguide applications. (c) 2006 Elsevier B.V. All rights reserved.

Importance of oxygen atmosphere to recover the ZnO-based varistors properties

A methodology to recover the non-ohmic properties of ZnO based varistors after degradation with long and short duration pulses was proposed in this work. The basic idea consists in submitt the degraded ceramics at different temperatures and oxygen flows. Thermal treatment at 900 degrees C for 2 h with oxygen flow of 15 l/h allowed to obtain better non-linear coefficient (alpha= 52.5) compared to the standard sample. Rietveld refinement showed that with the thermal treatment, the oxygen species and the beta-Bi2O3 phase, lost in the degradation process, are recovered in the grain boundary.

Influence of Ta2O5 on the electrical properties of ZnO- and CoO-doped SnO2 varistors

SnO2-based varistors doped with 0.5% cobalt, 0.5% zinc and various tantalum amounts were prepared by the solid-state route. Experimental evidence shows that small quantities of Ta2O5 improve the nonlinear properties of the samples significantly. It was found that samples doped with 0.05 mol% Ta2O5 exhibit the highest density (98.5%), the lowest electric breakdown field (E-b = 1050 V/cm) and the highest coefficient of nonlinearity (alpha = 11.5). The effect of Ta2O5 dopant could be explained by the substitution of Ta5+ by Sn4+. (C) 2004 Elsevier Ltd and Techna S.r.l. All rights reserved.

Nonlinear characteristics of Cr2O3, WO3, ZnO and CoO doped SnO2 varistors

SnO2 based ceramics doped with 1.0 mol% ZnO, 1.0 mol% CoO, 0.1 mol% WO3 and 0.05 mol% Cr2O3 show varistor behavior with nonlinear coefficient alpha = 33, breakdown electric field E-B = 12.5 kV/cm, leakage current I = 0.63 mA/cm(2) and average grain size of 1.52 mu m. Experimental evidence shows that the addition of Cr2O3 improves the nonlinear properties of the samples significantly, the impedance data, represented by means of Nyquist diagrams, show a dramatic increase in the resistivity for the samples doped with Cr2O3. (C) 2005 Elsevier B.V. All rights reserved.

Nanostructure and properties of ZnO films produced by the pyrosol process

Indium doped ZnO films were deposited by the pyrosol process on glass substrates at different temperatures from solutions containing In/Zn molar ratios up to 10%. The nanostructure of the films was investigated using grazing-incidence small angle X-ray scattering (GISAXS). The mass density was determined by X-ray reflectivity and the composition by X-ray photoelectron spectroscopy. The GISAXS measurements revealed an anisotropic pattern for films deposited at 573 and 623 K and a isotropic one for those deposited at higher temperatures. The anisotropic patterns indicate the presence of elongated nanopores with their long axes perpendicular to the film surface. In contrast, the isotropic nature of GISAXS patterns of films grown at high temperatures (673 and 723 K) suggests the presence of spherical voids. The pore size distribution function determined from the isotropic patterns indicates a multimodal size distribution. on the other hand, the measured mass density of the doped films with isotropic nanotexture is higher than that of the anisotropic films while the electric resistivity is significantly lower. This is in agreement with the detected strong reduction of the void density and specific surface area at approximately constant pore size.

Effect of PbO excess on the formation of lead magnesium niobate perovskite by the columbite method

The effect of lead excess on the pyrochlore-type formation in Pb(Mg1/3Nb2/3)O-3 (PMN) powders has been investigated. The polymeric precursor method was used in the synthesis of the columbite in association to the partial oxalate method to synthesize the PMN powder samples. Structure refinement of the columbite precursor and PMN powders was carried out using the Rietveld method. The quantitative phase analysis showed that the amount of perovskite phase is not affected by PbO excess, but a great excess drives the pyrochlore-type formation so that 3 wt.% of PbO causes the predominance of Mg-containing pyrochlore phase. Using the refined data obtained from the Rietveld refinement, the compositional fluctuation in the perovskite phase was calculated from Nb/Mg ratio values and Pb occupation factor. Mg inclusion occurs concomitant with Ph one into PMN perovskite phase and this effect is directed by PbO excess during powder synthesis. (C) 2003 Elsevier B.V. All rights reserved.