Physical characterization of K-doped 0.9PMN-0.1PT synthesized by an association of the columbite route and the polymeric precursor method

The solid solution 0.9PbMg 1/3Nb 2/3O 3-0.1PbTiO 3 is one of the most widely investigated relaxor ceramic, because of its high dielectric constant and low sintering temperatures. PMN-PT powders containing single perovskite phase were prepared by using a Timodified columbite precursor obtained by the polymeric precursor method. Such precursor reacts directly with stoichiometric amount of PbO to obtain pyrochlore-free PMN-PT powders. The structural effects of K additive included in the columbite precursor and 0.9PMN-0.1PT powders were also studied. The phase formation at each processing step was verified by XRD analysis, being these results used for the structural refinement by the Rietveld method. It was verified the addition of K in the columbite precursor promotes a slight increasing in the powder crystallinity. There was not a decrease in the amount of perovskite phase PMN-PT for 1mol% of K, and the particle and grain size were reduced, making this additive a powerful tool for grain size control.

Photoluminescence-structure relationships in ormosils for integrated optical devices

Planar waveguides with low losses in the infrared (from 0.6-1.1 dB/cm) were prepared with sol-gel derived poly(oxyethylene)/siloxane hybrid doped with zirconium(IV) n-propoxide (ZPO) and methacryloxypropyltrimethoxysilane (MAPTMS). The doped nanohybrids were characterized by small angle X-ray scattering, 29Si nuclear magnetic resonance and photoluminescence spectroscopy and compared with the undoped hybrid material. The results indicate an effective interaction between the zirconium particles and the siliceous nanodomains. © 2005 Materials Research Socicty.

Compositional influence on spectroscopic properties of Yb3+ doped tellurite glasses

Spectroscopic properties of ytterbium-doped tellurile glasses with different compositions are reported. Results of linear refractive index, absorption and emission spectra, and fluorescence lifetimes are presented. The studied samples present high refractive index (∼2.0) and large transmission window (380-6000nm). Absorption and emission cross-sections are calculated as well as the minimum pump laser intensity. The results are compared with the values of other laser materials, in order to investigate applications as laser media in the infrared region.

Energy transfer and frequency upconversion involving triads of Pr3+ ions in (Pr3+, Gd3+) doped fluoroindate glass

Blue and ultraviolet luminescence in (Pr3+, Gd3+) doped fluoroindate glass is studied for excitation in the red region (≈590 nm). Frequency upconversion (UC) is observed due to energy transfer (ET) among three Pr3+ ions initially excited to the D21 state corresponding to the ET process D21 + D21 + D21 → S01 + H53 + H53. Additionally, UC luminescence from states P 72 6 and I 72 6 of Gd3+ is observed for an excitation wavelength resonant with transitions of the Pr3+ ions. The characterization of the luminescence signals allowed to determine ET rate among the Pr3+ ions and provides evidence of interconfigurational ET between Gd3+ and Pr3+ ions. © 2006 American Institute of Physics.

Preparation of lanthanum doped Bi4Ti3O12 ceramics by the polymeric precursor method

Lanthanum-modified bismuth titanate, Bi4 - xLaxTi3O12 (BLT) ceramics, with x ranging from 0 to 0.75 were prepared by the polymeric precursor method. Orthorhombicity of the system is decreased with the increase of lanthanum content in the bismuth titanate (BIT) crystal lattice. No secondary phases were evident after lanthanum addition. Increasing lanthanum content causes a structural distortion in the bismuth titanate lattice. The shape of the grains is strongly influenced by the lanthanum added to the system. © 2005 Elsevier B.V. All rights reserved.

Determination of methyldopa in pharmaceutical formulations by combined spot test-diffuse reflectance spectroscopy

This paper describes a very simple and rapid quantitative reflectance spot test procedure for the determination of methyldopa in pharmaceutical formulations. This method is based on the complexation reaction of methyldopa with molybdate ions yielding a yellow stable complex on filter paper. Reflectance measurements were carried out at 410 nm. Under optimal conditions, the calibration graphs obtained for methyldopa by plotting the optical density of the reflectance signal (A R) vs. the log of the concentration were linear from 6.30 × 10 -3 to 1.89 × 10 -2 mol L -1, with a correlation coefficient of 0.998. The detection limit was 2.74 × 10 -3 mol L -1 (R.S.D. = 1.02%) for methyldopa. The common excipients used as additives in pharmaceuticals do not interfere in the proposed method. The method was applied to determine metyldopa in commercial pharmaceutical formulations. The results obtained by the proposed method compare favorably with those obtained by an official procedure at 95% confidence level. ©2006 Sociedade Brasileira de Química.

Magnetic resonance study of the crystallization behavior of InF3-based glasses doped with Cu2+, Mn2+ and Gd3+

The crystallization of fluoroindate glasses doped with Gd3+, Mn2+ and Cu2+ heat treated at different temperatures, ranging from the glass transition temperature (Tg) to the crystallization temperature (Tc), are investigated by electron paramagnetic resonance (EPR) and 19F nuclear magnetic resonance (NMR). The EPR spectra indicate that the Cu2+ ions in the glass are located in axially distorted octahedral sites. In the crystallized glass, the g-values agreed with those reported for Ba2ZnF6, which correspond to Cu2+ in a tetragonal compressed F- octahedron and to Cu2+ on interstitial sites with a square-planar F- co-ordination. The EPR spectra of the Mn2+ doped glasses exhibit a sextet structure due to the Mn2+ hyperfine interaction. These spectra suggest a highly ordered environment for the Mn2+ ions (close to octahedral symmetry) in the glass. The EPR spectra of the recrystallized sample exhibit resonances at the same position, suggesting that the Mn2+ ions are located in sites of highly symmetric crystalline field. The increase of the line intensity of the sextet and the decrease of the background line in the thermal treated samples suggest that the Mn2+ ions move to the highly ordered sites which contribute to the sextet structure. The EPR spectra of the Gd3+ doped glasses exhibit the typical U-spectrum of a s-state ion in a low symmetry site in disordered systems. The EPR of the crystallized glasses, in contrast, have shown a strong resonance in g ≈ 2.0, suggesting Gd3+ ions in environment close to cubic symmetry. The 19F NMR spin-lattice relaxation rates were also strongly influenced by the crystallization process that takes over in samples annealed above Tc. For the glass samples (doped or undoped) the 19F magnetization recoveries were found to be adjusted by an exponential function and the spin-lattice relaxation was characterized by a single relaxation time. In contrast, for the samples treated above Tc, the 19F magnetization-recovery becomes non-exponential. A remarkable feature of our results is that the changes in the Cu2+, Mn2+, Gd3+ EPR spectra and NMR relaxation, are always observed for the samples annealed above Tc. © 2006 Elsevier B.V. All rights reserved.

Effects in the population inversion of3H4 level in Tm, Tm-Tb and Tm-Eu doped germanate glasses for amplifiers applications

The population inversion of the Tm3+ in GLKZ glass involved in the 1470 nm emission (3H4 → 3F 4) as a function of Tb (or Eu) concentration was calculated by computational simulation for a CW laser pumping at 792 nm. These calculations were performed using the experimental Tm→Tb an Tm→Eu transfer rates and the spectroscopic parameters of the Tm (0.1 mol %) system. The result shows that 0.2 mol % (Tb3+) and 0.4 mol % of Eu3+ ions propitiate best population inversion of Tm3+ (0.1 mol %) maximizing the amplification coefficient of germanate (GLKZ) glass when operating as laser intensity amplification at 1470 nm. Besides the effective deactivation of the 3F4 level, the presence of Tb3+ or Eu 3+ ions introduce a depopulation of the 3H4 emitting level by means of a cross relaxation process with Tm3+ ions. In spite of this, the whole effect is verified to be benefic for using Tm-doped GLKZ glass codoped with Tb3+ or Eu3+ as a suitable material for confectioning optical amplifiers that operates in the S-band for telecommunication.

Sintering of cobalt and strontium doped lanthanum chromite obtained by combustion synthesis

Lanthanum chromite (LaCrO3) is one of the most adequate materials for use as interconnector in solid oxide fuel cell (SOFC) applications, due to its intrinsic properties, namely its good electrical conductivity and resistance to environment conditions in fuel cell operations. Due to difficulties in sintering, additives are usually added to help in the densification process. In this work, the influence of added cobalt and strontium, in the sintering of LaCrO3 obtained by combustion synthesis was studied. The starting materials were respectively nitrates of chromium, lanthanum, cobalt and strontium, and urea was used as fuel. The results show that by increasing the strontium and cobalt concentrations it is possible to reduce the temperature of sintering. Using both additives, the sintering processes took place in lesser times than normally used for this material, as well as greater values of density were attained.

Production of cellulolytic and hemicellulolytic enzymes from Aureobasidium pulluans on solid state fermentation

This article investigates a strain of the yeast Aureobasidium pullulans for cellulase and hemicellulase production in solid state fermentation. Among the substrates analyzed, the wheat bran culture presented the highest enzymatic production (1.05 U/mL endoglucanase, 1.3 U/mL β-glucosidase, and 5.0 U/mL xylanase). Avicelase activity was not detected. The optimum pH and temperature for xylanase, endoglucanase and β-glucosidase were 5.0 and 50, 4.5 and 60, 4.0 and 75°C, respectively. These enzymes remained stable between a wide range of pH. The β-glucosidase was the most thermostable enzyme, remaining 100% active when incubated at 75°C for 1 h. © 2007 Humana Press Inc.

Preparation and characterization of castor oil-based polyurethane/poly(o- methoxyaniline) blend film

Blends made up of castor oil-based polyurethane (PU) and poly(o-methoxyaniline) (POMA) were obtained in the form of films by casting and characterized by FTIR, UV-Vis-NIR spectroscopy, and electrical conductivity measurements. Doping was carried out by immersing the films in 1.0M HCl aqueous solution. Chemical bonds between NCO group of PU and NH group of POMA were observed by means of FTIR spectra. The UV-Vis-NIR spectra indicated that the presence of the PU in the blend does not affect doping and formation of the POMA phase. The electrical conductivity research was in the range of 10-3 S/cm. © 2007 Wiley Periodicals, Inc.

Effect of scandium on the structural and photocatalytic properties of titanium dioxide thin films

Pure and scandium doped-TiO2 thin films were prepared by the sol-gel process and coated by dip coating. The effects of scandium on the phase formation, optical properties and photoactivity of the TiO2 thin films were investigated. The lattice parameters and the crystallinity of the anatase phase, characterized by the Rietveld method, demonstrated that scandium doping affected the structural parameters and crystallinity of the films, modifying the absorption edge. A direct correlation was found between band gap energy and photodegradation efficiency, with lower values of band gap energy augmenting this efficiency. Moreover, a significant improvement in the catalyst's photodegradation efficiency was attained with a scandium concentration of 5.0 mol%. © 2007 Springer Science+Business Media, LLC.

α-SiAION: Development and machining test on gray cast iron

The α-SiAlON ceramic cutting tool insert is developed. Silicon nitride and additives powders are pressed and sintered in the form of cutting tool inserts at temperature of 1900 °C. The physics and mechanical properties of the inserts like green density, weight loss, relative density, hardness and fracture toughness are evaluated. Machining studies are conducted on grey cast iron workpiece to evaluate the performance of α-SiAlON ceramic cutting tool. In the paper the cutting tool used in higher speed showed an improvement in the tribological interaction between the cutting tools and the grey cast iron workpiece resulted in a significant reduction of flank wear and roughness, because of better accommodation and the presence of the graphite in gray cast iron. The above results are discussed in terms of their affect at machining parameters on gray cast iron.

The influence of the mixing time in the rheological behavior of cement pastes

Rheology has the purpose to study the flux and deformation of materials when submitted to some tension or outer mechanical solicitation. In practice, the effective scientific field broached by rheology is restricted only to the study of homogeneous fluids behavior, in which are included eminent liquids, particles suspensions, and emulsions. The viscosity (η) and the yield stress (τ 0) are the two basic values that define the fluids' behavior. The first one is the proportionality constant that relates the shear rate (γ) with the shear stress (τ) applied, while the second indicates the minimal tension for the flowage beginning. The fluids that obey the Newton's relation - Newtonians fluids - display the constant viscosity and the null yield stress. It's the case of diluted suspensions and grate amount of the pure liquids (water, acetone, alcohol, etc.) in which the viscosity is an intrinsic characteristic that depends on temperature and, in a less significant way, pressure. The suspension, titled Cement Paste, is defined as being a mixture of water and cement with, or without, a superplasticizer additive. The cement paste has a non-Newtonian fluid behavior (pseudoplastic), showing a viscosity that varies in accord to the applied shear stress and significant deformations are obtained from a delimited yield stress. In some cases, systems can also manifest the influence of chemical additives used to modify the interactions fluid/particles, besides the introduced modifications by the presence of incorporated air. To the cement paste the rheometric rehearsals were made using the rheometer R/S Brookfield that controls shear stress and shear rate in accord to the rheological model of Herschel-Bulkley that seems to better adapt to this kind of suspension's behavior. This paper shows the results of rheometrical rehearsals on the cement paste that were produced with cements HOLCIM MC-20 RS and CPV-ARI RS with the addition of superplasticizer additives based of napthaline and polycarboxilate, with and without a constant agitation of the mixture. The obtainment of dosages of superplasticizer additives, as well as the water/cement ratio, at the cement at the fluidify rate determination, was done in a total of 12 different mixtures. It's observed that the rheological parameters seem to vary according to the cement type, the superplasticizer type, and the methodology applied at the fluidity rate determination.

Influência da queima e aditivos químicos e bacterianos na composição química de silagens de cana-de-açúcar

The objective of this trial was to evaluate the effect of the chemical (urea, sodium benzoate, and sodium hydroxide) and microbiological (Propionibacterium acidipropionici + Lactobacillus plantarum, and Lactobacillus buchneri) additives on the sugarcane nutritive value, ensiled crude or after burned, using a factorial scheme 2 (burned or crude sugar cane) x 6 (five additives urea, sodium benzoate, sodium hydroxide, Propionibacterium acidipropionici + Lactobacillus plantarum, and Lactobacillus buchneri plus control). It was evaluated the sugar cane chemical composition, before and after ensilage. The sugar cane NDF contents increased (51.3%, before ensilage) to 67.8% after fermentation period. The highest true digestible dry matter recovery values, 83.6 and 79.8% were observed on the burned sugar cane silage treated with NaOH or L. buchneri, respectively. The NaOH, and L. buchneri showed more efficiency in reducing nutritive looses during the fermentation phase of the crude or burned sugar cane silage.