The Fabrication and Characterization of a Nickel Nanoparticle Modified Boron Doped Diamond Electrode for Electrocatalysis of Primary Alcohol Oxidation

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

External polyacrylate-coating as alternative material for preparation of photopolymerized sol-gel monolithic column

Photopolymerized sol-gel monolithic columns for use in capillary electrochromatography were prepared in 125 mu m i.d. polyacrylate-coated fused-silica capillaries. The polyacrylate-coating, unlike the polyimide one, is transparent to the radiation used (approximate to 370 nm), and thus, no coating removal is necessary. This is a very important particularity since intrinsic capillary column characteristics, such as flexibility and mechanical resistance, are unchanged. A mixture containing metacryloxypropyltrimethoxysilane (MPTMS) as the polymeric precursor, hydrochloric acid as the catalyst, toluene as the porogen and bis(2,4,6-trimethylbenzoyl)-phenylphosphine oxide (Irgacure 819) as the photoinitiator was irradiated at 370 nm for 20 min inside the capillaries to prepare the columns through sol-gel approach. The versatility and viability of the use of polyacrilate as a new capillary external coating were shown through preparation of two columns under different conditions, which were tested in electrochromatography for separation of standard mixture containing thiourea (marker compound), propylbenzene, phenanthrene and pyrene. (C) 2008 Elsevier B.V. All rights reserved.

Waveguides and gratings fabrication in zirconium-based organic/inorganic hybrids

Sol-gel derived poly(oxyethylene)/siloxane organic/inorganic di-ureasil hybrids containing different amounts of methacrylic acid (McOH, CH(2)=C(CH(3))COOH)) modified zirconium oxo-clusters (Zr-OMc) were processed as thin films deposited in glassy substrates via spin coating and as transparent and shape controlled monoliths. Channel monomode waveguides and diffraction gratings were UV patterned using the Talbot interferometer and the Lloyd mirror interferometer experimental setups. The time dependence of the diffraction gratings efficiency was studied for hybrids containing different amounts of Zr-OMc. Finally, the number of propagating modes and the refractive index gradient within the waveguide region, determined as a Gaussian section located below the patterned channel, was evaluated and modeled, a maximum index contrast of 2.43 X 10(-5) being estimated.

Optimization of photo-polymerized sol gel monolithic stationary phases prepared in polyacrylate-coated fused-silica capillaries for capillary electrochromatography

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Synthesis of SnO2 nanoparticles and their use in the fabrication of varistors

SnO2 nanoparticles doped with TiO2, CoO, Nb2O3 and Al2O3 were obtained in this work using the methods of coprecipitation and polymeric precursor. X Ray Diffraction (XRD), and Scanning Electron Microscopy (SEM) were used to characterize the ceramic powders obtained. Their synterization capacity was determined by dilatometric studies. Sinterized samples of the system on study were also characterized electrically and microstructurally to determine their suitability as varistors.

Fabrication and analysis of self-assembled photonic crystals structures

This paper presents the fabrication and analysis of a three-dimensional FCC photonic crystal (PhC) based on a self-assembly synthesis of monodispersive latex spheres. Experimental optical characterization, achieved by measurements of the specular reflectance under variable angles, indicated the clear presence of a Bragg diffraction pattern. Results are further explored by theoretical calculations based on the Finite Difference Time Domain (FDTD) method to determine the full PhC band structure.

Er3+/Yb3+ co-activated silica-alumina monolithic xerogels

Monolithic silica xerogels doped with different concentrations of Er3+, Yb3+ and Al3+ were prepared by sol-gel route. Densification was achieved by thermal treatment in air at 950degreesC for 120 h with a heating rate of 0.1degreesC/min. We studied the luminescence properties of the I-4(13/2)-->I-4(15/2) emission band of Er3+ as a function of the Al/Er/Yb concentration and we paid particular attention to the alumina effects. Raman spectroscopy and Vis-NIR absorption were used to monitor the degree of densification of the glasses and the residual OH content.

Lignin from sugar cane bagasse: Extraction, fabrication of nanostructured films, and application

Four lignin samples were extracted from sugar cane bagasse using four different alcohols (methanol, ethanol, n-propanol, and 1-butanol) via the organosolv-CO2 supercritical pulping process. Langmuir films were characterized by surface pressure vs mean molecular area (Pi-A) isotherms to exploit information at the molecular level carrying out stability tests, cycles of compression/expansion (hysteresis), subphase temperature variations, and metallic ions dissolved into the water subphase at different concentrations. Briefly, it was observed that these lignins are relatively stable on the water surface when compared to those obtained via different extraction processes. Besides, the Pi-A isotherms are shifted to smaller molecular areas at higher subphase temperatures and to larger molecular areas when the metallic ions are dissolved into the subphase. The results are related to the formation of stable aggregates (domains) onto the water subphase by these lignins, as shown in the Pi-A isotherms. It was found as well that the most stable lignin monolayer onto the water subphase is that extracted with 1-butanol. Homogeneous Langmuir-Blodgett (LB) films of this lignin could be produced as confirmed by UV-vis absorption spectroscopy and the cumulative transfer parameter. In addition, FTIR analysis showed that this lignin LB film is structured in a way that the phenyl groups are organized preferentially parallel to the substrate surface. Further, these LB films were deposited onto gold interdigitated electrodes and ITO and applied in studies involving the detection of Cd+2 ions in aqueous solutions at low concentration levels throughimpedance spectroscopy and electrochemical measurements. FTIR spectroscopy was carried out before and after soaking the thin films into Cd+2 aqueous solutions, revealing a possible physical interaction between the lignin phenyl groups and the heavy metal ions. The importance of using nanostructured systems is demonstrated as well by comparing both LB and cast films.

Fabrication and testing of a poly(vinylidene fluoride) (PVDF) microvalve for gas flow control

A microactuator made from poly(vinylidene fluoride) (PVDF), a piezoelectric polymer, was fabricated to control the gas flow rate through a glass micronozzle. The actuator was formed by gluing together two PVDF sheets with opposite polarization directions. The sheets were covered with thin conducting films on one side, that were then used as electrodes to apply an electric field to move the valve. The actuator has a rectangular shape, 3 mm x 6 mm. The device was incorporated with a micronozzle fabricated by a powder blasting technique. Upon applying a DC voltage across the actuator electrodes, one sheet expands while the other contracts, generating an opening motion. A voltage of +300 V DC was used to open the device by moving the actuator 30 mu m, and a voltage of -200 V DC was used to close the device by moving the actuator 20 mu m lower than the relaxed position. Flow measurements were performed in a low-pressure vacuum system, maintaining the microvalve inlet pressure constant at 266 Pa. Tests carried out with the actuator in the open position and with a pressure ratio (inlet pressure divided by outlet pressure) of 0.5, indicated a flow rate of 0.36 sccm. In the closed position, and with a pressure ratio of 0.2, a flow rate of 0.32 sccm was measured.

Isothermal structural evolution of SnO2 monolithic porous xerogels

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Effect of denture fabrication and wear on closest speaking space and interocclusal distance during deglutition

Statement of problem. The accuracy of assessing maxillomandibular relationships for trial bases and dentures using phonetic and swallowing methods has not been compared to that observed with definitive prostheses. Thus, there is no evidence to prove whether measurements obtained through such methods remain the same after adaptation to dentures.Purpose. This study investigated changes in the closest speaking space, interocclusal rest space, and interocclusal distance during deglutition in edentulous patients during and after complete denture treatment.Material and methods. Eighteen edentulous subjects participated in this study and measurements were performed after 7 Intervals of time: (1) with occlusion rims and record bases following creation of the maxillomandibular relationship record, (2) with trial dentures, (3) at Insertion of definitive complete dentures, (4) 1 week, (5) 2 weeks, (6) 1 month, and (7) 3 months after insertion. Recordings of interocclusal distances were made with a mandibular kinesiograph. Closest speaking space was measured during the pronunciation of the word 'seis'. The distance between postural rest position and centric occlusion, or interocclusal rest space, was measured using a kinesiograph. Interocclusal distance during deglutition was tested by recording the closest mandibular position recorded during swallowing of 20 mL of water. Data were analyzed using repeated-measure ANOVA, followed by the Student-Newman-Keuls test (alpha=.05).Results. A significant (P <.01)reduction in the mean closest speaking space was found when it was evaluated using occlusion rims and record bases (4.6 mm) compared with other stages (3.0 to 3.4 mm). No significant differences were found in mean interocclusal rest space and interocclusal distance during deglutition among the time periods evaluated.Conclusions. The presence of occlusion rims can influence mandibular position during pronunciation of the /s/ sound. The arrangement of artificial teeth changes the closest speaking space. However, rest position and deglutition were not affected, either during denture fabrication or short-term use.

Fabrication of novel light-emitting devices based on green-phosphor/conductive-polymer composites

We report on light-emitting devices based on a green-phosphor compound (Mn-doped zinc silicate, Zn2SiO4: Mn) dispersed in a conductive polymeric blend (poly-o-methoxyaniline/polyvinylene fluoride, POMA/PVDF-TrFE). The devices exhibited high luminance in the green, good stability and homogeneous brilliance over effective areas up to 5 cm(2). The electroluminescence (EL) spectrum presented essentially the same characteristics as the photoluminescence (PL) and cathodoluminescence spectra, indicating that the light emission originates from decay of the same excited species, regardless of the excitation source. Operating characteristics were analyzed with current density - voltage (J - V) and luminance voltage ( L - V) curves to investigate the nature of the electroluminescence of the active material, which is still not completely understood.

Fabrication of phytic acid sensor based on mixed phytase-lipid Langmuir-Blodgett films

This paper reports the surface activity of phytase at the air-water interface, its interaction with lipid monolayers, and the construction of a new phytic acid biosensor on the basis of the Langmuir-Blodgett (LB) technique. Phytase was inserted in the subphase solution of dipalmitoylphosphatidylglycerol (DPPG) Langmuir monolayers, and its incorporation to the air-water interface was monitored with surface pressure measurements. Phytase was able to incorporate into DPPG monolayers even at high surface pressures, ca. 30 mN/m, under controlled ionic strength, pH, and temperature. Mixed Langmuir monolayers of phytase and DPPG were characterized by surface pressure-area and surface potential-area isotherms, and the presence of the enzyme provided an expansion in the monolayers ( when compared to the pure lipid at the interface). The enzyme incorporation also led to significant changes in the equilibrium surface compressibility (in-plane elasticity), especially in liquid-expanded and liquid-condensed regions. The dynamic surface elasticity for phytase-containing interfaces was investigated using harmonic oscillation and axisymmetric drop shape analysis. The insertion of the enzyme at DPPG monolayers caused an increase in the dynamic surface elasticity at 30 mN m(-1), indicating a strong interaction between the enzyme and lipid molecules at a high-surface packing. Langmuir-Blodgett (LB) films containing 35 layers of mixed phytase-DPPG were characterized by ultraviolet-visible and fluorescence spectroscopy and crystal quartz microbalance nanogravimetry. The ability in detecting phytic acid was studied with voltammetric measurements.

Hydrodynamic aspects of the amorphous alloy ribbon fabrication

Conditions for as-quenched amorphous ribbon fabrication by a single roll-casting method are analyzed from a hydrodynamic standpoint. The analysis is based on the investigation of the processing conditions for Fe 4 0Ni 40P 14B 6 amorphous ribbons. It is shown that the dependence of ribbon thickness on the ejection pressure for different roll angular velocities and different dimensions of crucible and orifice can be obtained from general considerations on the melt flow regime.

SnO2:Eu nanocrystallites in SnO2 monolithic xerogels

By simple room temperature broad band time-resolved spectroscopy it was possible to discriminate different Eu3+ spectra in SnO2 monolithic gels obtained by a sol-gel synthetic route. Nanocrystalline domains of the cassiterite-like SnO2:Eu could be easily identified in the transparent medium. From X-ray diffraction profiles a mean particle radius of 2.2 nm was estimated. © 1992.