Comparación entre MgAl2O4 sintetizado por medio de sol-gel contra otros métodos

Este trabajo presenta los resultados de una comparación entre una espinela (MgAl2O4) obtenida mediante sol-gel contra otros procesos reportados, tales como el horno eléctrico de arco, la reacción en estado sólido y las microondas.

The creation and evaluation of novel canine training aids for cocaine using molecularly encapsulated sol-gel polymers and an investigation of canine field accuracy

Biological detectors, such as canines, are valuable tools used for the rapid identification of illicit materials. However, recent increased scrutiny over the reliability, field accuracy, and the capabilities of each detection canine is currently being evaluated in the legal system. For example, the Supreme Court case, State of Florida v. Harris, discussed the need for continuous monitoring of canine abilities, thresholds, and search capabilities. As a result, the fallibility of canines for detection was brought to light, as well as a need for further research and understanding of canine detection. This study is two-fold, as it looks to not only create new training aids for canines that can be manipulated for dissipation control, but also investigates canine field accuracy to objects with similar odors to illicit materials. ^ It was the goal of this research to improve upon current canine training aid mimics. Sol-gel polymer training aids, imprinted with the active odor of cocaine, were developed. This novel training aid improved upon the longevity of currently existing training aids, while also provided a way to manipulate the polymer network to alter the dissipation rate of the imprinted active odors. The manipulation of the polymer network could allow handlers to control the abundance of odors presented to their canines, familiarizing themselves to their canine’s capabilities and thresholds, thereby increasing the canines’ strength in court.^ The field accuracy of detection canines was recently called into question during the Supreme Court case, State of Florida v. Jardines, where it was argued that if cocaine’s active odor, methyl benzoate, was found to be produced by the popular landscaping flower, snapdragons, canines will false alert to said flowers. Therefore, snapdragon flowers were grown and tested both in the laboratory and in the field to determine the odors produced by snapdragon flowers; the persistence of these odors once flowers have been cut; and whether detection canines will alert to both growing and cut flowers during a blind search scenario. Results revealed that although methyl benzoate is produced by snapdragon flowers, certified narcotics detection canines can distinguish cocaine’s odor profile from that of snapdragon flowers and will not alert.^

On the Synthesis and Multifunctional Properties of some Nanocrystalline Spinel Ferrites and Magnetic Nanocomposites

This thesis lays importance in the preparation and characterization of a few selected representatives of the ferrite family in the nanoregime. The candidates being manganese zinc ferrite and cobalt ferrite prepared by coprecipitation and sol-gel combustion techniques respectively. The thesis not only stresses importance on the preparation techniques and optimization of the reaction conditions, but emphasizes in investigating the various properties namely structural, magnetic and electrical. Passivated nickel nanocomposites are synthesized using polystyrene beads and adopting a novel route of ion exchange reduction. The structural and magnetic properties of these magnetic nanocomposites are correlated. The magnetocaloric effect (MCE) exhibited by these materials are also investigated with a view to finding out the potential of these materials as magnetic refrigerants. Calculations using numerical methods are employed to evaluate the entropy change on selected samples.

Photoluminescence behavior of Eu(3+) ion doped into gamma- and alpha-alumina systems prepared by combustion, ceramic and Pechini methods

Al(2)O(3):Eu(3+)(1%) samples were prepared by combustion, ceramic, and Pechini methods annealed from 400 to 1400 degrees C. XRD patterns indicate that samples heated up to 1000 degrees C present disordered character of activated alumina (gamma-Al(2)O(3)). However, alpha-Al(2)O(3) phase showed high crystallinity and thermostability at 1200-1400 degrees C. The sample characterizations were also carried out by means of infrared spectroscopy (IR), scanning electron microscopy (SEM) and specific surface areas analysis (BET method). Excitation spectra of Al(2)O(3):Eu(3+) samples present broaden bands attributed to defects of Al(2)O(3) matrices and to LMCT state of O -> Eu(3+), however, the narrow bands are assigned to (7)F(0) -> (5)D(J),(5)H(J) and (5)L(J) transitions of Eu(3+) ion. Emission spectra of samples calcined up to 1000 degrees C show broaden bands for (5)D(0) -> (7)F(J) transitions of Eu(3+) ion suggesting that the rare earth ion is in different symmetry sites showed by inhomogeneous line broadening of bands, confirming the predominance of the gamma-alumina phase. For all samples heated from 1200 to 1400 degrees C the spectra exhibit narrow (5)D(0) -> (7)F(J) transitions of Eu(3+) ion indicating the conversion of gamma to alpha-Al(2)O(3) phases, a high intensity narrow peak around 695 nm assigned to R lines of Cr(3+) ion is shown. Al(2)O(3):Eu(3+) heated up to 1100 degrees C presents an increase in the Omega(2) intensity parameter with the increase of temperatures enhancing the covalent character of metal-donor interaction. The disordered structural systems present the highest values of emission quantum efficiencies (eta). CIE coordinates of Al(2)O(3):Eu(3+) are also discussed. (C) 2007 Elsevier Inc. All rights reserved.

Preparação de espuma cerâmica à base de zircônia pelo processo sol-emulsão-gel

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Preparação de espumas cerâmicas de 'TIO IND. 2' a partir do processo sol-emulsão-gel

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Characterization of pore structure and coordination of titanium in TiO2 and SiO2-TiO2 sol-pillared clays

Titania sol-pillared clay (TiO2 PILC) and silica-titania sol-pillared clay (SiO2-TiO2 PILC) were synthesized by the sol-gel method. Supercritical drying (SCD) and treatment with quaternary ammonium surfactants were used to tailor the pore structure of the resulting clay. It was found that SCD approach increased the external surface area of the PILCs dramatically and that treatment with surfactants could be used to tailor pore size because the mesopore formation in the galleries between the clay layers follows the templating mechanism as observed in the synthesis of MCM-41 materials. Highly mesoporous solids were thus obtained. In calcined TiO2 PILC, ultrafine crystallites in anatase phase, which are active for photocatalytic oxidation of organics, were observed. In SiO2-TiO2 PILCs and their derivatives, titanium was highly dispersed in the matrix of silica and no crystal phase was observed. The highly dispersed titanium sites are good catalytic centers for selective oxidation of organic compounds. (C) 2001 Academic Press.

Organic-inorganic hybrid sol-gelcoatings for metal corrosion protection: a review of recent progress

This paper is a review of the most recent and relevant achievements (from 2001 to 2013) on the development of organic–inorganic hybrid (OIH) coatings produced by sol–gel-derivedmethods to improve resistance to oxidation/corrosion of different metallic substrates and their alloys. This review is focused on the research of OIH coatings based on siloxanes using the sol–gel process conducted at an academic level and aims to summarize the materials developed and identify perspectives for further research. The fundamentals of sol–gel are described, including OIH classification, the interaction with the substrate, their advantages, and limitations. The main precursors used in the synthesis ofOIHsol–gel coatings for corrosion protection are also discussed, according to the metallic substrate used. Finally, a multilayer system to improve the resistance to corrosion is proposed, based on OIH coatings produced by the sol–gel process, and the future research challenges are debated.

Production of silica gel from residual rice husk ash

This paper presents a study on the production of silica gel in hydrothermal process using residual rice husk ash. Measurements of the chemical composition, X-ray diffraction, infrared spectroscopy, particle size distribution, and pozzolanic activity were carried out in order to characterize the obtained material, and the optimal silica gel was selected for use as a mineral additive in cement pastes. The compressive strengths were determined for cement pastes containing silica gel (0.0, 2.5 or 5% by mass) in different times. The results indicate that the mixtures containing silica gel showed improved mechanical behavior over all time periods evaluated.

Formulation and characterization of poloxamer 407®: thermoreversible gel containing polymeric microparticles and hyaluronic acid

The influence of the composition and preparation method on the sol-gel transition temperature (Tsol-gel) and rheological response of poloxamer-based formulations was determined. Manual and more complex mechanical stirring were found to provide similar results. In addition, a linear dependence of Tsol-gel on the poloxamer content was observed in the range of concentrations analyzed, and a Poloxamer 407® concentration of 18% was selected. The addition of hyaluronic acid did not lead to significant changes in the Tsol-gel values. In contrast, the addition of microparticles caused a reduction in Tsol-gel without a significant reduction in gel strength, and pseudoplastic characteristics were observed, indicating that a thermoreversible gel was obtained with a rheology suitable for application in the treatment of burn wounds.

NIR-Vis Up-Conversion Luminescence in the Yb3+,Er3+ Doped Y2O2S, ZrO2, and NaYF4 Nanomaterials

Since the discovery of the up-conversion phenomenon, there has been an ever increasing interest in up-converting phosphors in which the absorption of two or more low energy photons is followed by emission of a higher energy photon. Most up-conversion luminescence materials operate by using a combination of a trivalent rare earth (lanthanide) sensitizer (e.g. Yb or Er) and an activator (e.g. Er, Ho, Tm or Pr) ion in a crystal lattice. Up-converting phosphors have a variety of potential applications as lasers and displays as well as inks for security printing (e.g. bank notes and bonds). One of the most sophisticated applications of lanthanide up-conversion luminescence is probably in medical diagnostics. However, there are some major problems in the use of photoluminescence based on the direct UV excitation in immunoassays. Human blood absorbs strongly UV radiation as well as the emission of the phosphor in the visible. A promising way to overcome the problems arising from the blood absorption is to use a long wavelength excitation and benefit from the up-conversion luminescence. Since there is practically no absorption by the whole-blood in the near IR region, it has no capability for up-conversion in the excitation wavelength region of the conventional up-converting phosphor based on the Yb3+ (sensitizer) and Er3+ (activator) combination. The aim of this work was to prepare nanocrystalline materials with high red (and green) up-conversion luminescence efficiency for use in quantitative whole-blood immunoassays. For coupling to biological compounds, nanometer-sized (crystallite size below 50 nm) up-converting phosphor particles are required. The nanocrystalline ZrO2:Yb3+,Er3+, Y2O2S:Yb3+,Er3+, NaYF4:Yb3+,Er3+ and NaRF4-NaR’F4 (R: Y, Yb, Er) materials, prepared with the combustion, sol-gel, flux, co-precipitation and solvothermal synthesis, were studied using the thermal analysis, FT-IR spectroscopy, transmission electron microscopy, EDX spectroscopy, XANES/EXAFS measurements, absorption spectroscopy, X-ray powder diffraction, as well as up-conversion and thermoluminescence spectroscopies. The effect of the impurities of the phosphors, crystallite size, as well as the crystal structure on the up-conversion luminescence intensity was analyzed. Finally, a new phenomenon, persistent up-conversion luminescence was introduced and discussed. For efficient use in bioassays, more work is needed to yield nanomaterials with smaller and more uniform crystallite sizes. Surface modifications need to be studied to improve the dispersion in water. On the other hand, further work must be carried out to optimize the persistent up-conversion luminescence of the nanomaterials to allow for their use as efficient immunoassay nanomaterials combining the advantages of both up-conversion and persistent luminescence.

Magnetic resonance study of a vanadium pentoxide gel

In this work we report results from continuous-wave (CW) and pulsed electron paramagnetic resonance (EPR) and proton nuclear magnetic resonance (NMR) studies of the vanadium pentoxide xerogel V2O5:nH(2)O (n approximate to 1.6). The low temperature CW-EPR spectrum shows hyperfine structure due to coupling of unpaired V4+ electron with the vanadium nucleus. The analysis of the spin Hamiltonian parameters suggests that the V4+ ions are located in tetragonally distorted octahedral sites. The transition temperature from the rigid-lattice low-temperature regime to the high temperature liquid-like regime was determined from the analysis of the temperature dependence of the hyperfine splitting and the V4+ motional correlation time. The Electron Spin Echo Envelope Modulation (ESEEM) data shows the signals resulting from the interaction of H-1 nuclei with V4+ ions. The modulation effect was observed only for field values in the center of the EPR absorption spectrum corresponding to the single crystals orientated perpendicular to the magnetic field direction. At least three protons are identified in the xerogel by our magnetic resonance experiments: (I) the OH groups in the equatorial plane, (ii) the bound water molecules in the axial V=O bond and (iii) the free mobile water molecules between the oxide layers. Proton NMR lineshapes and spin-lattice relaxation times were measured in the temperature range between 150 K and 323 K. Our analysis indicates that only a fraction of the xerogel protons contribute to the measured conductivity.

Síntese e caracterização de óxidos de cério e cobalto obtidos por gel-combustão e Pechini aplicados às reações de oxidação de n-hexano

Oxide type spinel AB2O4 presents structure adjusted for application in the automobile industry. The spinel of cobalt has many practical applications had its excellent physical and chemical properties such as catalyst in hydrocarbon oxidation reaction. The CeO2 has been used in many of these processes because it assigns to a material with excellent thermal resistance and mechanics, high capacity of oxygen stockage (OSC) among others properties. This work deals with the synthesis, characterization and catalytic application of spinel of cobalt and CeO2 with fluorita structure, obtained for method of Pechini and method of Gel-Combustion. The process of Pechini, the puff was obtained at 300 ºC for 2 h in air. In the process of Gel-Combustion the approximately at 350 ºC material was prepared and burnt for Pyrolysis, both had been calcined at 500 ºC, 700 ºC, 900 ºC and 1050 ºC for 2 h in air. The materials of the calcinations had been characterized by TG/DTA, electronic microscopy of sweepings (MEV), spectroscopy of absorption in the infra-red ray (FTIR) and diffraction of X-rays (DRX). The obtained material reaches the phase oxide at 450 oC for Pechini method and 500 °C for combustion method. The samples were submitted catalytic reaction of n-hexane on superficies of materials. The reactor function in molar ration of 0, 85 mol.h-1.g-1 and temperature of system was 450 °C. The sample obtained for Pechini and support in alumine of superficial area of 178,63 m2.g-1 calcined at 700 ºC, give results of catalytic conversions of 39 % and the sample obtained for method of gel-combustion and support in alumina of 150 mesh calcined at 500 ºC result 13 % of conversion. Both method were selective specie C1

Utilização de sílica gel organofuncionalizada para adsorção de íons metálicos em solução aquosa

In this work the organosilanes aminopropyltriethoxysilane, 3-mercaptopropyltryethoxisilane and n[-3-(trimetoxisilyl)propyl]ethylenetriamine, as well as tetraethylortosilicate (TEOS), were employed to produce, by sol-gel method, organofuncionalized silicon samples. The prepared samples were characterized by elementar analys by thermogravimetry and infrared spectroscopy. Those samples were employed to adsorb Cd2+, Pb2+, Ni2+ and Zn2+ from aqueous solutions (10, 20, 40, 60 and 80 mg L-1). In typical experiments, 50 mg of the organometrix was suspended in 20 mL of metal cation solutions at four different contact times: 30, 60, 90 and 120 minutes. The total amount of adsorbed cations were measured by atomic absorption spectrometry. To all investigated matrices, the following adsorption capacity was observed: Ni2+ > Zn2+ > Cd2+ > Pb2+. Such sequence is closely related with the cation radius, as well as the cation hardness

Síntese e Caracterização de Titanatos de Cobalto e Níquel, dopados com Praseodímio, obtidos a partir da decomposição de Nitrilotriacetatos

In recent years, studies about the physicochemical properties of mixed oxides, call attention of the scientific community, properties like as piezoelectricity, photoluminescence, or applications as catalysts, arise in these compounds, when their chemical compositions are modified, in this context some routes are employed in the synthesis of these materials, among which can be cited these methods: ceramic, combustion, co-precipitation, Pechini or polymeric precursor method, hydrothermal, sol-gel; these routes are divided into traditional routes or chemical routes. In this work were synthesized oxides with variable composition, from the thermal decomposition of titanium, cobalt, nickel and praseodymium nitrilotriacetates. The nitrilotriacetates were characterized by IR Spectroscopy (FTIR), Thermogravimetric (TG/ DTG) and Differential Scanning Calorimetry (DSC), while oxides have been characterized by X-ray diffraction (XRD), Spectrofluorimetry and IR Spectroscopy (FTIR). From FTIR data, it was demonstrated that the displacement of the band corresponding to the carboxylate group (νCOOH) at 1712 cm-1, present in nitrilotriacetic acid (H3NTA), for 1680-1545 cm-1, these stretches are characteristics of coordinated nitrilotriacetates, By thermal analysis (TG/DTG /DSC), it was suggested, that in an oxidizing atmosphere (air) oxides are obtained at lower temperatures than in an inert atmosphere N2(g). By results from X-ray Diffraction (XRD), it was determinated that the oxides are crystalline and the predominant phases obtained are summarized titanate phases rutile and ilmenite. By fluorimetry was observed that the intensity of emission bands are directly proportional to the concentration of ions Ni2+, Co2+ and Pr3+, and IR spectroscopy (FTIR) from oxides, demonstrated the disappearance of characteristic bands by nitrilotriacetates, determining the complete decomposition of the nitrilotriacetates in oxides