Structural and morphological characteristics of (Pb1-x Sr (x) )TiO3 powders obtained by polymeric precursor method

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Preparation of hierarchically structured porous aluminas by a dual soft template method

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Structural and spectroscopic characterization of Al2-xCrxO3 powders obtained by polymeric precursor method

Al2O3 and Al2-x Cr (x) O-3 (x = 0.01, 0.02 and 0.04) powders have been synthesized by the polymeric precursors method. A study of the structural evolution of crystalline phases corresponding to the obtained powders was accomplished through X-Ray Diffraction and UV-vis spectroscopy (reflectance spectra and CIEL* a*b* color data). The obtained results allow to identify the gamma-Al2O3 to alpha-Al2O3 phase transition. The single-phase alpha-Al2O3 powder was obtained after heat treatment at 1050 degrees C for 2 h. The results show that the green to red color transition and ruby luminescence lines observed for the powders of Al2-x Cr (x) O-3 are related to the gamma to alpha-Al2O3 phase transition and the temperature and time range for such transition depends on the chromium content.

Structural and optical properties of GdAlO3:RE3+ (RE = Eu or Tb) prepared by the Pechini method for application as X-ray phosphors

In this work, GdAlO3:RE3+ (RE = Eu or Tb) was successfully prepared by the Pechini method at lower temperatures when compared to others methods as solid-state synthesis and sol-gel process. In accordance to the XRD data, the fully crystalline single-phase GdAlO3 could be obtained at 900 degrees C. The differential thermal analysis (DTA) shows a crystallization peak at 850 degrees C. The samples are composed by monocrystalline particles (50-120 nm) exhibiting the formation of aggregates among them, which indicates the beginning of the sinterization process. This feature indicates a strong tendency to the formation of aggregates, which is a suitable ability for the close-packing of particles, and hence a potential application in X-ray intensifying screens. Luminescence measurements indicate Gd3+ -> RE3+ energy transfer. The Eu3+ emission spectra exhibit all the characteristics D-5(0) -> F-7(j) transitions and the observed profile suggests that RE3+ ions occupy at least one site without center of symmetry. For terbium-doped samples, the D-5(3) -> F-7(j) (blue emission) and D-5(4) -> F-7(j) (green emission) transitions were observed and the ratio between them may depend on the Tb3+ content due to cross-relaxation processes. (C) 2009 Elsevier B.V. All rights reserved.

Heterogeneous Fenton reactants: a study of the behavior of iron oxide nanoparticles obtained by the polymeric precursor method

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Nanometric Pb1-xLaxTiO3 (x=0, 0.13 and 0.27) powders obtained by the polymeric precursor method

PLT (Pb1-xLaxTiO3, in which x = 0, 0.13 and 0.27) powders were successfully synthesized using the polymeric precursor method, based on the Pechini method. The polymeric precursors were calcined at temperatures ranging from 350 to 500 degrees C for 4 h. X-ray diffraction (XRD) showed the evolution of the crystalline phase starting from the amorphous precursor. Thermogravimetric analyses (TG) and differential thermal analyses (DTA) of the powder precursors showed the influence of the pH on the elimination of organic material. PLT powders have a tendency to form agglomerates, what can be verified by comparing the values of the average particle sizes obtained by Brunauer-Emmett-Teller method, BET (D-BET) with the values of the average crystallite sizes obtained by XRD (D-XRD). (C) 2007 Elsevier Ltd. All fights reserved.

Structural and surface morphology characterizations of oriented LiNbO3 thin films grown by polymeric precursor method

Polymeric precursor solution was used to deposit LiNbO3 thin films by dip coating on sapphire substrates. The effects of processing variables, such as heat treatment conditions and number of deposited layers, on crystallinity and morphology of the final films were investigated. X-ray diffraction patterns show the oriented growth of the films. The rocking curves, obtained around the (006) LiNbO3 peak, revealed that the shape peak and the FWHM value were influenced by the processing variables. According to these parameters, some films presented very homogeneous dense and smooth surfaces, as shown by the SEM and AFM studies.

Influence of the preparation method and the support on H2O 2electrogeneration using cerium oxide nanoparticles

This work describes the influence of the preparation method and the carbon support using a low contentof cerium oxide nanoparticles (CeO2/C 4%) on H2O2electrogeneration via the oxygen reduction reac-tion (ORR). For this purpose, the polymeric precursor (PPM) and sol-gel (SGM) methods with Vulcan XC72R (V) and Printex L6 (P) supports were employed. The materials were characterized by X-ray diffrac-tion (XRD), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). TheXRD analysis identified two phases comprising CeO2and CeO 2-x. The smallest mean crystallite size wasexhibited for the 4% CeO2/C PPM P material, which was estimated using the Debye-Scherrer equation tobe 6 nm and 4 nm for the CeO2and the CeO 2-xphases, respectively, and was determined by TEM to be5.9 nm. XPS analysis was utilized to compare the oxygen content of the 4% CeO2/C PPM P to Printex L6.The electrochemical analysis was accomplished using a rotating ring-disk electrode. The results showedthat the 4% CeO2/C specimen, prepared by PPM and supported on Printex L6, was the best electrocatalystfor H2O2production in 1 mol L -1NaOH. This material showed the highest ring current, producing 88%H2O2and transferring 2.2 electrons per O 2molecule via the ORR at the lowest onset potential. Addition-ally, the ring-current of the 4% CeO2/C PPM P material was higher than that of Vulcan XC 72R and PrintexL6, the reference materials for H2O 2production, indicating the highest electrocatalytic activity for the 4%CeO2/C PPM P material. © 2013 Elsevier Ltd. All rights reserved.

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

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Biogenic modified silica as a sorbent of cadmium ions: Preparation and characterization

This work describes the preparation and characterization of biogenic modified silica from rice hull ash and its use as a sorbent of cadmium ions. Thus, an agro-industrial residue has been used to produce a new adsorbent product which is able to remove toxic elements. Mesoporous biogenic silica was obtained by alkaline extraction of sodium silicate by hydrolysis with the sol-gel process, and it was modified with salen using 1,2-dichloroethane as a spacer. The surface area of the silica was measured by nitrogen adsorption/desorption analysis. Surface modification was measured by Fourier transform infrared spectroscopy. The degree of functionalization was obtained by elemental analysis. This work showed that biogenic modified silica can be produced in aqueous media from rice hull ash using a simple method, providing an alternative method for adsorbent preparation. Thermogravimetric analysis showed that the salen-modified silica is stable up to 209 C. The modified silica displays appropriate structural characteristics for an adsorbent. The cylindrical pores, open at both ends, allow free diffusion of cadmium ions to the adsorption sites on the silica surface. The surface modification increases cadmium adsorption on the silica surface 100-fold. The salen-modified silica showed specific adsorption for Cd2+ of 44.52 mg/g SiO2 at cadmium concentration of 100 mg/l.

XAS characterization of the RuO(2)-Ta(2)O(5) system local (crystal) structure

The influence of the preparation method on the structural properties of the RuO(2)-Ta(2)O(5) system was investigated. Both thin films on Ti substrates and powder samples of nominal composition Ti/RuO(2)-Ta(2)O(5) (Ru:Ta = 100:0, 90:10, 80:20, 30:70, and 0:100 at.%) were prepared through thermal decomposition of polymeric precursors (DPP). The thin films and powder samples were investigated using X-ray absorption spectroscopy (XAS). XANES analyses showed that Ru and Ta are present in the Ru(IV) and Ta(V) oxidation states. EXAFS signals of all the samples were analyzed, to obtain the average bond length (r), coordination number, and the Debye-Waller factor (sigma(2)) for each Ru-O, Ru-Ru, Ta-O nearest-neighbor. The first shell Ru-O distance was found at 1.91-1.92 angstrom with coordination number of 1.8-2.1, and at 2.01-2.02 angstrom with coordination number of 3.9-4.1. The Ta-O distance obtained for all the samples and in both modes (transmission and fluorescence) had significantly different values from the theoretical ones. The results revealed that the local structure around both the Ru and Ta sites are similar, and that they consist of distorted M-O(6) octahedra (where M = Ru or Ta). (C) 2010 Elsevier B.V. All rights reserved.

Preparação de adsorventes mesoporosos para a adsorção de poluentes em águas

Mestrado Engenharia Química. Ramo Tecnologias de Protecção Ambiental

Printed electronics for ubiquitous computing applications

Dissertação para obtenção do Grau de Doutor em Química

Risk assessment in a research laboratory during sol–gel synthesis of nano-TiO2

The occupational risks in the nanotechnology research laboratories are an important topic since a great number of researchers are involved in this area. The risk assessment performed by both qualitative and quantitative methods is a necessary step for the management of the occupational risks. Risk assessment could be performed by qualitative methods that gather consensus in the scientific community. It is also possible to use quantitative methods, based in different technics and metrics, as indicative exposure limits are been settled by several institutions. While performing the risk assessment, the information on the materials used is very important and, if it is not updated, it could create a bias in the assessment results. The exposure to TiO2 nanoparticles risk was assessed in a research laboratory using a quantitative exposure method and qualitative risk assessment methods. It was found the results from direct-reading Condensation Particle Counter (CPC) equipment and the CB Nanotool seem to be related and aligned, while the results obtained from the use of the Stoffenmanager Nano seem to indicate a higher risk level.

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.