Scanning tunneling microscope operating as a spin diode

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Caracterização dos eletrocatalisadores LaMnO3, LaFeO3, LaFe0,2Mn0,8O3 E La0,5Fe0,5MnO3 preparados por autocombustão assistida por microondas para cátodos de células a combustível do tipo SOFC

Materials consisting of perovskite-type oxides (ABO3) have been developed in this work for applications in fuel cell cathodes of solid oxide type (SOFC). These ceramic materials are widely studied for this type of application because they have excellent electrical properties, conductivity and electrocatalytic. The oxides LaMnO3, LaFeO3, LaFe0.2Mn0.8O3 e La0.5Fe0.5MnO3 were synthesized by the method of microwave assisted combustion and after sintering at 800°C in order to obtain the desired phases. The powders were characterized by thermogravimetry (TG), X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM) and voltammetric analysis (cyclic voltammetry and polarization curves). The results obtained by XRF technique showed that the microwave synthesis method was effective in obtaining doping oxides with values near stoichiometric. In general, powders were obtained with particle size less than 0.5 μm, having a porous structure and uniform particle size distribution. The particles showed spherical form, irregular and crowded of varying sizes, according to the analysis of SEM. The behavior of the oxides opposite the thermal stability was monitored by thermogravimetric curves (TG), which showed low weight loss values for all samples, especially those of manganese had its structure. By means of Xray diffraction of the samples sintered at 800°C was possible to observe the formation of powders having high levels of crystallinity. Furthermore, undesirable phases such as La2O3 and MnOx were not identified in the diffractograms. These phases block the transport of oxygen ions in the electrode/electrolyte interface, affecting the electrochemical activity of the system. The voltammetric analysis of the electrocatalysts LF-800, LM-800, LF2M8-800 e L5F5M-800 revealed that these materials are excellent electrical conductors, because it increased the passage of electrical current of the working electrode significantly. Best performance for the oxygen reduction reaction was observed with iron-rich structures, considering that the materials obtained have characteristics suitable for use in fuel cell cathodes of solid oxide type

Síntese, caracterização e estudo das propriedades magnéticas de ortoferritas de lantânio dopadas com manganês

Orthoferrites AFeO3 (A = rare earth) are an important class of perovskite oxides that exhibit weak ferromagnetism. These materials find numerous applications as chemical sensors, cathodes for fuel cells and catalysis, which make them interesting from the standpoint of science and technology. Their structural, electrical and magnetic properties are dependent on many factors such as the preparation method, heat treatment conditions, chemical composition and replacement of cations in sites A and/or B. In this paper, LaFe1-xMnxO3 (0 ≤ x ≤ 1) orthoferrites-type was prepared by Pechini method and Microwave-assisted combustion reaction in order to evaluate the influence of synthesis route on the formation of oxide, as well as the effect of parcial replacement of iron by manganese and heat treatment on the magnetic properties. The precursor powders were calcined at 700°C, 900°C, 1100°C and 1300°C for 4 hours and they were characterized by the techniques: Thermogravimetric analysis (TGA), X ray diffraction (XRD), Refinement by Rietveld method, Scanning electron microscopy (SEM), Reduction temperature programmed (RTP) and Magnetic hysteresis measurements performed at room temperature. According to the XRD patterns, the formation of perovskite phase with orthorhombic structure was observed for the systems where 0 ≤ x ≤ 0.5 and rhombohedral for x = 1. The results also showed a decrease of lattice parameters with the parcial replacement of iron by manganese and consequently a reduction in cell volume. The hysteresis curves exhibited weak ferromagnetism for the systems prepared by both synthesis methods. However, a dependence of magnetization as a function of dopant content was observed for samples produced by Pechini method. As for the systems prepared by combustion reaction, it was found that the secondary phases exert a strong influence on the magnetic behavior

Síntese e caracterização de ferritas de níquel dopadas com cobalto e efeito da substituição nas suas propriedades magnéticas

The ferrite composition Ni1 - xCoxFe2O4 (0 ≤ x ≤ 0.75) were obtained by the method of microwave assisted synthesis and had their structural and magnetic properties evaluated due to the effect of the substitution of Ni by Co. The compounds were prepared: according to the concept of chemical propellants and heated in the microwave oven with power 7000kw. The synthesized material was characterized by absorption spectroscopy in the infrared (FTIR), Xray diffraction (XRD) using the Rietveld refinement, specific surface area (BET) , scanning electron microscopy (SEM) with aid of energy dispersive analysis (EDS) and magnetic measurements (MAV). The results obtained from these techniques confirmed the feasibility of the method of synthesis employed to obtain the desired spinel structure, the ferrite, nickel ferrite as for nickel doped with cobalt. The results from XRD refinement ally showed the formation of secondary phases concerning stages α - Fe2O3, FeO, (FeCo)O e Ni0. On the other hand, there is an increase in crystallite size with the increase of cobalt in systems, resulting in an increased crystallinity. The results showed that the BET systems showed a reduction in specific surface area with the increase of cobalt and from the SEM, the formation of irregular porous blocks and that the concentration of cobalt decreased the agglomerative state of the system. The magnetic ferrites studied showed different characteristics according to the amount of dopant used, ranging from a very soft magnetic material (easy magnetization and demagnetization ) - for the system without cobalt - a magnetic material with a little stiffer behavior - for systems containing cobalt. The values of the coercive field increased with the increasing growth of cobalt, and the values of saturation magnetization and remanence increased up to x = 0,25 and then reduced. The different magnetic characteristics presented by the systems according to the amount of dopant used, allows the use of these materials as intermediates magnetic

Síntese de catalisadores nanoporosos na ausência total e parcial de direcionadores orgânicos para pirólise catalítica de óleos pesados e intermediários

The processing of heavy oil produced in Brazil is an emergency action and a strategic plan to obtain self-sufficiency and economic surpluses. Seen in these terms, it is indispensable to invest in research to obtain new catalysts for obtaining light fraction of hydrocarbons from heavy fractions of petroleum. This dissertation for the degree of Doctor of Philosophy reports the materials preparation that combine the high catalytic activity of zeolites with the greater accessibility of the mesoporosity, more particularly the HZSM-5/MCM-41 hybrid, done by synthesis processes with less environmental impact than conventional ones. Innovative methodologies were developed for the synthesis of micro-mesoporous hybrid material by dual templating mechanism and from crystalline zeolitic aluminosilicate in the absence of organic template. The synthesis of hybrid with pore bimodal distribution took place from one-single organic directing agent aimed to eliminate the use of organic templates, acids of any kind or organic solvents like templating agent of crystalline zeolitic aluminosilicate together with temperature-programmed microwave-assisted, making the experimental procedures of preparation most practical and easy, with good reproducibility and low cost. The study about crystalline zeolitic aluminosilicate in the absence of organic template, especially MFI type, is based on use of H2O and Na+ cation playing a structural directing role in place of an organic template. Advanced characterization techniques such as X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Highresolution Transmission Electron Microscopy (HRTEM), Adsorption of N2 and CO2, kinetic studies by Thermogravimetric Analysis (TGA) and Pyrolysis coupled to Gas Chromatography/Mass Spectrometry (Pyrolysis-GC/MS) were employed in order to evaluate the synthesized materials. Achieve the proposed objectives, has made available a set of new methodologies for the synthesis of zeolite and hybrid micro-mesoporous material, these suitable for catalytic pyrolysis of heavy oils aimed at producing light fraction

Comparative analysis of root surface smear layer removal by different etching modalities or erbium:yttrium-aluminum-garnet laser irradiation. A scanning electron microscopy study

The purpose of this study was to evaluate the effect of erbium:yttrium-aluminum-garnet (Er:YAG) laser (2.94 mu m) irradiation on the removal of root surface smear layer of extracted human teeth and to compare its efficacy with that of citric acid, ethylenediamine tetra-acetic acid (EDTA), or a gel containing a mixture of tetracycline hydrochloride (HCl) and citric acid, using scanning electron microscopy (SEM). Thirty human dentin specimens were randomly divided into six groups: G1 (control group), irrigated with 10 ml of physiologic saline solution; G2, conditioned with 24% citric acid gel; G3, conditioned with 24% EDTA gel; G4, conditioned with a 50% citric acid and tetracycline gel; G5, irradiated with Er:YAG laser (47 mJ/10 Hz/5.8 J/cm(2)/pulse); G6, irradiated with Er:YAG laser (83 mJ/10 Hz/10.3 J/cm(2)/pulse). Electron micrographs were obtained and analyzed according to a rating system. Statistical analysis was conducted with Kruskal-Wallis and Mann-Whitney tests (P < 0.05). G1 was statistically different from all the other groups; no statistically significant differences were observed between the Er:YAG laser groups and those undergoing the other treatment modalities. When the two Er:YAG laser groups were compared, the fluency of G6 was statistically more effective in smear layer removal than the one used in G5 (Mann-Whitney test, P < 0.01). Root surfaces irradiated by Er:YAG laser had more irregular contours than those treated by chemical agents. It can be concluded that all treatment modalities were effective in smear layer removal. The results of our study suggest that the Er:YAG laser can be safely used to condition diseased root surfaces effectively. Furthermore, the effect of Er:YAG laser irradiation on root surfaces should be evaluated in vivo so that its potential to enhance the healing of periodontal tissues can be assessed.

Evaluation of the Smear Layer and Hybrid Layer in Noncarious and Carious Dentin Prepared by Air Abrasion System and Diamond Tips

Purpose: To analyze the smear layer and the hybrid layer in noncarious and carious dentin prepared by different cutting instruments and restored with composite resin. Study design: Cavities were randomly prepared in 160 specimens (noncarious and artificial carious dentin) by high-speed diamond tips (KG Sorensen 1013), air abrasion system (Prepstart, Danville Engineering), ultrasonic tip (CVDentus 8.3231-1), and ultrasonic tip associated with ultrasonic cavitation by water for 10 s. Half of the cavities in each group were conditioned with 37% phosphoric acid for 15 s. The amount of smear layer and dentinal tubules present were analyzed using scanning electron microscopy and graded from 0 to 3. Cavities were prepared in another 20 noncarious specimens and 20 carious specimens and restored with adhesive composite resin system. The restorations were hemisected longitudinally and analyzed using scanning electron microscopy to evaluate the hybrid layer and resinous prolongation characteristics, using scores ranging from 1 to 6. Results: The data were statistically analyzed using Kruskal-Wallis and Dunn tests at 5% of significance level. There was evidence that the most efficient smear layer removal was the acid etching in the noncarious dentin and the water ultrasonic cavitation in the carious dentin. The hybrid layer formed on the noncarious and carious dentin prepared by the ultrasonic tip was more regular than in the specimens prepared by high-speed diamond tip, with many resinous prolongations. Conclusion: The ultrasonic tip seems to be a promising tool for carious dentin cavity preparation. Microsc. Res. Tech. 73:597-605, 2010. (C) 2009 Wiley-Liss, Inc.

Flexural strength of acrylic resin repairs processed by different methods: water bath, microwave energy and chemical polymerization

Denture fractures are common in daily practice, causing inconvenience to the patient and to the dentists. Denture repairs should have adequate strength, dimensional stability and color match, and should be easily and quickly performed as well as relatively inexpensive. Objective: The aim of this study was to evaluate the flexural strength of acrylic resin repairs processed by different methods: warm water-bath, microwave energy, and chemical polymerization. Material and methods: Sixty rectangular specimens (31x10x2.5 mm) were made with warm water-bath acrylic resin (Lucitone 550) and grouped (15 specimens per group) according to the resin type used to make repair procedure: 1) specimens of warm water-bath resin (Lucitone 550) without repair (control group); 2) specimens of warm water-bath resin repaired with warm water-bath; 3) specimens of warm water-bath resin repaired with microwave resin (Acron MC); 4) specimens of warm water-bath resin repaired with autopolymerized acrylic resin (Simplex). Flexural strength was measured with the three-point bending in a universal testing machine (MTS 810 Material Test System) with load cell of 100 kgf under constant speed of 5 mm/min. Data were analyzed statistically by Kruskal-Wallis test (p<0.05). Results: The control group showed the best result (156.04 +/- 1.82 MPa). Significant differences were found among repaired specimens and the results were decreasing as follows: group 3 (43.02 +/- 2.25 MPa), group 2 (36.21 +/- 1.20 MPa) and group 4 (6.74 +/- 0.85 MPa). Conclusion: All repaired specimens demonstrated lower flexural strength than the control group. Repairs with autopolymerized acrylic resin showed the lowest flexural strength.

The occurrence of porosity in reline acrylic resins. Effect of microwave disinfection

Microwave energy has proved to be an effective method for disinfecting acrylic dentures. However, the effect of microwave heating on the porosity of autopolymerising denture reline resins has not been investigated.The purpose of the study was to determine the effect of microwave disinfection on the porosity of autopolymerised denture reline materials (Kooliner-K, New Truliner-NT, Tokuso Rebase Fast-TR and Ufi Gel Hard-UGH) and a conventional heat-polymerised denture base resin (Lucitone 550-L).Specimens (10 mm x 20 mm x 1 mm) were obtained from the impression surface of the palatal mucosa in a single person and divided into four groups (n = 5). The porosity was evaluated after polymerisation (C1), after two cycles of microwave disinfection (MW2), after seven cycles of microwave disinfection (MW7) and after 7 days storage in water at 37 degrees C (C2). Specimens from group MW7 were exposed to microwave disinfection daily being stored in water at 37 degrees C between exposures. All the replicas were sputter coated with gold and micrographs/digital images were taken of each replica using scanning electron microscopy at magnification x 100. The SEM micrographs were then examined using an image analyser to determine the number of pores. Comparison between materials and groups were made using Kruskal-Wallis tests.MW7 resulted in a significant increase in the number from the pores of material K, but decreased in number in reline material TR and UGH reline resin. The number of pores in materials NT and L remained unaffected following microwave disinfection.Differences in the porosity amongst the materials and for different experimental conditions were observed following microwave disinfection.

Adhesive Bonding of Resin Composite to Various Ni-Cr Alloy Surfaces Using Different Metal Conditioners and a Surface Modification System

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

Comparative scanning electron microscopic study of the effect of different dental conditioners on dentin micromorphology

This study evaluated comparatively by scanning electron microscopy (SEM) the effect of different dental conditioners on dentin micromorphology, when used according to the same protocol. Forty dentin sticks were obtained from 20 caries-free third human molars and were assigned to 4 groups corresponding to 3 conditioners (phosphoric acid 37%, Clearfil SE Bond and iBond) and an untreated control group. After application of the conditioners, the specimens were immersed in 50% ethanol solution during 10 s, chemically fixed and dehydrated to prepare them to SEM analysis. In the control group, dentin surface was completely covered by smear layer and all dentinal tubules were occluded. In the phosphoric acid-etched group, dentin surface was completely clean and presented exposed dentinal tubule openings; this was the only group in which the tubules exhibited the funnel-shaped aspect. In the groups conditioned with Clearfil SE Bond primer and iBond, which are less acidic than phosphoric acid, tubule openings were occluded or partially occluded, though smear layer removal was observed. SE Bond was more efficient in removing the smear layer than iBond. In the Clearfil SE Bond group, the cuff-like aspect of peritubular dentin was more evident. It may be concluded all tested conditioners were able to change dentin morphology. However, it cannot be stated that the agent aggressiveness was the only cause of the micromorphological alterations because a single morphological pattern was not established for each group, but rather an association of different aspects, according to the aggressiveness of the tested conditioner.

Female reproductive system of the decapitating fly Pseudacteon wasmanni Schmitz (Diptera : Phoridae)

Pseudacteon wasmanni is a South American decapitating fly that parasitizes workers of Solenopsis fire ants. We used light microscopy (historesin serial-sectioning stained with Haematoxylin/Eosin) and scanning electron microscopy to show and analyze internal and whole external views of the female reproductive system. All specimens analyzed (n = 9) by light microscopy showed post-vitellogenic oocytes inside the ovaries. The lack of typical follicles (oocyte-nurse cell complexes) in all specimens suggests that oogenesis occurs during the pupal stage. The total number of eggs found ranged from 31 to 280 (X = 142 +/- 73, SD). The egg has a slugform or torpedo shape (about 130 by 20 mum) with a pointed apex at the posterior pole as defined by the fly; the micropyle appears to be in a depression or invagination at the anterior pole. An acute hypodermic-like ovipositor is evaginated from the hard sclerotized external genitalia during egg laying. The existence of a muscular bulb associated with the end of the common oviduct suggests that the egg is injected into the ant's body by a strong contraction of the bulb which probably is stimulated by bending of several ventral sensilla. During contraction, the abdomen extends out along a large fold between the sixth and seventh tergites in such a way that the sclerotized genitalia is rotated ventrally into a slightly anterior orientation in preparation for oviposition. (C) 2003 Elsevier B.V. Ltd. All rights reserved.

Thermal and Structural Behavior of Dioctadecyldimethylammonium Bromide Dispersions Studied by Differential Scanning Calorimetry and X-Ray Scattering

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

Simultaneous observation of the magnetic and electric behavior in a correlated system near a metal-semiconductor transition: ESR in pellets of conducting polymers

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

Photoluminescence properties and synthesis of a PZT mesostructure obtained by the microwave-assisted hydrothermal method

Micro-cube-shaped lead zirconate titanate was synthesized using the microwave-assisted hydrothermal method. Photoluminescence and field emission scanning electron microscopy were used for monitoring the formation of mesocrystals. Based on these results, a growth mechanism was then proposed which involved nanoparticle aggregation, nanoplate self-assembly on specific architecture and the final formation of mesoscopic micro-cube-shaped lead zirconate titanate. (C) 2011 Elsevier B. V. All rights reserved.