923 resultados para XRD, Raman, SEM, TEM, XPS, cobalt hydroxide, cobalt oxyhydroxide, cobalt oxide


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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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In this work Ba0.99Eu0.01MoO4 (BEMO) powders were prepared by the first time by the Complex Polymerization Method. The structural and optical properties of the BEMO powders were characterized by Fourier Transform Infra-Red (FTIR), X-ray Diffraction (XRD), Raman Spectra, High-Resolution Scanning Electron Microscopy (HR-SEM) and Photoluminescent Measurements. XRD show a crystalline scheelite-type phase after the heat treatment at temperatures greater than 400 degrees C. The ionic radius of Eu3+ (0.109 nm) is lower than the Ba2+ (0.149 nm) one. This difference is responsible for the decrease in the lattice parameters of the BEMO compared to the pure BaMoO4 matrix. This little difference in the lattice parameters show that Eu3+ is expected to occupy the Ba2+ site at different temperatures, stayed the tetragonal (S-4) symmetry characteristic of scheelite-type crystalline structures of BaMoO4. The emission spectra of the samples, when excited at 394 nm, presented the D-5(1)-> F-7(0, 1 and 2) and D-5(0)-> F-7(0, 1, 2, 3 and 4) Eu3+ transitions at 523, 533, 554, 578, 589, 614, 652 and 699 nm, respectively. The emission spectra of the powders heat-treated at 800 and 900 degrees C showed a marked increase in its intensities compared to the materials heat-treated from 400 to 700 C. The decay times for the sample were evaluated and all of them presented the average value of 0.61 ms. Eu3+ luminescence decay time follows one exponential curve indicating the presence of only one type of Eu3+ symmetry site.

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

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A preparation method for a new electrode material based on the LiNi0.8Co0.2O2/polyaniline (PANI) composite is reported. This material is prepared by in situ polymerization of aniline in the presence of LiNi0.8Co0.2O2 assisted by ultrasonic irradiation. The materials are characterized by XRD, TG-DTA, FTIR, XPS, SEM-EDX, AFM, nitrogen adsorption (BET surface area) and electrical conductivity measurements. PANI in the emeraldine salt form interacts with metal-oxide particles to assure good connectivity. The dc electrical conductivity measurements at room temperature indicate that conductivity values are one order of magnitude higher in the composite than in the oxide alone. This behavior determines better reversibility for Li-insertion in charge-discharge cycles compared to the pristine mixed oxide when used as electrode of lithium batteries. (c) 2005 Elsevier B.V. All rights reserved.

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The BaMoO4 nanopowders were prepared by the Complex Polymerization Method (CPM). The structure properties of the BaMoO4 powders were characterized by FTIR transmittance spectra, X-ray diffraction (XRD), Raman spectra, photoluminescence spectra (PL) and high-resolution scanning electron microscopy (HR-SEM). The XRD, FTIR and Raman data showed that BaMoO4 at 300 degrees C was disordered. At 400 degrees C and higher temperature, BaMoO4 crystalline scheelite-type phases could be identified, without the presence of additional phases, according to the XRD, FTIR and Raman data. The calculated average crystallite sizes, calculated by XRD, around 40 nm, showed the tendency to increase with the temperature. The crystallite sizes, obtained by HR-SEM, were around of 40-50 nm. The sample that presented the highest intensity of the red emission band was the one heat treated at 400 degrees C for 2 h, and the sample that displayed the 'highest intensity of the green emission band was the one heat treated at 700 degrees C for 2 h. The CPM was shown to be a low cost route for the production of BaMoO4 nanopowders, with the advantages of lower temperature, smaller time and reduced cost. The optical properties observed for BaMoO4 nanopowders suggested that this material is a highly promising candidate for photoluminescent applications. (C) 2005 Elsevier B.V. All rights reserved.

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SnO2:m mol% CoO (0.5 less than or equal to m less than or equal to 6.0) ceramic specimens were studied by impedance spectroscopy in the 5 Hz-13 MHz frequency range during heating cold-pressed specimens from room temperature to 1250 degrees C. The electrical resistivity during sintering decreases from 4 to 6 orders of magnitude in the 400-1500 K temperature range depending on the amount of CoO. An increase in electrical resistivity in the 570-670 K range is related to the release of adsorbed water. The results for the 970-1500 K show that the higher the amount of the CoO addition, the lower is the temperature at which SnO2:CoO reaches a minimum electrical resistivity. This suggests that oxygen point defects created by dissolution of cobalt ions in the SnO2 lattice are controlling the densification rate of these ceramics.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Bi4Ti3O12 powder was synthesized from bismuth oxide and titanium oxide. Mixture of oxides was milled in zirconium oxide jar in the planetary ball-mill during 1, 3 and 6 h. Extended time of milling directed to formation of higher amount of titanates perovskite phase. Bi4Ti3O12 was formed between 1 and 3 h of milling time. The phase formation of Bi4Ti3O12, crystal structure and powder particle size were followed by XRD, Raman spectroscopy and SEM analysis. After milling for various times the powders were compacted by pressing and isothermal sintering. Sample milled for 3 h and subsequently sintered at 1000C for 24 h exhibit a hysteresis loop, confirming that the synthesized material possesses ferroelectric properties. All results affect that the structure Bi4Ti3O12 is strongly dependent on the milling time.

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This study was conducted to observe the rat subcutaneous connective tissue reaction to the implanted dentin tubes filled with calcium hydroxide or mineral trioxide aggregate. The animals were sacrificed after 7 and 30 days, and the specimens were prepared for morphological study. Some undecalcified specimens were prepared for histological analysis with polarized light and Von Kossa technique for calcium. The results were similar for both studied materials. At the tube openings, there were Von Kossa-positive granules that were birefringent to polarized light. Next to these granulations, there was an irregular tissue like a bridge that was Von Kossa-positive. The dentin walls of the tubes exhibited in the tubules a structure highly birefringent to polarized light, usually like a layer and at different depths. It is possible that the mechanism of action of both materials has some similarity. Copyright © 1999 by The American Association of Endodontists.

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This study was conducted to observe the rat subcutaneous connective tissue reaction to implanted dentin tubes that were filled with mineral trioxide aggregate, Sealapex, Calciobiotic Root Canal Sealer (CRCS), Sealer 26, and the experimental material, Sealer Plus. The animals were sacrificed after 7 and 30 days, and the specimens were prepared for histological analysis after serial sections with a hard-tissue microtome. The undecalcified sections were examined with polarized light after staining according to the Von Kossa technique for calcium. At the tube openings, there were Von Kossa-positive granules that were birefringent to polarized light. Next to these granulations, there was irregular tissue, like a bridge, that was Von Kossa-positive. The dentin walls of the tubes exhibited a structure highly birefringent to polarized light, usually like a layer, in the tubules. These results were observed with all the studied materials, except the CRCS, which didn't exhibit any kind of mineralized structure. The results suggest that among the materials studied, the CRCS could have the least possibility of encouraging hard tissue deposition.

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Objectives: To compare the response of human dental pulp capped with a mineral trioxide aggregate (MTA) and Ca(OH) 2 powder. Methods and Material: Pulp exposures were performed on the occlusal floor of 40 permanent premolars. The pulp was then capped with either Ca(OH) 2 powder (CH) or MTA and restored with resin composite. After 30 days (groups CH30 and MTA30) and 60 days (groups CH60 and MTA60), the teeth were extracted and processed for HE and categorized in a histological score system. The data were subjected to Kruskal-Wallis and Conover tests (α=0.05). Results: In regard to dentin bridge formation, CH30 showed a tendency towards superior performance compared to MTA30 (p>0.05), although the products showed comparable results at day 60. In the item Inflammation and General State of the Pulp (p>0.05), CH showed a tendency towards presenting a higher inflammatory response. In the item Other Pulpal Findings, MTA and Ca(OH) 2 showed equal and excellent performance after 30 and 60 days (p>0.05). Conclusion: After 30 days, Ca(OH) 2 powder covered with calcium hydroxide cement showed faster hard tissue bridge formation compared to MTA. After 60 days, Ca(OH) 2 powder or MTA materials showed a similar and excellent histological response with the formation of a hard tissue bridge in almost all cases with low inflammatory infiltrate. © Operative Dentistry, 2008.

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The purpose of this study was to evaluate the radiopacity of root canal sealers containing calcium hydroxide and MTA (Acroseal, Sealer 26, Sealapex, Endo CPM Sealer, Epiphany and Intrafill). Five disc-shaped specimens (10 x 1 mm) were fabricated from each material, according to the ISO 6876/2001 standard. After setting of the materials, radiographs were taken using occlusal film and a graduated aluminum stepwedge varying from 2 to 16 mm in thickness. The dental X-ray unit (GE1000) was set at 50 kVp, 10 mA, 18 pulses/s and distance of 33.5 cm. The radiographs were digitized and the radiopacity compared to that of the aluminum stepwedge using VIXWIN-2000 software (Gendex). The data (mmAl) were analyzed statistically by ANOVA and Tukey's test at the 5% significance level. Epiphany and Intrafill presented the highest radiopacity values (8.3 mmAl and 7.5 mmAl respectively, p < 0.05) followed by Sealer 26 (6.3 mmAl), Sealapex (6.1 mmAl) and Endo CPM Sealer (6 mmAl). Acroseal was the least radiopaque material (4 mmAl, p < 0.05). In conclusion, the calcium hydroxide- and MTA-containing root canal sealers had different radiopacities. However, all materials presented radiopacity values above the minimum recommended by the ISO standard. © 2009 Sociedade Brasileira de Pesquisa Odontológica.

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The main aim of this study was to develop dense and conducting SnO 2 ceramics without precipitated phases on the grain boundaries, which was verified using field emission scanning microscopy (FE-SEM) coupled with an energy-dispersive X-ray spectroscopy (FE-SEM/EDS). Two sample groups were investigated, where the first sample group was doped with zinc while the second one was doped with cobalt. The ceramics were prepared using the oxides mixture method and the sintering was carried out in a conventional muffle oven as well as in microwave oven. The results obtained were found to be similar regarding the relative density for the two sintering methods while time and temperature gains were observed for the microwave sintering method. The relative densities obtained were nearly 95%, for the two sintering methods. Concerning the electrical characterization measurements-electric field x current density as well as the environment temperature, the ceramics obtained through the conventional sintering method presented non-ohmic behavior. For the microwave sintered ceramics, we observed an ohmic behavior with electrical resistivity of 1.3 Ωcm for the samples doped with ZnO/Nb 2O 5 and 2.5 Ωcm for that of the samples doped with CoO/Nb 2O 5. The FE-SEM/EDS results for the microwave sintered ceramics indicated a structure with a reduced number of pores and other phases segregated at the grain boundaries, which leads to a better conductive ceramic than the conventional oven sintered samples. The dilatometry analysis determined the muffle sintering temperature and the difference between the densification of cobalt and zinc oxides. The addition of niobium oxide resulted in the decrease in resistivity, which thus led us to conclude that it is possible to obtain dense ceramics with low electrical resistivity based on SnO 2 using commercial oxides by the oxides mixture technique and the microwave oven sintering method. Copyright © 2011 American Scientific Publishers All rights reserved.

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Newly available materials for retrograde obturation should have their sealing properties evaluated. The goal of this study was to evaluate the sealing ability of Endo CPM sealer, an MTA-based endodontic cement. Single-rooted extracted human teeth were endodontically treated. After apical sectioning, retrograde cavities were prepared. Teeth were divided into five experimental groups (n=12), in which the following materials were used: Sealer 26 (S26), white Mineral Trioxide Aggregate (MTA), Endo CPM Sealer (CPM1), Endo CPM Sealer in thicker consistency (CPM 2), and zinc oxide and eugenol cement (ZOE), and two control groups (n=3). After retrograde obturation, the teeth were immersed in 0.2% rhodamine B dye for 48 hours in a vacuum chamber Marginal leakage data were subjected to ANOVA and Tukey tests at 5% significance level. S26 presented greater sealing ability (p<0.05) than ZOE, MTA, CPM1, and CPM2, all of which had similar results (p>0.05). We concluded that Sealer 26 has the greatest sealing ability. Endo CPM Sealer, with sealing ability similar to MTA, could be used as a retrograde obturation material.