896 resultados para ASSISTED GALVANIC REDUCTIONS
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We have studied the experimental conditions needed to produce LaNiO3 (LNO) nanostructures using a template-assisted method. In this route, a mesoporous anodic aluminum oxide template was filled with a chemical solution that had been prepared with polymeric precursors route. The precursor solutions and synthesized samples were characterized by X-ray diffraction (XRD), thermogravimetric analysis, infrared spectroscopy and high-resolution scanning electron microscopy (HRSEM). The XRD results for the samples that were heat-treated at 700 degrees C revealed that these samples crystallize in a perovskite-like LaNiO3 structure. HRSEM images revealed that the samples prepared with different deposition times (0.5, 1 and 2 h) promoted the formation of LaNiO3 nanotubes with different wall thicknesses.
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In the work presented here, Ce0.97Cu0.03O2 nanoparticles were synthesized by a microwave-assisted hydrothermal method under different synthesis temperatures. The obtained nanoparticles were tested as catalysts in preferential oxidation of CO to obtain CO-free H2 (PROX reaction). The samples were characterized by X-ray diffraction, transmission electron microscopy (TEM), electron paramagnetic resonance spectroscopy (EPR) and temperature-programmed reduction (TPR). X-ray diffraction measurements detected the presence of pure cubic CeO2 for all synthesized samples. TEM images of the Ce0.97Cu0.03O2 nanoparticles revealed that samples synthesized at 80°C are composed mainly of nanospheres with an average size of 20 nm. The formation of some nanorods with an average diameter of 8 nm and 40 nm in length, and the size reduction of the nanoparticles from 20 to approximately 15 nm is observed with increasing synthesis temperature. EPR spectra indicated that copper is found well dispersed in sample synthesized at 160°C, located predominant in surface sites of ceria. For samples synthesized at 80 and 120°C, the species are less dispersed than in the other one, resulting in the formation of Cu2+−Cu2+ dimmers at the surface of ceria. TPR profiles presented two reduction peaks, one below 400°C attributed to the reduction of different copper species and a second peak around 800°C attributed to the reduction of Ce4+→ Ce3+ species located in the volume of the nanoparticles. The peak related to the reduction of copper species shifts to lower temperatures with increasing synthesis temperature, i.e., the sample synthesized at 160°C is more easily reduced than the ones synthesized at 120 and 80°C. The nanoparticles showed active as catalysts for the CO-PROX reaction. The microwave-assisted method revealed efficient for the synthesis of Ce0.97Cu0.03O2 nanoparticles with copper species selective for the CO-PROX reaction, which reaches CO conversions up to 92% for the sample synthesized at 160°C.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
Microwave-assisted hydrothermal synthesis of NiO-Ce1-XEuxO2-δ powders for fuel cell catalytic anodes
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CeO2-based materials doped with rare earth (TR +3) can be used as alternative to traditional NiO-YSZ anodes in solid oxide fuel cells as they have higher ionic conductivity and lower ohmic losses compared to YSZ. Moreover, they allow fuel cell operation at lower temperatures (500-800°C). In the anode composition, the concentration of NiO acting as catalyst in YSZ provides high electrical conductivity and high electrochemical activity of reactions, promoting internal reform in the cell. In this work, NiO - Ce1-xEuxO2-δ compounds (x = 0.1, 0.2 and 0.3) have been synthesized by microwave-assisted hydrothermal method. The materials were characterized by TG, XRD, TPR and SEM-FEG techniques. The refinement of data obtained by X-ray diffraction showed the presence of ceria doped with europium crystallized in a cubic phase with fluorite structure, in addition to the presence of NiO. The microwave-assisted hydrothermal method showed significant reduction in the average particle size and good mass control of phase compositions compared to other chemical synthesis techniques.
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In the present work, we report the synthesis and characterization of NaNbO3 particles obtained by microwave-assisted hydrothermal method from Nb2O5 and NaOH. The synthesis was made at different periods at 180 °C and 300W. The crystallization of NaNbO3 structures produced Na2Nb2O6.H2O in the intermediate phase with fiber-like morphology, and this is associated with the synthesis time. Pure orthorhombic NaNbO3 with cube-like morphology originates after synthesizing for 240 minutes. To verify the remnant polarization of particles, films were obtained by electrophoresis process and sintered at 800°C for 10 minutes in a microwave furnace. The films characterization indicated that films of niobate with fiber-like morphology present remaining polarization, and the morphology of cubes did not show remaining polarization. Considering these results, it can be concluded that the morphology implemented ferroelectric property of NaNbO3.
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Bone defects at interdental osteotomy sites are as a complication of surgi-cally assisted rapid palatal expansion (SARPE). The replacement of osseoustissue by fibrous connective tissue impairs the spontaneous closure of adiastema between central incisors, and orthodontic tooth movementthrough the defect area may lead to root resorption. Treatment of such asituation requires an orthodontic-surgical approach. In this report, wedescribe the lack of bone healing at the midline osteotomy site after SARPE,which was treated by autogenous bone grafting as assessed by cone beamcomputed tomography. In addition, we discuss factors related to the aetiol-ogy and treatment of a bone defect after SARPE.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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ObjectiveThis study aimed to evaluate the benefit and specifically the feasibility of using ultrasound in ophthalmologic periconal block, and the occurrence of complications.Study designProspective experimental study.AnimalsTen healthy New Zealand White rabbits (6-8months of age), weighing 2.0-3.5kg.MethodsRabbits were anesthetized by intramuscular injection of acepromazine (1mgkg(-1)), ketamine (30mgkg(-1)) and xylazine (3mgkg(-1)). Ultrasound-assisted periconal block with lidocaine was performed on 18 eyes. Intraocular pressure was measured by applanation tonometry whereas corneal sensitivity was assessed using an esthesiometer, before and after each periconal anesthesia.ResultsIn all 18 eyes, it was possible to adequately visualize the needle shaft within the periconal space, as well as muscular cone, optic nerve and local anesthetic solution spread. Lidocaine 2% without epinephrine (0.790.19mL) was injected into the periconal space. There was no statistical difference between the intraocular pressure (meanSD) measured before (10.9 +/- 2.9mmHg) and after (11.9 +/- 3.8mmHg) the periconal anesthesia (p=0.38). The effectiveness of the ultrasound-assisted technique was shown according to the values for corneal sensitivity, assessed before and after periconal anesthesia (p<0.0001). Complications were not observed in this study.ConclusionsEye ultrasonography allowed visualization of all anatomic structures necessary to perform a periconal block, as well as the needle insertion and anesthetic spread in real time. Further studies are required to prove the real potential of ultrasound for reducing the incidence of complications associated with ophthalmic blocks, especially when anatomic disorders of the eye could potentially increase the risk.Clinical relevanceUltrasonography is a painless, noninvasive tool that may improve safety of ophthalmic regional blocks, potentially by reducing the prevalence of globe perforation or penetration of the optic nerve associated with the needle-based techniques.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Isolates of Paracoccidioides brasiliensis and Paracoccidioides lutzii, previously characterized by molecular techniques, were identified for the first time by matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS). All isolates were correctly identified, with log score values of >2.0. Thus, MALDI-TOF MS is a new tool for differentiating species of the genus Paracoccidioides.
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A pretreatment with microwave irradiation was applied to enhance enzyme hydrolysis of corn straw and rice husk immersed in water, aqueous glycerol or alkaline glycerol. Native and pretreated solids underwent enzyme hydrolysis using the extract obtained from the fermentation of Myceliophthora heterothallica, comparing its efficiency with that of the commercial cellulose cocktail Celluclast (R). The highest saccharification yields, for both corn straw and rice husk, were attained when biomass was pretreated in alkaline glycerol, method that has not been previously reported in literature. Moreover, FTIR, TG and SEM analysis revealed a more significant modification in the structure of corn straw subjected to this pretreatment.Highest global yields were attained with the crude enzyme extract, which might be the result of its content in a great variety of hydrolytic enzymes, as revealed zymogram analysis. Moreover, its hydrolysis efficiency can be improved by its supplementation with commercial beta-glucosidase.
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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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The rapid synthesis of Mn3O4 powders by a two-step process of pyro-synthesis of ethylene glycol-metal nitrate precursor assisted by nitric acid is reported. A new strategy that accelerates the synthesis and allows obtaining highly pure crystalline Mn3O4 is discussed. The structural and morphological characteristics of the Mn3O4 powders are presented and discussed. The mechanism of formation of the Mn3O4 is also discussed. In comparison with other synthesis methods, the present method shows that the proposed route of synthesis has the main advantage of high production of the powder material in a very short time.
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In this work we studied the synthesis of BSCCO-2212 superconducting phase associating a quite similar method developed by Pechini with the microwave-assisted hydrothermal method. To study the influence of the microwaves on the properties of BSCCO system, we synthesized two samples by such method. For one sample we used carbonates and for the other one we used nitrates as chemical reagents. We also produced a reference sample just using carbonates by Pechini's method to compare their morphological and superconducting properties. The structural properties of the samples were analyzed by scanning electron microscopy and X-ray diffraction. The Bi-2212 phase is predominant in all samples and despites the nitrates-like sample has a broader distribution of grain size in comparison with the reference sample, its magnetic behaviour is closer to that presented by the reference one.