Síntese de nanopartículas de magnetita via decomposição térmica em meio não-aquoso

This work aims at obtaining nanoparticles of iron oxide, the magnetite one (Fe3O4), via synthesis by thermal decomposition through polyol. Thus, two routes were evaluated: a simple decomposition route assisted by reflux and a hydrothermal route both without synthetic air atmosphere using a synthesis temperature of 260ºC. In this work observed the influence of the observe of surfactants which are generally applied in the synthesis of iron oxide nanoparticles decreasing cluster areas. Further, was observed pure magnetite phase without secondary phases generally found in the iron oxide synthesis, a better control of crystallite size, morphology, crystal structure and magnetic behavior. Finally, the introduction of hydroxyl groups on the nanoparticles surface was analyzed besides its employment in the polymer production with OH radicals. The obtained materials were characterized by XRD, DLS, VSM, TEM, TG and DSC analyses. The results for the magnetite obtainment with a particle size greater than 5 nm and smaller than 11 nm, well defined morphology and good magnetic properties with superparamagnetic behavior. The reflux synthesis was more efficient in the deposition of the hydroxyl groups on the nanoparticles surface

Estudo tribológico de biolubrificantes com adição de nanopartículas de óxidos (zinco e cobre)

Currently, vegetable oils have been studied for bio-lubricants base that fits the new environmental standards. Since, in a world full of finite natural resources, mineral oils bring consequences to the environment due to its low biodegradability and toxicity, also it is important to consider that synthetic oils have a high cost The aim of this work is to obtain a biolubricant additived with oxide nanoparticles (ZnO and CuO) for better resistance to friction and wear, which is not toxic to the environment and have better adherence under boundary lubrication. The methodology consisted in the synthesis of bio-lubricants (soybean and sunflower base) by epoxidation reaction. Then, some physical-chemical analysis in bio-lubricants are made to characterize theses lubricants, such as, density, acidity, iodine value, viscosity, viscosity index. Later, the lubricants were additive with nanoparticles. The tribological performance was evaluated by the equipment HFRR (High Frequency Reciprocating Rig) consisting of a wear test ball-plan type. The characterization of wear analysis was performed by SEM / EDS. The results show that bio-lubricants may be synthesized by reaction of epoxidation with good conversion. Tribological point of view, the epoxidized oils are more effective than lubricant additived with the oxide nanoparticles, they had lower coefficients of friction and better rate of film formation in the study. However, because they are environmentally friendly, bio-lubricants gain the relevant importance in tribological field

Investigação da estabilidade térmica e das propriedades elétricas do TiO2 em função da dopagem com Ce(SO4)2

The metalic oxides have been studies due to differents applications as materials semiconductor in solar cells, catalysts, full cells and, resistors. Titanium dioxide (TiO2) has a high electric conductivity due to oxygen vacancies. The Ce(SO4)2.2H2O doped samples TiO2 and TiO2 pure was obtained sol-gel process, and characterized by X-ray diffractometry,thermal analysis, and impedance spectroscopy. The X-ray diffraction patterns for TiO2 pure samples shows at 700°C anatase phase is absent, and only the diffraction peaks of rutile phase are observed. However, the cerium doped samples only at 900°C rutile in the phase present with peaks of cerium dioxide (CeO2). The thermal analysis of the TiO2 pure and small concentration cerium doped samples show two steps weight loss corresponding to water of hydration and chemisorbed. To larger concentration cerium doped samples were observed two steps weight loss in the transformation of the doped cerium possible intermediate species and SO3. Finally, two steps weight loss the end products CeO2 and SO3 are formed. Analyse electric properties at different temperatures and concentration cerium doped samples have been investigated by impedance spectroscopy. It was observed that titanium, can be substituted by cerium, changing its electric properties, and increased thermal stability of TiO2 anatase structure

Síntese e caracterização de óxidos de zinco e de magnésio suportados em A1SBA-15 para produção de biodiesel

To overcome the challenge of meeting growing energy demand in a sustainable way, biodiesel has shown very promising as alternative energy can replace fossil fuels, even partially. Industrially, the biodiesel is produced by homogeneous transesterification reaction of vegetable oils in the presence of basic species used as catalysts. However, this process is the need for purification of the esters obtained and the removal of glycerin formed after the reaction. This context, the alternative catalysts have that can improve the process of biodiesel production, aiming to reduce costs and facilitate its production. In this study, the AlSBA-15 support with Si / Al ratio = 50 was synthesized, as like as the heterogeneous catalysts of zinc oxide and magnesium supported on mesoporous AlSBA-15 silica, in the concentrations of 5, 10, 15 and 30 %, relative to the support. The textural properties and structural characterization of catalysts and supports were determined by techniques: X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) coupled to the chemical analyzer, adsorption / desorption of N2, thermal analysis (TG / DTG), absorption spectroscopy in the infrared (FTIR) and X-ray photoelectron spectroscopy (XPS). Characterization results indicated that the support AlSBA-15 retained the hexagonal ordered after the incorporation of zinc oxide and magnesium oxide in the holder. For heterogeneous catalysts, ZnO-AlSBA-15, that was observed the presence of zinc oxide nanoparticles dispersed in the surface and interior channels of the mesoporous and microporous support. The catalytic activity was evaluated by the transesterification reaction of sunflower oil via methylic route, and some reaction parameters were optimized with the most active catalyst in biodiesel production by sunflower oil. For the series of heterogeneous catalysts, the sample with 30 % ZnO supported on AlSBA-15 showed a better conversion of triglyceride to methyl esters, about 95.41 % of reaction conditions: temperature 175 °C, with molar ratio of 42:1, stirring at 200 rpm and under a pressure of 14 bar for 6 h. The catalyst MgO-AlSBA-15 showed no catalytic activity in the studied reactions

Activity and characterization by XPS, HR-TEM, Raman spectroscopy, and BET surface area of CuO/CeO2-TiO2 catalysts

Structural and textural studies of a CuO/TiO2 System modified by cerium oxide were conducted using Raman spectroscopy, transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and N-2 absorption (BET specific surface area). The introduction of a minor amount of CeO2 (Ce0.09Ti0.82O1.91CU0.09 sample) resulted in a material with the maximum surface area value. The results of Raman spectroscopy revealed the presence of only two crystalline phases, TiO2 anatase and CeO2 cerianite, with well-dispersed copper species. TEM micrographs showed a trend toward smaller TiO2 crystallites when the cerium oxide content was increased. The XPS analysis indicated the rise of a second peak in Ti 2p spectra with the increasing amount of CeO2 located at higher binding energies than that due to the Till in a tetragonal symmetry. The CuO/TiO2 system modified by CeO2 displayed a superior performance for methanol dehydrogenation than the copper catalyst supported only on TiO2 or CeO2.

Síntese e caracterização textural do catalisador CeO2/TiO2 obtido via sol-gel: fotocatálise do composto modelo hidrogenoftalato de potássio

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

XPS study of the corrosion protection of fluorozirconate glasses dip-coated with SnO2 transparent thin films

Tin oxide nanoparticles prepared by an aqueous sol-gel method were deposited by dip-coating on fluorozirconate glass, ZBLAN (53%ZrF4-20%BaF2-4%LaF3-3%AlF3-20%NaF) to improve its resistance against wet corrosion. The aqueous leaching of uncoated and SnO2-coated fluorozirconate glass was studied by X-ray photoemission spectroscopy (XPS) and it was shown that even an ultra thin tin dioxide film provides good protection of the glass surface against the bulk propagation of the hydrolytic attack.

Rare Earth Doped SnO(2) Nanoscaled Powders and Coatings: Enhanced Photoluminescence in Water and Waveguiding Properties

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

PEGylation of SPIONs by polycondensation reactions: A new strategy to improve colloidal stability in biological media

In this study, we report on a new route of PEGylation of superparamagnetic iron oxide nanoparticles (SPIONs) by polycondensation reaction with carboxylate groups. Structural and magnetic characterizations were performed by X-ray diffractometry (XRD), transmission electron microscopy (TEM), thermogravimetric analysis (TGA), and vibrating sample magnetometry (VSM). The XRD confirmed the spinel structure with a crystallite average diameter in the range of 3.5-4.1 nm in good agreement with the average diameter obtained by TEM (4.60-4.97 nm). The TGA data indicate the presence of PEG attached onto the SPIONs' surface. The SPIONs were superparamagnetic at room temperature with saturation magnetization (M S) from 36.7 to 54.1 emu/g. The colloidal stability of citrate- and PEG-coated SPIONs was evaluated by means of dynamic light scattering measurements as a function of pH, ionic strength, and nature of dispersion media (phosphate buffer and cell culture media). Our findings demonstrated that the PEG polymer chain length plays a key role in the coagulation behavior of the Mag-PEG suspensions. The excellent colloidal stability under the extreme conditions we evaluated, such as high ionic strength, pH near the isoelectric point, and cell culture media, revealed that suspensions comprising PEG-coated SPION, with PEG of molecular weight 600 and above, present steric stabilization attributed to the polymer chains attached onto the surface of SPIONs. © 2013 Springer Science+Business Media Dordrecht.

Preparação de catalisadores de reforma de glicerol para células a combustível de eletrólito sólido

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Hibridos siloxano-polímero no comportamento hidrofilico de diferentes materiais

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Síntese e aplicação de catalisadores à base de óxidos de cério, tungstênio e HZSM-5 para a produção do biodiesel

This work presents a study on the production of biodiesel by esterification reaction of oleic acid with methanol using batch reactor and different catalysts based on CeO2 and WO3 and HZSM-5. Acid treatment was performed in order to increase the catalytic activity. Different characterization techniques were performed, among them X-ray diffraction (XRD), Thermogravimetric analysis TGA/DTA, Spectroscopy in the Region in Fourier Transform Infrared (FTIR) and X-ray fluorescence (XRF). The effects of independent variables: temperature, molar ratio of oil: alcohol and the amount of catalyst and their interactions on the dependent variable (conversion of oleic acid to the corresponding ester). Overall, through the results obtained in the characterization was observed that the applied treatments were efficient, however the XRF technique, indicated that tungsten oxide leaching could occur during the preparation of the materials. The treatments performed on HZSM-5 caused no significant changes in the structure indicating that the zeolite was quite resistant to the treatments used. It was evaluated using complete 23 factorial design. For the catalysts investigated, the best reaction conditions were obtained when using higher levels of the independent variables temperature and amount of catalyst. However, for the variable molar ratio the lowest level showed significant yields for most of the synthesized catalyst, obtaining maximum conversion to the OC (67.97%), OW (74.37%), HZSM-5 (61.16%) OC-OW 1 (75.93%), OC-OW 2 (82.57%), OC-OW 3 (79.15%), S/OC-OW 1 (86.90%), S/OC-OW 2 (91.04%), S/OC-OW 3 (88.60%), S/OC-OW/H 1 (92.34%), S/OC-OW/H 2 (100%) and S/OC-OW/H 3 (98.16%). According to the experimental design, the temperature has the biggest influence on the reaction variable for all the synthesized catalysts. Among the catalysts investigated S/OC-OW/H 2 e S/OC-OW/H 3 were more effective. Reuse tests showed that the catalyst activity decreased after each cycle, indicating that the regeneration process was effective. The leaching test indicated that the catalysts are heterogeneous in the evaluated operating range. The catalysts investigated showed themselves promising for the production of biodiesel.

Síntese e caracterização da cerâmica 'Ti IND. x''('Sm IND. 0,2''Ce IND. 0,8') IND. (1-x)''O IND. (2-Б) para aplicação como anodo em células a combustível de óxido sólido

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Síntese e funcionalização de superfícies de óxido de ferro superparamagnéticos

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Estudo do crescimento de nanofitas de céria dopada com gadolínio por sistema de aquecimento por micro-ondas

O óxido de cério (céria) tem atraído atenção devido às suas importantes aplicações, como em células a combustível de óxido sólido, catalisadores de gases de exaustão de automóveis, catalisadores para a obtenção de hidrogênio, bloqueadores de raios ultravioleta, biomateriais, entre outros. Controlar os métodos de síntese da céria é de grande importância para explicar ou prever essas propriedades. Desta forma, o objetivo deste trabalho foi estudar o crescimento de nanofitas de óxido de cério em um sistema hidrotérmico assistido por micro-ondas, no qual 8 min foram obtidas nanofitas com comprimentos próximos a 330 nm, em 130 ºC e pressão de 3 atm. Os resultados colaboram para pesquisas em reformadores para obtenção de etanol e/ou anodos de células combustíveis de óxido sólido.