JAQUELINE DE SOUZA DA SILVA
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Artigo IPEN-doc 27152 Properties and DEFC tests of Nafion2020 - MATOS, B.R.; GOULART, C.A.; TOSCO, B.; SILVA, J.S. da; ISIDORO, R.A.; SANTIAGO, E.I.; LINARDI, M.; SCHADE, U.; PUSKAR, L.; FONSECA, F.C.; TAVARES, A.C.Nafion based composites are promising materials to improve the performance of direct ethanol fuel cells. In this work, composite membranes of Nafion and titanate nanotubes functionalized with sulfonic acid groups were prepared by melt-extrusion and tested in a direct ethanol fuel cell. Far and mid infrared spectroscopies evidenced the formation of ionic bridges between the sulfonic acid groups of both functionalized nanoparticles and the ionomer. Small angle X-ray scattering measurements revealed that the melt-extrusion method leads to an uniform distribution of the inorganic phase in the ionomer matrix. Such structural analysis indicated that the improved the proton conduction properties of the composites, even with the addition of a high concentration of functionalized nanoparticles, are an outcome of the synergistic ionic network due to the hydrid organic/inorganic proton conducting phases. However, an improvement of the fuel cell performance is observed for 2.5 wt% of functionalized titanate nanotubes, which is a result of the lower ethanol crossover and the plasticizing effect of the aliphatic segments of the organic moieties grafted at the surface of the titanate nanoparticles.Dissertação IPEN-doc 26101 Membranas nanoestruturadas de Nafion obtidas por conformação por moldagem assistida por campo elétrico e magnético2019 - SILVA, JAQUELINE de S. daDentre os materiais aplicados como eletrólito em células a combustível de membrana de troca protônica (PEMFC do inglês Proton Exchange Membrane Fuel Cell), os ionômeros perfluorados, como o Nafion, são os mais promissores por possuírem alta condutividade protônica e estabilidade química. A estrutura do Nafion é composta pelo empacotamento eletrostático de agregados poliméricos cilíndricos que possuem maior condutividade protônica ao longo de seu comprimento. Destarte, o alinhamento dos agregados poliméricos do Nafion pode permitir o aumento da condutividade ao longo da espessura do filme, visando o aumento do desempenho da PEMFC. A proposta deste trabalho de mestrado é investigar os mecanismos de polarização do Nafion e aplicar os conhecimentos obtidos para confecção de filmes nanoestruturados por meio da aplicação do campo elétrico e magnético. Para isso, membranas de Nafion com diferentes concentrações de íons foram preparadas por substituição nucleofílica para estudar o mecanismo de polarização e, a partir dos resultados obtidos, membranas de Nafion foram nanoestruturadas por conformação por evaporação em molde (casting) assistido por campo elétrico e magnético. A caracterização da microestrutura e das propriedades elétricas das membranas poliméricas fabricadas foi realizada por meio da espectroscopia vibracional no infravermelho (FTIR), espalhamento de raios X em baixo ângulo (SAXS), espectroscopia de impedância elétrica (EIS) e microscopia de força atômica (AFM). Os resultados obtidos no estudo das membranas com diferentes valores de peso equivalente mostraram que os domínios iônicos do Nafion possuem alta polarizabilidade, a qual permitiu a nanoestruturação de tais domínios pela aplicação de campo elétrico e magnético de baixa intensidade. Os filmes de Nafion conformados pelo método de casting assistido por campo elétrico e magnético revelaram uma estrutura lamelar para o empacotamento dos domínios iônicos. Testes iniciais de células a combustível usando os eletrólitos fabricados por meio da aplicação do campo magnético indicaram um aumento pronunciado do desempenho.Resumo IPEN-doc 25425 Electrostatic interactions of Ionomer Films as Probed by Variable Temperature Synchrotron Infrared Spectroscopy2018 - SILVA, J.S. da; MATOS, B.R.; SCHADE, U.; PUSKAR, L.; FONSECA, F.C.The state of the art polymer electrolyte of Proton Exchange Membrane Fuel Cells (PEM), Nafion®, has poor mechanical and electrical properties at T > 100 °C. Specifically, long-term operation leads to irreversible performance losses that are related to an irreversible modification of the ionomer morphology above the temperature of alpha-transition (Talpha ~ 110 °C). Previous characterizations showed that the alpha-transition is dependent on the different states of covalent and ionic interactions among sulfonic acid groups, such as: ionic repulsions among RSO3-, dipolar attractions among RSO3H dipoles, hydrogen bonding of sulfonic groups with bulk and coordinated water molecules. The identification of both the functional groups interactions in the MIR bands and the “ion-hopping bands” in the FIR bands for annealed Nafion samples can give new insights into the role played by the ionic interactions on the alpha of ionomer membranes. Such approach for understanding the relationship between the dynamics of aplha-relaxation and Nafion morphology is missing in the literature, possibly due to the incipient number of FIR studies of Nafion. The central objective of this work is to advance the understanding of the chemical features involved during the aplha-transition of in situ annealed Nafion membranes with the high-resolution mid (MIR) and far (FIR) infrared spectroscopy using the IRIS beamline of BESSY II synchrotron light source. Herein, the effect of short-term annealing of Nafion at RH ~ 0% and selected temperatures below and above the alphatransition is presented. The comparison between SAXS and FTIR data of Nafion membranes annealed in situ revealed that the alpha-transition is due to the long range motion of the ionomer chains via weakening of electrostatic interactions of the ionomer functional groups.Resumo IPEN-doc 23626 Properties and defc tests of nafion added functionalized titanate nanotubes prepared by extrusion2016 - MATOS, B.R.; GOULART, C.A.; ISIDORO, R.A.; SILVA, J.S. da; SANTIAGO, E.I.; FONSECA, F.C.; TAVARES, A.C.Composite electrolyte membranes based on the incorporation of a second inorganic phase into ionomer matrices such as Nafion revealed to possess enhanced properties such as increased mechanical resistance and reduced permeability of solvents. It has been reported that surface functionalized titanate nanotubes (H2Ti3O7.nH2O) display a proton conductivity of ~ 10-2 Scm-1, which is attractive for the use of such composites in direct ethanol fuel cells (DEFC). Herein, composite membranes based on the addition of sulfonic acid groups functionalized titanate nanotubes into Nafion matrix were prepared by grafting followed by extrusion. These membranes were characterized by infrared spectroscopy (FTIR), Brunauer–Emmett–Teller (BET), acid-base titration, proton conductivity measurements and DEFC tests. FTIR measurements confirmed both the grafting of the titanate nanotubes. BET measurements showed that the functionalized titanate nanotubes possess a high surface specific area. Acid-base titration evidenced that additional sulfonic acid groups are present in the composite membranes compared to the pristine ionomer. The conductivity measurements show that the increase in the titanate nanotube volume fraction into the ionomers has not resulted in a decrease of the proton conductivity. The results show that the addition of functionalized titanate nanotubes into Nafion polymer matrix resulted in an improvement of the electric transport properties, reduction of the fuel crossover and, consequently, a higher DEFC performance for the composites were observed with respect to the pristine Nafion.