JAQUELINE DE SOUZA DA SILVA
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Artigo IPEN-doc 27193 SAXS signature of the lamellar ordering of ionic domains of perfluorinated sulfonic-acid ionomers by electric and magnetic field-assisted casting2020 - SILVA, JAQUELINE S. da; CARVALHO, SABRINA G.M.; SILVA, RODRIGO P. da; TAVARES, ANA C.; SCHADE, ULRICH; PUSKAR, LJILJANA; FONSECA, FABIO C.; MATOS, BRUNO R.At present, small angle X-ray scattering (SAXS) studies of perfluorinated sulfonic-acid ionomers (PFSAs) are unable to fully determine the true shape of their building blocks, as recent SAXS modelling predicts disk- and rod-like nanoionic domains as being equally possible. This scenario requires evidence-based findings to unravel the real shape of PFSA building blocks. Herein, a SAXS pattern signature for a lamellar nanophase separation of the ionic domains of Nafion is presented, backed by mid and far infrared spectroscopy (MIR and FIR) and wide angle X-ray scattering (WAXS) data of Nafion in different ionic forms, a broad range of ionic phase contents (EW ~ 859–42 252 g eq-1) and temperatures. The study indicates that the lamellar arrangement of the ionic domains is the most representative morphology that accounts for the physical properties of this ionomer. The lamellar SAXS reflections of Nafion are enhanced in electric and magnetic field-aligned membranes, as confirmed by atomic force microscopy (AFM). Electric and magnetic field-assisted casting of Nafion allowed producing nanostructured and anisotropic films with the lamellas stacked perpendicularly to the field vector, which is the direction of interest for several applications. Such nanostructured Nafion membranes are bestowed with advanced optical and proton transport properties, making them promising materials for solar and fuel cells.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 23728 Structure and transport properties of annealed nafion membranes2016 - MATOS, BRUNO R.; SILVA, JAQUELINE de S. da; FONSECA, FABIO C.The relationship between electrical properties and the structural features of annealed Nafion samples was investigated by X-ray diffraction (XRD), small angle X-ray scattering (SAXS), scanning electron microscopy (SEM), and impedance spectroscopy. Understanding of the observed effects on the proton conductivity due to annealing at controlled humidity at high temperature is crucial for improving the polymer electrolyte fuel cell (PEFC) at high operating temperatures (T > 100 °C) [1]. The experimental results reveal that membranes submitted to a heat treatment in the 100 – 200 °C temperature interval at low relative humidity (RH), display higher crystallinity and irreversibly shrinking of the ionic domains. However, the electrical properties of the polymer matrix were mostly affected by the irreversible destabilization of the ionic phase. The increase in crystallinity and shrinking of the hydrophilic domains reduce the ionomer conductivity. These features were reflected in the polymer electrolyte fuel cell (PEFC) tests in which the measured performance was lower for Nafion samples annealed at high T compared to pristine membranes. Such results are relevant for the preparation of membrane electrode assemblies as well as for the development of highperformance ionomer membranes.