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M.Sc. (Physics) / Please refer to full text to view abstract

Thesis (M.Sc.)--Memorial University of Newfoundland, 1992. / Typescript. Bibliography: leaves 140-157. Also available online.

Progischrift--Amsterdam. / Includes bibliographical references.

Progischrift--Amsterdam. / Bibliographical foot-notes.

[pt] Em 1990, com a adoção da Escala Internacional de Temperatura de 1990, o termopar de platina e platina/ródio deixou de ser o instrumento de interpolação entre 630 graus Celsius e 1064 graus Celsius, em virtude de sua pouca estabilidade, sendo a partir daí utilizados o termômetro de resistência de platina de alta temperatura (TRPAT) e o termômetro de radiação. Este estudo realiza uma investigação prática das características de um termopar de ouro e platina, ambos com pureza superior a 99,999 por cento, no que diz respeito à sua estabilidade termoelétrica e à homogeneidade de seus termoelementos, questionando a possibilidade de seu uso como alternativa ao emprego do TRPAT em processos de medição que exijam grande exatidão com custo mais baixo. Neste trabalho, o termopar estudado foi submetido a temperaturas próximas ao seu limite máximo de operação, que é de 1000 graus Celsius, por mais de 1500 horas, sendo avaliadas a sua estabilidade e a sua homogeneidade em função do tempo de uso, com o auxílio de uma célula de ponto fixo da prata do Inmetro, que é um padrão primário de temperatura. / [en] In 1990, with the adoption of the International Temperature Scale of 1990, the platinum/platinum-rhodium thermocouple was removed as the interpolation instrument between 630 graus Celsius and 1064 Celsius degrees, due its low stability, in favor of the high temperature standard platinum resistance thermometer (HTSPRT) and the radiation thermometer. In this work, it is performed a practical investigation of the characteristics of a 99,999 percent purity gold-platinum thermocouple, concerning its thermoelectric stability and homogeneity of its thermoelements, questioning the possibility of its use as an alternative to the HTSPRT in measurement processes requiring high accuracy with lower costs. In this work, the test thermocouple was exposed to temperatures close to its upper limit (1000 Celsius degrees) for more than 1500 hours, being its stability and homogeneity evaluated as function of time, with aid of a silver fixed point cell from Inmetro, that is a temperature primary standard.

Une méthode de dépôt de platine sur or a récemment été développée. Le substrat est, dans une première phase, modifié par un dépôt d’un métal moins noble que le platine, tel que le cuivre ou le plomb. Ce dépôt métallique est, dans une seconde phase, mis en contact avec une solution de sel de platine et la substitution spontanée du cuivre ou du plomb par du platine métallique se produit.<p><p>\ / Doctorat en Sciences / info:eu-repo/semantics/nonPublished

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Porous, conductive metallic nanostructures are required in several fields, such as energy conversion, low-cost sensors etc. This thesis reports on the development of an electrocatalytically active and conductive membrane for use in Polymer Electrolyte Membrane Fuel Cells (PEMFCs) and fabrication of low-cost substrates for Surface Enhanced Raman Spectroscopy (SERS). One of the main challenges facing large-scale deployment of PEMFCs currently is to fabricate a catalyst layer that minimizes platinum loading, maximizes eletrocatalytically active area, and maximizes tolerance to CO in the feed stream. Modeling the kinetics of platinum catalyzed half cell reactions occurring in a PEMFC using the kinetic theory of gases and incorporating appropriate sticking coefficients provides a revealing insight that there is scope for an order of magnitude increase in maximum current density achievable from PEMFCs. To accomplish this, losses due to concentration polarization in gas diffusion layers, which occur at high current densities, need to be eliminated. A novel catalyst design, based on a porous metallic nanostructure, which aims to overcome the limitations of concentration polarization as well as minimize the amount of platinum loading in PEMFCs is proposed. Fabrication steps involving controlled in-plane fusion of self-assembled arrays of core-shell gold-platinum nanoparticles (Au@Pt) is envisioned. The key steps involved being the development of a facile synthesis route to form Au@Pt nanoparticles with tunable platinum shell thicknesses in the 5 nm size range, the formation of large-scale 2D arrays of Au@Pt nanoparticles using guided self-assembly, and optimization of an RF plasma process to promote in-plane fusion of the nanoparticles to form porous, electrocatalytically active and electrically conductive membranes. This thesis consists of seven chapters. The first chapter provides an introduction into the topic of PEMFCs, some perspective on the current status of research and development of PEMFCs, and an outline of the thesis. The second chapter provides an overview on the methods used, characterization techniques employed and protocols followed for sample preparation. The third chapter describes the modelling of a PEMFC using the Kinetic theory of gases to arrive at an estimate of the maximum feasible current density, based on the kinetics of the electrocatalytic reactions. The fourth chapter presents the development of a simple protocol for synthesizing Au@Pt nanoparticles with control over platinum shell thicknesses from the sub monolayer coverage onwards. The results of spectroscopic and microscopic characterization establish the uniformity of coating and the absence of secondary nucleation. Chapter five describes the formation of a nanoporous, electrocatalytically active membrane by self-assembly to form bilayers of 2D arrays of Au@Pt nanoparticles and subsequent fusion using an RF plasma based process. The evolution of the electrocatalytic activity and electrical conductivity as a function of the duration of RF plasma treatment is monitored for Au@Pt nanoparticles with various extent of platinum coating. Spectroscopic, microscopic, electrical and cyclic voltammetry characterization of the samples at various stages were used to understand the structural evolution with RF plasma treatment duration and discussed. Next durability studies were carried out on the nanoporous, Au@Pt bilayer nanoparticle array with an optimum composition of Pt/Au atomic ratio of 0.88 treated to 16 minutes of argon plasma exposure. After this the novel catalyst membrane design of PEM fuel cell is revisited. Two different techniques are proposed so that the thin, nanoporous, metallic catalyst membrane achieves horizontal electronic resistance equivalent to that of the conventional gas diffusion layer with catalyst layer. The first technique proposes the introduction of gold coated polymeric mesh in between the thin, nanoporous, metallic catalyst membrane and bipolar plate and discusses the advantages. Later the gold coated polymeric mesh is introduced in a conventional membrane electrode assembly and efficiency of the polarization curves probed with and without the introduction of gold coated polymeric mesh. The second technique describes the results of fabrication of a nanoporous metallic membrane using multiple layers of 2D Au@Pt nanoparticle arrays at an optimum composition of Pt/Au atomic ratio of 0.88 to reduce the horizontal electronic resistance. Preliminary studies on the permeability of water through such membranes supported on a porous polycarbonate filter membrane are also presented. In chapter six, a simple reactive inkjet printing process for fabricating SERS active silver nanostructures on paper is presented. The process adapts a simple room temperature protocol, using tannic acid as the reducing agent, developed earlier in our group to fabricate porous silver nanostructures on paper using a commercial office inkjet printer. The results of SERS characterization, spectroscopic and microscopic characterizations of the samples and the comparison of the substrate’s long-term performance with respect to a substrate fabricated using sodium borohydride as the reducing agent is discussed. Preliminary findings on attempts to fabricate a conductive silver network using RF plasma induced fusion area also presented. Chapter seven provides a summary of the results, draws conclusions and a perspective on work required to accomplish the goals of incorporating the porous metallic nanostructures into PEMFCs.