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Niobium is well known for its excellent corrosion resistance based on the formation of a stable passive oxide layer, which protects the metal against corrosion in most aqueous media and makes it an interesting candidate for corrosion resistant coating applications. However, deposition of Nb films is restricted to few technologies and difficulties arise from the toxic nature of the electrolytes employed in electrodeposition of Nb, the high reactivity of the metal with residual gases in vacuum plasma spraying and its high melting point (Tm = 2500 0C) in PVD deposition. The present thesis describes the development of corrosion resistant Nb coatings on stainless steel and brass substrates by the combined steered arc/unbalanced magnetron sputtering technique. Evaluation of the corrosion behaviour is performed by potentiodynamic polarisation measurements in 3% NaCl. It is shown that corrosion resistant Nb coatings, with passivation characteristics similar to that of bulk Nb, can be produced on stainless steel substrates by unbalanced magnetron sputtering at a low deposition temperature (T = 250 0C) under reduced ion bombardment. However, the ion etching pre-treatment of the substrate prior to deposition has a significant influence on the corrosion resistance of the coating/substrate system. The employed polarisation measurements reveal that a fully passive and protective behaviour could only be achieved if Nb ions from the cathodic arc source are chosen as the etching species. In contrast, coatings deposited after Cr ion etching from the arc source and inert Ar ion etching, utilising a glow discharge, exhibit localised breakdown and pitting of the substrate. Cross sectional TEM imaging and STEM-EDX analyses reveal that bombardment of the stainless steel substrate by the multiply charged Nb ions generates a compositionally intermixed, very fine crystalline or "amorphised" interface layer, with a thickness of ~3-8nm, depending on the Nb ion energy. It is proposed that this layer acts as an additional barrier against corrosion due to (i) the structural homogeneity achieved by amorphisation and (ii) chemical stabilisation due to the introduction of Nb in the near surface region. The energy of the bombarding Nb ions, i.e. the substrate bias voltage during the etching stage, was found to further influence the corrosion resistance. Best results are achieved with "medium" bias voltages in the range of -600V to -800V, which is believed to be due to an optimum combination of structural and chemical protection mechanisms. The fully passive corrosion behaviour could not be observed in the case of brass substrates. However, the PVD coating systems on brass and on stainless steel are superior, in the employed polarisation measurements, to commercially produced, electroplated Cr, Ni and Ni/Cr coatings on the same substrate materials. Other coating properties investigated in the present study include microstructure, hardness, crystallographic orientation and residual film stresses.

No / This paper investigates the sliding wear performance of two types of co-electrodeposited cermet coatings com- posed of nano-sized tungsten carbide (WC) and combined tungsten carbide and alumina (Al2O3) particles incor- porated in a nickel matrix. For this purpose, the effects of alternating the ceramic particle concentration in the electrolyte solutions on microhardness of the coatings and also the effect of applied loads on wear performance of the coatings have been studied using ball-on-flat sliding wear tests. The wear track volumes and the progres- sion of wear depths as a function of time and at three applied loads were recorded and wear track morphologies were investigated using FE-SEM and microhardness testing. The results showed that microstructure, microhard- ness and wear performance of the coatings composed of WC improved when Al2O3 particles were introduced into the matrix. It was also found that the rule of mixtures for composite materials provides a good explanation for microhardness behaviour while Archard equation can explain the changes in wear performance due to the hardness and microstructural changes. / Alberta Innovates Future Technologies (Nanoworks) Canada

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Submitted by FERNANDO SANTOS DA SILVA null (fernandoquimicauems@hotmail.com) on 2017-09-28T02:21:06Z No. of bitstreams: 1 Tese_Fernando_Santos_da_Silva_IQ_UNESP.pdf: 19317124 bytes, checksum: b4f79b295bc22505ca8f3f01bd3db519 (MD5) / Approved for entry into archive by Monique Sasaki (sayumi_sasaki@hotmail.com) on 2017-09-28T14:59:57Z (GMT) No. of bitstreams: 1 silva_fs_dr_araiq.pdf: 19317124 bytes, checksum: b4f79b295bc22505ca8f3f01bd3db519 (MD5) / Made available in DSpace on 2017-09-28T14:59:57Z (GMT). No. of bitstreams: 1 silva_fs_dr_araiq.pdf: 19317124 bytes, checksum: b4f79b295bc22505ca8f3f01bd3db519 (MD5) Previous issue date: 2017-09-15 / Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) / Este trabalho teve como objetivo investigar a microestrutura, resistência à corrosão e propriedades mecânicas de revestimentos produzidos por Aspersão Fria (AF) a base de: (I) pó de alumínio (Al), com ou sem alumina (Al2O3), depositados sobre aço comum; (II) revestimentos metálico-cerâmicos de WC-12Co e WC-25Co depositados sobre a liga Al7075-T6 e (III) revestimentos de cobre depositados sobre aço e obtidos a partir de pós submetidos a diferentes tratamentos. A análise dos materiais de partida e dos revestimentos, antes e após os ensaios de corrosão, foi realizada por difração a laser (DL), microscopia óptica (OM), microscopia eletrônica de varredura (SEM) acoplado a um sistema de espectroscopia de dispersão de energia de raios X (EDS) e difração de raios X (DRX). Foram realizadas medidas de dureza e ensaios de resistência ao desgaste por abrasão (Rubber Wheel) e por deslizamento (Ball on disk). A resistência à corrosão dos revestimentos foi avaliada por medidas eletroquímicas em meio de NaCl 3,5% e testes de névoa salina. Foram realizadas medidas de potencial em circuito aberto (ECA), espectroscopia de impedância eletroquímica (EIS) e curvas de polarização linear e cíclica. As imagens de SEM da secção transversal mostram que os revestimentos são densos, não possuem porosidade interconectada e nem trincas. Os resultados eletroquímicos e de névoa salina mostram que todos os revestimentos investigados protegem o substrato por longos tempos de imersão por serem compactos quando obtidos pela tecnologia de AF. Para os revestimentos a base de alumínio, os estudos mostram que o eletrólito atinge o substrato em alguns pontos somente após 2000 h de imersão e os ensaios de desgaste indicam que o revestimento compósito Al-Al2O3 apresenta melhores propriedades mecânicas. Quanto aos revestimentos metálicocerâmicos, o revestimento de WC-25Co apresentou maior espessura e também maior proteção contra corrosão até tempos maiores do que 2000 h. A caracterização dos revestimentos de cobre mostra claramente que os diferentes tratamentos dos materiais de partida exercem influência na eficiência de deposição, formação dos revestimentos e principalmente na sua resistência à corrosão. / The purpose of this work was to investigate the microstructure, corrosion resistance and mechanical properties of coatings prepared by Cold Gas Spray (CGS) based on: (I) aluminum (Al) powder with or without alumina (Al2O3), deposited on common steel; (II) WC-12Co and WC-25Co metallic-ceramic coatings deposited onto Al7075- T6 alloy and (III) copper coatings deposited onto common steel and obtained from powders submitted to different treatments. The analysis of the feedstock materials and the coatings before and after the corrosion tests were performed by laser diffraction (LD), optical microscopy (OM), scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy system (EDS) and X-ray diffraction (XRD). Hardness measurements, abrasion testing (Rubber Wheel) and sliding wear test (Ball on disk) were performed. The corrosion resistance of the coatings was evaluated by electrochemical measurements in 3.5% NaCl medium, and salt fog tests. Open circuit potential (EOC), electrochemical impedance spectroscopy (EIS), linear and cyclic polarization measurements were performed. SEM images of the cross section showed that coatings are dense, without interconnected porosity and cracks. Electrochemical and salt fog results show that all investigated coatings protect the substrate during long immersion times because they are compact when obtained by CGS technology. For the aluminum based coatings, the studies show that the electrolyte reaches the substrate at some points only after 2000 h of immersion and the wear tests show that the Al-Al2O3 composite coating has better mechanical properties. For the metal-ceramic coatings, the WC-25Co coating show higher thickness and corrosion protection up to 2000 h of immersion when compared to WC-12Co. Copper coatings characterization clearly shows that the different treatments of the feedstock materials exert influence on the deposition efficiency, coating formation and especially on their corrosion resistance. / CNPq: 153177/2014-4

<p>With the extreme increases in power density of electronic devices, the contact thermal resistance imposed at interfaces between mating solids becomes a major challenge in thermal management. This contact thermal resistance is mainly caused by micro-scale surface asperities (roughness) and wavy profile of surface (nonflatness) which severely reduce the contact area available for heat conduction. High contact pressures (1~100 MPa) can be used to deform the surface asperities to increase contact area. Besides, a variety of conventional thermal interface materials (TIM), such as greases and pastes, are used to improve the contact thermal conductance by filling the remaining air gaps. However, there are still some applications where such TIMs are disallowed for reworkability concerns. For example, heat must be transferred across dry interfaces to a heat sink in pluggable opto-electronic transceivers which needs to repeatedly slide into / out of contact with the heat sink. Dry contact and low contact pressures are required for this sliding application.</p> <p>This dissertation presents a metallized micro-spring array as a surface coating to enhance dry contact thermal conductance under ultra-low interfacial contact pressure. The shape of the micro-springs is designed to be mechanically compliant to achieve conformal contact between nonflat surfaces. The polymer scaffolds of the micro-structured TIMs are fabricated by using a custom projection micro-stereolithography (μSL) system. By applying the projection scheme, this method is more cost-effective and high-throughput than other 3D micro-fabrication methods using a scanning scheme. The thermal conductance of polymer micro-springs is further enhanced by metallization using plating and surface polishing on their top surfaces. The measured mechanical compliance of TIMs indicates that they can deform ~10s μm under ~10s kPa contact pressures over their footprint area, which is large enough to accommodate most of surface nonflatness of electronic packages. The measured thermal resistances of the TIM at different fabrication stages confirms the enhanced thermal conductance by applying metallization and surface polishing. Thermal resistances of the TIMs are compared to direct metal-to-metal contact thermal resistance for flat and nonflat mating surfaces, which confirms that the TIM outperforms direct contact. A thin layer of soft polymer is coated on the top surfaces of the TIMs to accommodate surface roughness that has a smaller spatial period than the micro-springs. For rough surfaces, the polymer-coated TIM has reduced thermal resistance which is comparable to a benchmark case where the top surfaces of the TIM are glued to the mating surface. A polymer base is designed under the micro-spring array which can provide the advantages for handling as a standalone material or integration convenience, at the toll of an increased insertion resistance. Through-holes are designed in the base layer and coated with thermally conductive metal after metallization to enhance thermal conductance of the base layer; a thin layer of epoxy is applied between the base layer and the working surface to reduce contact thermal resistance exposed on the base layer. Cycling tests are conducted on the TIMs; the results show good early-stage reliability of the TIM under normal pressure, sliding contact, and temperature cycles. The TIM is thermally demonstrated on a pluggable application, namely, a CFP4 module, which shows enhanced thermal conductance by applying the TIM. </p> To further enhance the potential mechanical compliance of microstructured surfaces, a stable double curved beam structure with near-zero stiffness composed of intrinsic negative and positive stiffness elastic elements is designed and fabricated by introducing residual stresses. Stiffness measurements shows that the positive-stiffness single curved beam, which is the same as the top beam in the double curved beam, is stiffer than the double curved beam, which confirms the negative stiffness of the bottom beam in the double curved beam. Layered near zero-stiffness materials made of these structures are built to demonstrate the scalability of the zero-stiffness zone.