Processo de conversão química da liga de alumínio 2024-T3 de aplicação aeronáutica

A presente tese teve por base o estudo da conversão química da liga de alumínio 2024T3 de aplicação aeronáutica. O trabalho experimental foi desenvolvido na OGMA, Indústria Aeronáutica de Portugal S.A., durante o período de, aproximadamente 1 ano, que coincidiu com a realização de um estágio profissional nesta empresa por parte da mestranda. A referida empresa, tem como actividade a prestação de serviços de Manutenção, Revisão, Modernização, de Aeronaves, Motores e Componentes, Fabricação e Montagem de Estruturas. Integrada na OGMA, encontra-se a área de tratamentos electroquímicos, TE’S, na qual são realizados serviços de manutenção de material aeronáutico e de peças de fabricação. Estes serviços baseiam-se em processos de electrodeposição e conversão química. De modo a garantir um controlo de qualidade e correcto funcionamento dos diversos processos existe, inserido na área TE’S, um laboratório químico. O presente trabalho experimental, realizado na área TE’S, assenta no processo de conversão química, por imersão, de provetes da liga Al 2024-T3, referente a todos os contratos da OGMA. Estes contratos possuem especificações para aplicação do revestimento de conversão química, por imersão, em alumínio e suas ligas. Estas especificações incluem requisitos de qualidade, nos quais se encontra inserido o controlo periódico do processo. Deste modo, o processo é sujeito a um controlo periódico mensal que consiste na avaliação da qualidade dos tratamentos. A qualidade dos revestimentos obtidos, por conversão química, é assegurada através da avaliação dos resultados dos ensaios aos provetes. O estudo experimental desenvolvido focou-se nos ensaios de resistência à corrosão (nevoeiro salino) requeridos nos contratos. O intuito de realizar um estudo sobre o processo de conversão química por imersão de provetes da liga Al 2024 T3 e subsequente foco no ensaio de resistência à corrosão (nevoeiro salino), assenta no facto de ter-se vindo a observar, nos últimos anos, corrosão por pitting em vários lotes destes provetes, após serem sujeitos às sequências de processo de conversão química e antes de perfazerem a totalidade de 168 horas na câmara de nevoeiro salino, não superando este critério de qualidade do revestimento. Na perspectiva de colmatar a referida situação, procedeu-se à realização de ensaios de despiste nos provetes representativos da liga, com especial incidência na variação dos intervalos de tempo de imersão, pré-estabelecidos pelas especificações aplicáveis, e observação do seu comportamento quando sujeitos ao ensaio de nevoeiro salino.

Emissions of nanoparticles during friction stir welding (FSW) of aluminium alloys

Friction stir welding (FSW) is now well established as a welding process capable of joining some different types of metallic materials, as it was (1) found to be a reliable and economical way of producing high quality welds, and (2) considered a "clean" welding process that does not involve fusion of metal, as is the case with other traditional welding processes. The aim of this study was to determine whether the emission of particles during FSW in the nanorange of the most commonly used aluminum (Al) alloys, AA 5083 and AA 6082, originated from the Al alloy itself due to friction of the welding tool against the item that was being welded. Another goal was to measure Al alloys in the alveolar deposited surface area during FSW. Nanoparticles dimensions were predominantly in the 40- and 70-nm range. This study demonstrated that microparticles were also emitted during FSW but due to tool wear. However, the biological relevance and toxic manifestations of these microparticles remain to be determined.

Anti-Corrosion performance of a new silane coating for corrosion protection of AZ31 Magnesium alloy in Hank’s solution

Mg alloys can be used as bioresorsable metallic implants. However, the high corrosion rate of magnesium alloys has limited their biomedical applications. Although Mg ions are essential to the human body, an excess may cause undesirable health effects. Therefore, surface treatments are required to enhance the corrosion resistance of magnesium parts, decreasing its rate to biocompatible levels and allowing its safe application as bioresorbable metallic implants. The application of biocompatible silane coatings is envisaged as a suitable strategy for retarding the corrosion process of magnesium alloys. In the current work, a new glycidoxypropyltrimethoxysilane (GPTMS) based coating was tested on AZ31 magnesium substrates subjected to different surface conditioning procedures before coating deposition. The surface conditioning included a short etching with hydrofluoric acid (HF) or a dc polarisation in alkaline electrolyte. The silane coated samples were immersed in Hank's solution and the protective performance of the coating was studied through electrochemical impedance spectroscopy (EIS). The EIS data was treated by new equivalent circuit models and the results revealed that the surface conditioning process plays a key role in the effectiveness of the silane coating. The HF treated samples led to the highest impedance values and delayed the coating degradation, compared to the mechanically polished samples or to those submitted to dc polarisation.

"In-vitro" corrosion behaviour of the magnesium alloy with Al and Zn (AZ31) protected with a biodegradable polycaprolactone coating loaded with hydroxyapatite and cephalexin

Mg alloys are very susceptible to corrosion in physiological media. This behaviour limits its widespread use in biomedical applications as bioresorbable implants, but it can be controlled by applying protective coatings. On one hand, coatings must delay and control the degradation process of the bare alloy and, on the other hand, they must be functional and biocompatible. In this study a biocompatible polycaprolactone (PCL) coating was functionalised with nano hydroxyapatite (HA) particles for enhanced biocompatibility and with an antibiotic, cephalexin, for anti-bacterial purposes and applied on the AZ31 alloy. The chemical composition and the surface morphology of the coated samples, before and after the corrosion tests, were studied by scanning electron microscopy (SEM) coupled with energy dispersive x-ray analysis (EDX) and Raman. The results showed that the presence of additives induced the formation of agglomerates and defects in the coating that resulted in the formation of pores during immersion in Hanks' solution. The corrosion resistance of the coated samples was studied in Hank's solution by electrochemical impedance spectroscopy (EIS). The results evidenced that all the coatings can provide corrosion protection of the bare alloy. However, in the presence of the additives, corrosion protection decreased. The wetting behaviour of the coating was evaluated by the static contact angle method and it was found that the presence of both hydroxyapatite and cephalexin increased the hydrophilic behaviour of the surface. The results showed that it is possible to tailor a composite coating that can store an antibiotic and nano hydroxyapatite particles, while allowing to control the in-vitro corrosion degradation of the bioresorbable Mg alloy AZ31. (C) 2015 Elsevier Ltd. All rights reserved.

Biofunctional composite coating architectures based on polycaprolactone and nanohydroxyapatite for controlled corrosion activity and enhanced biocompatibility of magnesium AZ31 alloy

In this work a biofunctional composite coating architecture for controlled corrosion activity and enhanced cellular adhesion of AZ31 Mg alloys is proposed. The composite coating consists of a polycaprolactone (PCL) matrix modified with nanohydroxyapatite (HA) applied over a nanometric layer of polyetherimide (PEI). The protective properties of the coating were studied by electrochemical impedance spectroscopy (EIS), a non-disturbing technique, and the coating morphology was investigated by field emission scanning electron microscopy (FE-SEM). The results show that the composite coating protects the AZ31 substrate. The barrier properties of the coating can be optimized by changing the PCL concentration. The presence of nanohydroxyapatite particles influences the coating morphology and decreases the corrosion resistance. The biocompatibility was assessed by studying the response of osteoblastic cells on coated samples through resazurin assay, confocal laser scanning microscopy (CLSM) and scanning electron microscopy (SEM). The results show that the polycaprolactone to hydroxyapatite ratio affects the cell behavior and that the presence of hydroxyapatite induces high osteoblastic differentiation. (C) 2014 Elsevier B.V. All rights reserved.