MARIANA XAVIER MILAGRE

MARIANA XAVIER MILAGRE

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Investigação da atividade eletroquímica de liga Al-Cu-Li após processo de soldagem por fricção e mistura
2023 - SILVA, REJANE M.P. da; MILAGRE, MARIANA X.; ARAUJO, JOAO V. de S.; RAMIREZ, OSCAR M.P.; MACHADO, CARULINE de S.C.; ANTUNES, RENATO A.; COSTA, ISOLDA
In this work, the local electrochemical activity of the zones coupled by Friction Stir Welding (FSW) of an Al-Cu-Li alloy was studied and the results were correlated to the microstructural characteristics of each zone. Electrochemical studies were carried out in the zones affected by welding using cyclic voltammetry (CV) and scanning electrochemical techniques (namely, SECM - Scanning Electrochemical Microscopy and LEIS – Local electrochemical impedance spectroscopy). The results showed that the welding joint (WJ) is predominantly cathodic relatively to the heat affected zones (HAZ). The HAZ was always anodic and showed the highest electrochemical activities among the tested ones. The high electrochemical activity of the HAZ was associated with the effect of galvanic coupling between the cathodic region (WJ) and the anodic region (HAZ). In addition, the advancing side (AS) presented increased electrochemical activity compared to the retreating one (RS).
Surface finishing effects on the corrosion behavior and electrochemical activity of 2098-T351 aluminum alloy investigated using scanning microelectrochemical techniques
2022 - SILVA, REJANE M.P. da; MILAGRE, MARIANA X.; IZQUIERDO, JAVIER; BETANCOR-ABREU, ABENCHARA M.; OLIVEIRA, LEANDRO A. de; ARAUJO, JOAO V. de S.; ANTUNES, RENATO A.; SOUTO, RICARDO M.; COSTA, ISOLDA
The effects of surface finishing on the corrosion behavior and electrochemical activity of AA2098-T351 (Al–Cu–Li alloy) were investigated on the basis of the correlation between surface chemistry, microstructure and electrochemical activity. The alloy was evaluated in the as-received and polished conditions. The morphology of the two types of surfaces was investigated using confocal laser scanning microscopy (CLSM), optical microscopy and optical 3D profilometry. The surface chemistry was analyzed by X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDX). Scanning microelectrochemical techniques (namely, localized electrochemical impedance spectroscopy (LEIS), the scanning vibrating electrode technique (SVET) and scanning electrochemical microscopy (SECM) in potentiometric mode) were used to examine the electrochemical activity of the surfaces. The results showed that on the as-received surface, the near surface deformed layer (NSDL), which is composed of Mg-rich bands, influenced the corrosion activity of the alloy. Higher electrochemical activity and greater susceptibility to severe localized corrosion were related to the polished surface condition compared to the as-received one.
Electrochemical characterization of alloy segregation in the near-surface deformed layer of welded zones of an Al-Cu-Li alloy using scanning electrochemical microscopy
2022 - SILVA, REJANE M.P. da; IZQUIERDO, JAVIER; MILAGRE, MARIANA X.; ARAUJO, JOAO V. de S.; ANTUNES, RENATO A.; SOUTO, RICARDO M.; COSTA, ISOLDA
The development of heterogeneous electrochemical activity in the welded zones of aluminum alloy 2098-T351 by friction stir welding (FSW) associated with the formation of a near-surface deformed layer (NSDL) upon exposure to an aqueous chloride-containing solution was characterized using scanning electrochemical microscopy (SECM) in potentiometric operation. A solid-contact Mg2+ ion-selective microelectrode allowed in situ monitoring of the corrosion reactions sites for magnesium dissolution from different zones of the FSW weld upon exposure to a chloride-containing aqueous environment. In this way, localized corrosion reactions developing in the galvanically coupled joint/heat affected zones (WJ/HAZ) of the weld were detected and imaged with spatial resolution. The most active domains for local Mg2+ concentrations were associated with the HAZ of the retreating side (RS), and these corresponded to Mg oxidation from the Mg-enriched oxide bands in NSDL.
Corrosion behaviour of the 2098-T351 Al–Cu–Li alloy after different surface treatments
2022 - BARBOZA, WANESSA das G.; MILAGRE, MARIANA X.; DONATUS, UYIME; MACHADO, CARULINE de S.C.; RAMIREZ, OSCAR M.P.; ARAUJO, JOAO V. de S.; SILVA, REJANE M.P. da; COSTA, ISOLDA
The effect of different surface treatments on the corrosion resistance of the AA2098 Al–Cu–Li alloy has been investigated. Surface characterization was performed using 3D optical profilometry, energy dispersive X-ray spectroscopy and scanning electron microscopy. The corrosion resistance of the 2098 alloy after the surface treatments was investigated in 0.1 mol L−1 NaCl solution by electrochemical techniques and microscopy. Corrosion results showed that the untreated and the chemically etched surfaces were more active than the mechanically abraded and mechanically polished surfaces owing to differences in the nature of the native oxides formed after the surface treatments. Corrosion rate and mode were also affected by how close the exposed surface was to the mid-thickness region of the AA2098-T351 plate relative to the actual top surface (before polishing). This is associated with the variation in the volume fraction and distribution of the T1 phase as the mid-thickness region of the AA2098-T351 plate is approached.
Compreendendo os mecanismos de corrosão de ligas de Al-Cu-Li
2022 - ARAUJO, JOAO V. de S.; SILVA, REJANE M.P. da; VIVEIROS, BARBARA V.; MILAGRE, MARIANA X.; MACHADO, CARULINE de S.C.; COSTA, ISOLDA
In this study, the corrosion mechanism of an Al-Cu-Li alloy manufactured by two different treatment routes (T3 and T851) was evaluated by immersion and electrochemical tests in solutions containing chloride ions (Cl-). For both alloys, the formation of cavities on the surface was associated with micrometer-sized intermetallics (IM’s), however, in addition to this attack, the alloy submitted to T851 treatment also presented an attack called severe localized corrosion (SLC), caused by the preferential attack to the nanometric T1 (Al2CuLi) phase. The electrochemical concepts involved in these two types of attacks were discussed. During the IM’s corrosive process, whereas the O2 reduction occurred over the IM’s, the Al dissolution is favored around the particle, forming trenching and cavities (with 2 and 6 mm of depth). On the other hand, the mechanism associated with the SLC is related to the formation of a differential aeration cell followed by the evolution of H2, with greater depth of attack penetration (8 and 35 mm). Additionally, by the use of the Scanning Vibrating Electrode Technique (SVET), it was concluded that the higher anodic currents observed for the T851 temper were related to the relation between the anodic area (Aa) and the cathodic area (Ac).
Development of an Al3+ ion-selective microelectrode for the potentiometric microelectrochemical monitoring of corrosion sites on 2098-T351 aluminum alloy surfaces
2022 - SILVA, REJANE M.P. da; IZQUIERDO, JAVIER; MILAGRE, MARIANA X.; ANTUNES, RENATO A.; SOUTO, RICARDO M.; COSTA, ISOLDA
A novel potentiometric Al3+−ion selective microelectrode (ISME), with internal solid contact, based on the use of a neutral carrier morin as ionophore is reported. The ability of the ISME to image local ion concentration distributions was tested on aluminum alloy surfaces freely corroding in an aqueous solution containing chloride ions. The microelectrode was then used as the sensing tip for scanning electrochemical microscopy (SECM) in potentiometric operation to monitor the reactive sites associated with the dissolution of aluminum that developed in the 2098−T351 Al−Cu−Li alloy as a result of welding by the Friction Stir Welding (FSW) process. The ISME detected differences in the local concentrations of Al3+ species arising from the 2098−T351 Al−Cu−Li alloy (base material) and from the coupled weld joint/heat affected zones (WJ/HAZ) of the alloy produced by the FSW process. More active domains for Al3+ dissolution were found in the HAZ regions coupled to WJ, more specially in the HAZ of the advancing side (AS). These results demonstrate that the Al3+−ISME presented in this work can be used to monitor corrosion sites on aluminum alloys surfaces with combined chemical and spatial resolution.
Influence of chloride ions concentration on the development of severe localised corrosion and its effects on the electrochemical response of the 2198-T8 alloy
2021 - MACHADO, CARULINE de S.C.; SILVA, REJANE M.P. da; ARAUJO, JOAO V. de S.; MILAGRE, MARIANA X.; DONATUS, UYIME; VIVEIROS, BARBARA V.G. de; KLUMPP, RAFAEL E.; COSTA, ISOLDA
The development of severe localised corrosion (SLC) on the 2198-T8 alloy was investigated in solutions of various NaCl concentrations (0.001, 0.005 and 0.01 mol L−1). Immersion tests, optical profilometry, conventional and local electrochemical analyses were performed to evaluate the corrosion behaviour of the alloy. Immersion tests showed that the alloy is susceptible to SLC in all conditions, although the pits sizes were dependent on the solution concentration. The largest anodic areas, corresponding to SLC sites, were observed for the sample immersed in 0.001 mol L−1 NaCl, whereas pits with similar sizes were observed for the samples immersed in solutions with 0.005 and 0.01 mol L−1 of NaCl. Moreover, the maximum depth of attack was observed for the sample immersed in 0.001 mol L−1 NaCl. These results were in agreement with the scanning ionselective electrode technique (SIET) maps which showed stronger acidification on the sample exposed to 0.001 mol L−1 NaCl solution.
Microelectrochemical evaluation of severe localized corrosion sites developing on third-generation aluminium alloys
2021 - IZQUIERDO, J.; SILVA, R.M.P. da; MILAGRE, M.X.; COSTA, I.; BETANCOR-ABREU, A.M.; SOUTO, R.M.
Third-generation aluminium-copper-lithium alloys exhibit attractive mechanical properties, in particular light-weight and significant strength. However, the developed microstructure often results in severe localized corrosion (SLC) sites with fast in-depth pit propagation accompanied by H2 evolution.1 Such phenomena stem from a strong galvanic coupling, mainly established between Fe- and Cu-rich particles and the surrounding matrix. As a result, strong concentration and pH gradients develop throughout the aluminium surface, determining the local breakdown of the passive regime eventually provided by aluminium oxides and corrosion products. Understanding the development of such distributions is key to outline appropriate strategies for the prevention of fast degradation and materials failure. Scanning Electrochemical Microscopy (SECM) and Scanning Vibrating Electrode Technique (SVET) are capable of providing local information on the distribution of active sites and the presence of reactive chemical species. SVET has previously demonstrated the formation of gas bubbles ascribed to hydrogen evolution (i.e., electro-reduction process) at the anodically-activated sites,2,3; whereas local hydrogen production, oxygen consumption and pH changes are readily accessible using SECM, although with some limitations with regards to the detection of evolving gas.4 The present contribution reports recent advances in the investigation of local degradation phenomena occurring at the surface of Al-Cu-Li alloy AA-2098, as bare material and after friction stir welding. Oxygen consumption over nobler particles acting as cathodic sites, and SLC accompanied with strong acidification and H2 production at the local anodes were observed. The determined pH and concentration gradients allow to progress in the knowledge of the mechanistic aspects involved in the degradation processes on these materials.
Use of amperometric and potentiometric probes in scanning electrochemical microscopy for the spatially-resolved monitoring of severe localized corrosion sites on aluminum alloy 2098-T351
2021 - SILVA, REJANE M.P. da; IZQUIERDO, JAVIER; MILAGRE, MARIANA X.; BETANCOR-ABREU, ABENCHARA M.; COSTA, ISOLDA; SOUTO, RICARDO M.
Amperometric and potentiometric probes were employed for the detection and characterization of reactive sites on the 2098-T351 Al-alloy (AA2098-T351) using scanning electrochemical microscopy (SECM). Firstly, the probe of concept was performed on a model Mg-Al galvanic pair system using SECM in the amperometric and potentiometric operation modes, in order to address the responsiveness of the probes for the characterization of this galvanic pair system. Next, these sensing probes were employed to characterize the 2098-T351 alloy surface immersed in a saline aqueous solution at ambient temperature. The distribution of reactive sites and the local pH changes associated with severe localized corrosion (SLC) on the alloy surface were imaged and subsequently studied. Higher hydrogen evolution, lower oxygen depletion and acidification occurred at the SLC sites developed on the 2098-T351 Al-alloy.
On the local corrosion behavior of coupled welded zones of the 2098-T351 Al-Cu-Li alloy produced by Friction Stir Welding (FSW)
2021 - SILVA, REJANE M.P. da; IZQUIERDO, JAVIER; MILAGRE, MARIANA X.; BETANCOR-ABREU, ABENCHARA M.; OLIVEIRA, LEANDRO A. de; ANTUNES, RENATO A.; SOUTO, RICARDO M.; COSTA, ISOLDA
Localized electrochemical methods supported by surface analytical characterizations were employed to investigate galvanic coupling effects and local electrochemical activity developed along the welded zones in Friction Stir Welded 2098-T351 Al-Cu-Li alloy. The investigation was carried out in the coupled weld joint/heat affected zones (WJ/HAZ) for both, the retreating (RS) and the advancing (AS) sides. The correlation between the surface chemistry, the microstructural characteristics and the electrochemical activity of these welded areas was studied. The results showed the development of galvanic interactions within and between the WJ and HAZ regions, which were imaged using the scanning vibrating electrode technique (SVET), and scanning electrochemical microscopy (SECM). SVET analyses showed that HAZ was more susceptible to the development of anodic sites than WJ. SECM in amperometric operation mode showed that WJ coupled to HAZ exhibited higher oxygen consumption and higher cathodic activity compared to HAZ. Furthermore, SECM in potentiometric operation showed alkalinization around WJ and increased acidity in HAZ, mainly at sites of severe localized corrosion (SLC). Based on the SVET and SECM results in combination with the surface analyses, it is proposed that the microgalvanic cells formed within these welded zones are due to the presence of secondary phases in the 2098-T351 alloy and their interactions with the adjacent matrix.