MARIANA XAVIER MILAGRE

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  • Artigo IPEN-doc 29764
    A historical, statistical and electrochemical approach on the effect of microstructure in the anodizing of Al alloys
    2023 - ARAUJO, JOAO V. de S.; MILAGRE, MARIANA; COSTA, ISOLDA
    Anodizing is a well-documented surface treatment that is inserted in a complex protection system against corrosion applied to Al alloys. In the scientific literature, there are many works about this topic, which are concentrated on: (1) anodic aluminum oxide (AAO) growth mechanism; (2) anodized alloys corrosion behavior, or (3) the influence of anodizing parameters on the following steps of corrosion protection of the anodized layer. However, the effect of the microstructure on the AAO formation is not yet well established. This paper aims to review the effect of the microstructure of Al and its alloys on the anodizing process by a historical, statistical, and electrochemical approach, considering the advantages in understanding the influence of intermetallics in this process. Besides, this review brings a comparison among the number of publications and the types of alloys studied by statistical analyses. Finally, it emphasizes the importance of anodizing in the aeronautical industry, in which a great number of studied alloys are applied, mainly the 2XXX (Al-Cu) and 7XXX (AlZn) series alloys.
  • Artigo IPEN-doc 29682
    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).
  • Resumo IPEN-doc 29501
    The effect of tartaric-sulfuric acid (TSA) anodizing on the corrosion resistance of the AA7475-T761
    2022 - ARAUJO, JOAO V.; MILAGRE, MARIANA X.; GABBARDO, ALINE D.; KLUMPP, RAFAEL E.; COSTA, ISOLDA
    The microstructure of the high strength aluminum alloy, AA7475–T761, in the as-received condition was characterized by optical microscopy, scanning electron microscopy and transmission electron microscopy, and statistical analyses of grain size and micrometer precipitates distribution and density were performed. An anodic aluminum oxide (AAO) film was potentiostatically grown on the alloy in tartaric sulfuric acid (TSA). The anodizing behavior of the alloy and the mechanisms of localized corrosion initiation and propagation in bare (not anodized) and anodized conditions were discussed. The alloy corrosion behavior was investigated in sodium chloride solutions using electrochemical techniques (cyclic potentiodynamic polarization) and the morphology and extent of corrosion propagation was investigated through optical microscopy, optical profilometry and scanning electron microscopy analyses. It was observed that the two alloy surface conditions (bare and anodized) play different roles in the propagation of the localized corrosion process. The bare alloy presented lower localized corrosion potentials and the propagation of the localized corrosion was shallower, but more heavily distributed, than in the anodized condition. However, the alloy in the anodized condition presented lower repassivation potentials due to the deeper pits formed. In addition, the variability of pitting potentials for the anodized condition was high, due to the heterogenous structure of the AAO film formed, and dependent on the time and drying storage conditions previous to electrochemical characterizations. The electrochemical results were correlated with the microstructural characteristics of the oxide surface film of the alloy in both conditions, bare (not anodized) and anodized.
  • Artigo IPEN-doc 29075
    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.
  • Artigo IPEN-doc 29046
    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.
  • Artigo IPEN-doc 28933
    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.
  • Resumo IPEN-doc 28893
    A homemade electrochemical hanging droplet cell to evaluate the corrosion resistance of friction stir weld zones of the AA2198-T8 Al-Cu-Li alloy
    2021 - MACHADO, CARULINE de S.C.; HERNANDEZ, JOSE W.C.; MILAGRE, MARIANA X.; ARAUJO, JOAO V. de S.; DONATUS, UYIME; COSTA, ISOLDA
    In this study, the corrosion resistance of the different zones of the AA2198-T8 alloy welded using friction stir welding (FSW) was investigated by immersion and electrochemical tests during exposure to 0.005 mol L-1 NaCl solution. After immersion tests, the welding zones were classified in two groups, according to their severe localized corrosion (SLC) morphology. Zones exposed to higher temperatures during welding presented intergranular attack, whereas those exposed to lower temperatures presented intragranular attack. Electrochemical measurements performed employing a homemade hanging droplet cell revealed potential galvanic coupling between the two groups. The base metal (BM) presented the most anodic potentials. The open circuit potential (OCP) increased from BM towards the stir zone (SZ). The results obtained by the hanging droplet cell were reproducible and coherent with the classification of the zones in the two proposed groups. The homemade electrochemical hanging droplet cell proved a very reliable tool to investigate the electrochemical behavior of the FSWed zones in Al-Cu-Li alloys.
  • Artigo IPEN-doc 28885
    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).
  • Artigo IPEN-doc 28851
    Corrosion behavior of the 6061 Al–Mg–Si alloy in different soils extracts
    2022 - MILAGRE, MARIANA X.; ARAUJO, JOAO V. de S.; MACHADO, CARULINE de S.C.; PEREIRA, MARCO S.; ANTUNES, RENATO A.; GENEZINI, FREDERICO; COSTA, ISOLDA
    In this work, the corrosion behavior of the 6061 Al-alloy in different temper conditions was studied in different soil extracts using electrochemical and surface monitoring techniques. The results showed that the corrosion behavior of the 6061 alloy depends on the soil extract composition, with the highest electrochemical activities related to the soil extracts with the lowest nitrate and sulfate concentrations. The 6061-T6 condition was more susceptible to corrosion than the 6061-HCR one. The results were related to the higher amounts of MgSi particles in the 6061-T6 alloy compared to the 6061-HCR. Sulfate and nitrate ions acted as corrosion inhibitor reducing the corrosion kinetics of the 6061 alloy in solutions with high concentration of chloride ions.
  • Artigo IPEN-doc 28826
    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.