A comprehensive strategy for exploring corrosion in iron-based artefacts through advanced Multiscale X-ray Microscopy

Bernabale, Martina; Cognigni, Flavio; Nigro, Lorenzo; Rossi, Marco; de, Tilde; Vito, Caterina De

doi:10.1038/s41598-022-10151-w

Cited by 12 publications

(4 citation statements)

References 33 publications

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“…23,29,31,37 Among all phases of Fe oxides reported during Fe oxidation, we considered the most thermodynamically stable phases, Fe3O4 and Fe2O3 (Fig. 2b), [38][39][40][41] also known respectively as magnetite and hematite. Further discussion on this topic can be found later in the manuscript.…”

Section: Data Processingmentioning

confidence: 99%

Deciphering the Interplay Between Local and Global Dynamics of Anodic Metal Oxidation

Makogon,

Noël,

Kanoufi

et al. 2023

Preprint

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The stark difference between global and local metal oxidation dynamics underscores the need for methodologies capable of performing precise sub-µm-scale and wide-field measurements. In this study, we present Reflective Microscopy (RM) as a tool developed to address this challenge, illustrated by the example of chronoamperometric Fe oxidation in NaCl solution. Analysis at a local scale of 10s of µm has revealed three distinct periods of Fe oxidation: the initial covering of the metal interface with a surface film, followed by the electrochemical conversion of the formed surface film, and finally, the in-depth oxidation of Fe. In addition, thermodynamic calculations and the quantitative analysis of changes in optical signal (light intensity), correlated with variations in refractive indexes, suggests the initial formation of hematite, followed by its subsequent conversion to magnetite. The reactivity maps for all three periods are heterogeneous, which can be attributed to the preferential oxidation of certain crystallographic grains. Notably, at the global scale of 100s of µm, reactivity initiates at the electrode border and progresses towards its center, demonstrating a unique pattern that is independent of local metal structure. This finding underscores the significance of simultaneously employing sub-µm-precise and wide-field measurements for a comprehensive description of metal oxidation processes.

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Section: Data Processingmentioning

confidence: 99%

Deciphering the Interplay Between Local and Global Dynamics of Anodic Metal Oxidation

Makogon,

Noël,

Kanoufi

et al. 2023

Preprint

View full text Add to dashboard Cite

show abstract

“…23,29,31,37 Among all phases of Fe oxides reported during Fe oxida�on, we considered the most thermodynamically stable phases, Fe3O4 and Fe2O3 (Fig. 2b), [38][39][40][41] also known respec�vely as magne�te and hema�te. Further discussion on this topic can be found later in the manuscript.…”

Section: Data Processingmentioning

confidence: 99%

Deciphering the Interplay Between Local and Global Dynamics of Anodic Metal Dissolution

Makogon

Noël

Kanoufi

et al. 2023

Preprint

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The stark difference between global and local metal dissolution dynamics underscores the need for methodologies capable of performing precise sub-µm-scale and wide-field measurements. In this study, we present Reflective Microscopy (RM) as a tool developed to address this challenge, illustrated by the example of chronoamperometric Fe oxidation in NaCl solution. Analysis at a local scale of 10s of µm has revealed three distinct periods of Fe oxidation: the initial covering of the metal interface with a surface film, followed by the electrochemical conversion of the formed surface film, and finally, the in-depth oxidation of Fe. In addition, thermodynamic calculations and the quantitative analysis of changes in optical signal (light intensity), correlated with variations in refractive indexes, suggests the initial formation of hematite, followed by its subsequent conversion to magnetite. The reactivity maps for all three periods are heterogeneous, which can be attributed to the preferential oxidation of certain crystallographic grains. Notably, at the global scale of 100s of µm, reactivity initiates at the electrode border and progresses towards its center, demonstrating a unique pattern that is independent of local metal structure. This finding underscores the significance of simultaneously employing sub-µm-precise and wide-field measurements for a comprehensive description of metal dissolution processes.

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“…Researchers also proposed an integrated workflow to explore corrosion mechanisms in ancient metallic artifacts based on CLEM, XRM, and Raman spectroscopy, which permits the extraction of the maximum information with the minimum sampling. The results revealed the internal structure of the artefact and the structural discontinuities which lead to the corrosion [32].…”

Section: Introductionmentioning

confidence: 97%

Correlative Light and Electron Microscopy (CLEM): A Multifaceted Tool for the Study of Geological Specimens

Cognigni,

Miraglia,

Contessi

et al. 2023

JETA

Self Cite

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Correlative light and electron microscopy (CLEM) is an advanced imaging approach that faces critical challenges in the analysis of both materials and biological specimens. CLEM integrates the strengths of both light and electron microscopy, in a hardware and software correlative environment, to produce a composite image that combines the high resolution of the electron microscope with the large field of view of the light microscope. It enables a more comprehensive understanding of a sample’s microstructure, texture, morphology, and elemental distribution, thereby facilitating the interpretation of its properties and characteristics. CLEM has diverse applications in the geoscience field, including mineralogy, petrography, and geochemistry. Despite its many advantages, CLEM has some limitations that need to be considered. One of its major limitations is the complexity of the imaging process. CLEM requires specialized equipment and expertise, and it can be challenging to obtain high-quality images that are suitable for analysis. In this study, we present a CLEM workflow based on an innovative sample holder design specially dedicated to the examination of thin sections and three-dimensional samples, with a particular emphasis on geosciences.

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A comprehensive strategy for exploring corrosion in iron-based artefacts through advanced Multiscale X-ray Microscopy

Cited by 12 publications

References 33 publications

Deciphering the Interplay Between Local and Global Dynamics of Anodic Metal Oxidation

Deciphering the Interplay Between Local and Global Dynamics of Anodic Metal Oxidation

Deciphering the Interplay Between Local and Global Dynamics of Anodic Metal Dissolution

Correlative Light and Electron Microscopy (CLEM): A Multifaceted Tool for the Study of Geological Specimens

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