Micro‐Raman spectroscopy and complementary techniques for the study of iron weapons from Motya and Lilybaeum (Sicily, Italy): Corrosion patterns in lagoon‐like and calcarenitic hypogea environments

Bernabale, Martina; Nigro, Lorenzo; Vaccaro, Carmela; Nicoli, Maria Cristina; Montanari, Daria; Bigini, Pierpaolo; Vito, Caterina De

doi:10.1002/jrs.6285

Cited by 9 publications

(6 citation statements)

References 60 publications

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“…The occurrence of magnetite, goethite and lepidocrocite and the absence of chloride phases suggest a low Cl − activity in alkaline media, typical of the Lagoon-like system of Motya, as reported in 27 .…”

Section: Resultssupporting

confidence: 60%

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

Bernabale

Cognigni

Nigro

et al. 2022

Sci Rep

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The best strategy to tackle complexity when analyzing corrosion in iron artefacts is to combine different analytical methods. Traditional techniques provide effective means to identify the chemistry and mineralogy of corrosion products. Nevertheless, a further step is necessary to upgrade the understanding of the corrosion evolution in three dimensions. In this regard, Multiscale X-ray Microscopy (XRM) enables multi-length scale visualization of the whole object and provides the spatial distribution of corrosion phases. Herein, we propose an integrated workflow to explore corrosion mechanisms in an iron-nail from Motya (Italy) through destructive and non-destructive techniques, which permit the extraction of the maximum information with the minimum sampling. The results reveal the internal structure of the artefact and the structural discontinuities which lead the corrosion, highlighting the compositional differences between the tip and the head of the iron nail.

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Section: Resultssupporting

confidence: 60%

“…Indeed, the main phase observed at the interface between the metal and the rust layer is goethite. The formation of the TM, in red, could be explained by the dissolution of iron and reprecipitation of iron corrosion/oxidation products over the surface of the object, perhaps over the original surface 27 , 30 – 33 .…”

Section: Resultsmentioning

confidence: 99%

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

Bernabale

Cognigni

Nigro

et al. 2022

Sci Rep

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“…Raman spectroscopy represents an excellent tool in the investigation of Cultural Heritage field, not only because of its non‐invasiveness but also because it allows the identification of the corrosion phases occurring at microscopic scale, providing a fingerprint of the compound under study. [ 15,16 ]…”

Section: Introductionmentioning

confidence: 99%

“…Raman spectroscopy represents an excellent tool in the investigation of Cultural Heritage field, not only because of its noninvasiveness but also because it allows the identification of the corrosion phases occurring at microscopic scale, providing a fingerprint of the compound under study. [15,16] At the current state of knowledge, the technological skill of Phoenicians in metal production is still lacking for the Central Mediterranean area. Attempts to reconstruct the development of Phoenician metallurgy go back to the limited surveys of copper and iron production at Phoenician sites of the Iberian Peninsula, Sardinia, and North Africa.…”

Section: Introductionmentioning

confidence: 99%

Micro‐Raman spectroscopy and complementary techniques applied for the study of copper and iron wastes from Motya (Italy)

Bernabale

Montanari

Nigro

et al. 2022

J Raman Spectroscopy

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This work is the first archaeometric investigation on copper and iron wastes from the Phoenician site of Motya (Sicily, Italy), dating back to the 8 th to the 4 th century BC. The samples were analyzed through micro-Raman Spectroscopy (μ-RS), Optical Microscopy (OM), Scanning Electron Microscope-Energy-Dispersive X-ray Spectroscopy (SEM-EDS), High-Resolution Field Emission Scanning Electron Microscopy (HR-FESEM), and Electron Micro-Probe Analysis (EMPA). Micro-Raman techinique permitted to identify both primary phases, for example, calchopyrite, and secondary products such as cuprite and copper thrihydroxychlorides in the Cu-slags and goethite in the Fe-slags. SEM and HR-FESEM imaging showed the occurrence of inhomogeneous microstructures in the Cu-and Fe-slags due to elements segregation, solidification, and corrosion. EMPA data revealed that the archaeometallurgical wastes from Motya can be differentiated on the basis of their chemical compositions. These preliminary results showed different typologies of byproducts, such as base metals speiss, copper slags from smelting sulfide ore with matte, and iron smelting and smithing slags, suggesting different stages of copper and iron productions.

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“…All the metallic samples were observed under Optical Reflected Light Microscopy, and then some samples were analyzed using both SEM-EDS and Micro-Raman analyses. These techniques are generally used to characterize mineral phases of corroded iron materials or archaeological metals in general [15].…”

Section: Introductionmentioning

confidence: 99%

Microstructure, Chemistry and Mineralogy Approach for the Diagnostics of Metallic Finds of the Tomba della Biga (Adria, Italy)

et al. 2022

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This work is focused on the characterization of metallic finds that are part of an ancient war biga from the Tomba della Biga, using different approaches for the diagnostics and also the conservation of this important cultural heritage. The materials analyzed were brought to light in the necropolis of Canal Bianco (Adria, Italy). The samples were analyzed using Optical Reflected Light Microscopy (ORLM), Scanning Electron Microscopy (SEM) and micro-Raman Spectroscopy (µ-RS). The results highlighted the occurrence of two different alloys (Fe and Cu-Sn-bronze) showing important structural and textural variations. These results, along with µ-RS, gave details on the surface and subsurface morphology, as well as the microstructures and the chemical and mineralogical composition of the finds. In particular, µ-RS highlighted the presence of magnetite and goethite as the main mineralogical phases for Fe-samples and malachite, azurite and Cu-oxide for bronze samples. In addition, an attempt was made to trace the manufacturing process, the purity of the alloys and the degree of slagging. Results of analytical studies show corrosion products of the samples which could be evidence of metallurgical aspects. The good state of conservation due to favorable conditions in the burial environment preserved the metal finds from intense corrosion, supporting the hypothesis that the samples reached equilibrium with soil during their life in the burial environment. This proposed methodology based on the microstructure, chemistry and mineral microanalysis allows the diagnostic and evaluation of the state of conservation of metallic finds.

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Micro‐Raman spectroscopy and complementary techniques for the study of iron weapons from Motya and Lilybaeum (Sicily, Italy): Corrosion patterns in lagoon‐like and calcarenitic hypogea environments

Cited by 9 publications

References 60 publications

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

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

Micro‐Raman spectroscopy and complementary techniques applied for the study of copper and iron wastes from Motya (Italy)

Microstructure, Chemistry and Mineralogy Approach for the Diagnostics of Metallic Finds of the Tomba della Biga (Adria, Italy)

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