Abstract: Iron palaeometallurgy was carried out on three artefacts, classified as nails and excavated from the archaeological site of Loiola (La Arboleda, Biscay, northern Spain), to investigate Roman manufacturing techniques. Energy Dispersive Spectroscopy (EDS) coupled with Environmental Scanning Electron Microscopy (ESEM) and micro-Raman spectroscopy were used to obtain elemental composition and structural characterization of mineral phases. Metallurgical properties and crystallographic texture were studied by combining microscopic methods such as optical microscopy (OM), Electron Backscatter Diffraction realized in environmental mode (EBSD) and measurements of local Vickers microhardness. The three artefacts had different microstructures, distinguished by a large gradient of carbon content, although important segregations (inclusions) were observed in all of them. Two pearlite-rich artefacts showed a high density of structural defects (geometrically necessary dislocations and large crystallographic orientation gradients in pearlitic ferrite, curved pearlitic cementite) resulting from a high level of plastic deformation that occurred during the manufacturing process. The third artefact consisted of pure ferrite without structural defects. This one was clearly manufactured differently from the two others, so it probably had another functionality.

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