A large number of pyrometallurgical materials such as tuyeres, slags and refractory tools likely associated with metal extraction processes have been found at Tharros (north-western Sardinia, Italy) during archaeological excavations stratigraphically related to the Phoenician–Punic period (VI–III centuries BC). Micro-chemical, microstructural and mineralogical studies have been carried out by means of the combined use of X-ray diffraction (XRD), selected-area X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) combined with energy-dispersive X-ray analysis (EDS) in order to identify pyrometallurgical processes and main relevant technological parameters. The results reveal that tuyeres, slags and refractory tools can be associated with an iron ore smelting process to extract the metal by slagging the unwanted by-products. Moreover, temperature and duration of the smelting process have been estimated through mineralogical studies and by a comparative analysis between the micro-chemical and structural features of thermally treated refractory materials and tuyeres. The results disclose the high level of technological competence of the ancient metallurgists able to carry out complex high-temperature processes to extract iron from ores by separating the metal from unwanted siliceous species.
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