Micro-EDXRF, SEM-EDS and OM characterisation of tin soldering found in handle attachments of Roman situlae from Conimbriga (Portugal)

Abstract

Tin (Sn) or a Sn-rich solder applied to copper-based artefacts has been frequently used at least, since the Ancient Greece, although scarce studies have been published concerning the technology of this metallurgical joining technique. Several filler remnants were reported to be found in a Roman collection of handle attachments of situlae or cauldrons (2nd century BCE-5th century CE) from the archaeological site of Conimbriga, a Roman city from the Lusitania Province (Portugal). All these artefacts were cast in high leaded coppers and bronzes. The present study aims to contribute to the knowledge of Sn-rich soldering, an ancient metallurgical joining technique, by the characterisation of the fusible metallic alloy present in 10 Roman artefacts by means of micro-energy dispersive X-ray fluorescence spectrometry (micro-EDXRF), scanning electron microscopy with energy dispersive X-ray (SEM-EDS) microanalysis and optical microscope (OM) observations. Results of studied solders show the presence of Cu-Sn alloys, with Sn contents ranging from δ to η phase composition (30-60 wt% Sn). As the attachments were made in leaded copper alloys, it was also observed, in some cases, the melting of the interdendritic Pb-rich chains with long-range diffusion of the solder alloy into the substrate. The fillers compositions suggest that the handle attachments have been joined to a situla body by the soldering metallurgical process with Sn or a Sn-rich alloy. The studied leaded Cu-Sn attachments, probably formulated by local craftsman, were joined into the body of a situla or cauldron with a soft solder (soldering), a common metallurgical joint from Antiquity, although no relation was found between composition or typology and the Sn or Sn-rich solder.

X-ray fluorescence mapping: Insights into mesoscale structure impact on battery functional electrochemistry

“…Using a tightly-focused primary X-ray beam to induce X-ray fluorescence emission as a sample is scanned, micro-X-ray fluorescence (µ-XRF) enables spatially resolved characterization of metal centers and their oxidation states [4]. Synchrotron light sources are desirable for µ-XRF due to their high X-ray intensity, although benchtop and even portable solutions have been reported [5,6].…”