Mineralogical characterization of carreaux de pavement from Northern Spain (Tiebas, Navarre)

Several medieval tiles from Tiebas Castle in Navarre, classified as carreaux de pavement, were mineralogically analyzed. The aim was to add information to the very scarce analytical data available for carreaux de pavement in order to provide a quality primary work, mainly descriptive, in this topic. The characterization techniques applied were: optical microscopy (OM), colorimetry, Fourier transform infrared (FT-IR) spectroscopy, differential thermal analysis and thermogravimetry (DTA-TG), X-ray fluorescence (XRF) spectroscopy, petrographic microscopy (PM), X-ray diffraction (XRD), scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-EDS). The tiles comprised three layers: a top glaze with mainly silicon and lead-based compounds; a thin layer of silicoaluminate (very possibly kaolinite) called engobe under it; and the pastes, composed of quartz, hematite, potassium feldspars and calcite. Honey glazes were richer in iron, being copper-based compounds responsible for dark green glazes. The orangish-reddish color of the pastes was provided by hematite. Although the tiles were found in three different locations within the castle, no significant differences were detected among them. The carreaux de pavement from Tiebas had similarities with that from the Bordeaux region. According to the composition data and thickness of tiles from other French carreaux de pavement, the Tiebas artifacts were dated to the 13th century