ACTA

A New Era in Ceramic Archaeometry: A Comprehensive Multimodal Methodological Workflow

R. Abdelrahman^a,b, J. Depciuch^c, P. Grzywa^a, S. Wroński^a, L. Alluhaibi^d, M. Środa^e, A. Maximenko^d, M. Wojenka^f, J. Tarasiuk^a, L. Samek^a
^aAGH University of Krakw, Faculty of Physics and Applied Computer Science, al. Mickiewicza 30, 30-059 Kraków, Poland
^bFuture University in Egypt, Faculty of Engineering and Technology, 90th Street, Fifth Settlement, New Cairo, 11835 Cairo, Egypt
^cInstitute of Nuclear Physics Polish Academy of Science, Radzikowskiego 152, 31-342 Kraków, Poland
^dSOLARIS National Synchrotron Radiation Centre, Jagiellonian University, Czerwone Maki 98, 30-392 Kraków, Poland
^eAGH University of Kraków, Faculty of Materials Science and Ceramics, al. Mickiewicza 30, 30-059 Kraków, Poland
^fJagiellonian University Institute of Archaeology, Gołębia 11, 31-007 Kraków, Poland

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This study establishes a comprehensive, sequential multimodal workflow for archaeometric analysis of medieval ceramics, integrating seven measurement techniques to characterize elemental, crystalline, amorphous, microstructural, structural, and chemical-state properties of the material, while preserving artefact integrity. Therefore, (i) X-ray fluorescence establishes baseline major (Si, Al, Fe, Ca, K, Na) and trace (Cr, Mn, Zr) profiles for paste discrimination; (ii) X-ray diffraction identifies kaliophilite/oligoclase phases (~ 800–900°C firing); (iii) Fourier transform infrared resolves amorphous networks (Si–O–Si 950–1100 cm^-1); (iv) Raman spectroscopy detects microscale oxide impurities (anatase TiO₂ lattice modes at 110–160 cm^-1, ZrO₂, Al₂O₃ corundum M–O stretching modes at 440–465 cm^-1) and lattice defects, revealing heavy mineral tempers (rutile sands) and refractory phases undetectable by bulk diffraction analysis or the broad spectral envelopes of infrared spectroscopy; (v) scanning electron microscope with energy dispersive spectroscopy quantifies temper distributions; (vi) X-ray computed tomography reveals 3D void networks, and (vii) X-ray absorption near-edge structure constrains speciation of Fe²⁺/Fe³⁺, Ca carbonate–silicates, and K-feldspars. This standardized framework enables precise reconstruction of provenance, fluxing strategies, pyrotechnology, and post-firing alterations, beyond the limitations of single- and dual-technique approaches, providing a reproducible protocol for heritage science.

DOI:10.12693/APhysPolA.149.S198
topics: medieval ceramics, multimodal analytical framework, archaeometry, cultural heritage