Synchrotron Micro-X-ray Diffraction in Transmission Geometry: A New Approach to Study Polychrome Stratigraphies in Cultural Heritage

Author:

Morabito Giulia1,Marinoni Nicoletta1,Bais Giorgio2ORCID,Cantaluppi Marco1,Botteon Alessandra3,Colombo Chiara3,Gatta G. Diego1,Polentarutti Maurizio2,Realini Marco3ORCID,Possenti Elena3ORCID

Affiliation:

1. Dipartimento di Scienze della Terra “Ardito Desio”, Università degli Studi di Milano, Via Botticelli 23, 20133 Milano, Italy

2. ELETTRA Sincrotrone Trieste S.C.p.A., Strada Statale 14 - km 163,5 in Area Science Park, 34149 Basovizza, Italy

3. Istituto di Scienze del Patrimonio Culturale (ISPC), Consiglio Nazionale delle Ricerche (CNR), Via R. Cozzi 53, 20125 Milano, Italy

Abstract

In cultural heritage, paint stratigraphies are complex systems typically consisting of various paint layers with fine crystalline phases mixed with coarse pigment and filler grains. This complexity poses significant challenges for X-ray diffraction (XRD) analysis. In this work, we employed synchrotron radiation micro-X-ray diffraction in transmission geometry (SR-µTXRD) with linear mapping to develop a novel approach for studying the crystalline phases (pigments and fillers) in mock-up paint stratigraphies. A targeted approach was followed for qualitative, quantitative, and microstructural analysis, combining signals from micrometric crystallites and coarse single crystals as well as from randomly oriented and iso-oriented crystalline phases. This allows for identifying, localizing, and quantifying these phases even in low fractions and distinguishes the same phases across different layers with varying grain sizes or spatial orientations. Critical analysis of 2D XRD patterns, coupled with full-profile fitting performed by the Rietveld method, provides insights into material preparation (e.g., grinding), painting technique (e.g., color palette, use of fillers, brushing), and crystallo-chemical modifications over time. This analytical approach, integrating spatially resolved investigation with high-quality phase characterization, enhances the potential of specific XRD methodologies for a 2D investigation of multi-phase materials in cultural heritage, even without dedicated micro-mapping techniques.

Funder

Italian Ministry of Education

Publisher

MDPI AG

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