Raman scattering features of lead pyroantimonate compounds. Part I: XRD and Raman characterization of Pb2Sb2O7 doped with tin and zinc

• Published in: Journal of Raman spectroscopy Vol. 40; no. 1; pp. 107 - 111
• Main Authors: Rosi, F., Manuali, V., Miliani, C., Brunetti, B. G., Sgamellotti, A., Grygar, T., Hradil, D.
• Format: Journal Article
• Language: English
• Published: Chichester, UK John Wiley & Sons, Ltd 01-01-2009
• Subjects: Cations; Cubic lattice; cubic pyrochlores; Diffraction; Doping; lead antimonate yellow; Naples yellow; Polyhedrons; Raman spectroscopy; Tin; XRD; Zinc
• ISSN: 0377-0486; 1097-4555
• DOI: 10.1002/jrs.2092

Yellow pyroantimonates PbSb, PbSbSn and PbSbZn were synthesized by solid‐state reactions at high temperature and characterized by X‐ray diffraction and Raman spectroscopy. The lattice size of cubic pyrochlores increases with Sn and Zn doping and with Pb overstoichiometry, indicating the replacement of Sb5+ by the larger cations. This fact permits the understanding of the corresponding Raman spectral modifications as a consequence of the changes in the local symmetry of the SbO polyhedra, justifying the exploitation of Raman spectroscopy to noninvasively identify structural modifications of pyroantimonate pigments in artworks. Copyright © 2008 John Wiley & Sons, Ltd.
Reference lead antimonate pigments were synthesized following historical recipes and then characterized by X‐ray powder diffraction with Rietveld refinement, obtaining the crystallographic structures and lattice parameters. The structural information was used to interpret the modification induced by Sn and Zn doping on Raman scattering signatures of the corresponding pyrochlore structures.