Novel characterization techniques for cultural heritage using a TEM orientation imaging in combination with 3D precession diffraction tomography: a case study of green and white ancient Roman glass tesserae

Abstract

Abstract We present new transmission electron microscopy (TEM) based electron diffraction characterization techniques (orientation imaging combined with 3D precession electron diffraction tomography-ADT) applied on cultural heritage materials. We have determined precisely unit cell parameters, crystal symmetry, atomic structure, and orientation/phase mapping of various pigment/opacifier crystallites at nm scale which are present in green and white Roman glass tesserae. Such TEM techniques can be an alternative to Synchrotron based techniques, and allow to distinguish accurately at nm scale between different crystal structures even in cases of same/very close chemical composition, where is also possible to visualize between different crystal orientations and amorphous/crystalline phases. This study additionally demonstrates that although opacifiers in green and white tesserae are found to have average Pb 2 Sb 2 O 7 cubic and CaSb 2 O 6 trigonal structures, their pyrochlore related framework can host many other elements like Cu, Ca, Fe through ionic exchanges at high firing temperatures which in turn may also contribute to the tesserae colour appearance.