Abstract
Three major corpora of architectural glazed bricks from Ancient Mesopotamia dating to the Neo-Assyrian (Aššur and Khorsabad sites) and the Neo-Babylonian (Babylon site) Periods have been submitted to an in-depth comparative study of the orange–yellow and black glazes. Distinct hues in the orange–yellow range were observed according to the archaeological site. They appear to have been well mastered by the glassmakers, consisting in the ex situ preparation of the antique lead antimonate pigment and its mixing with transparent soda-lime glass frit or with the glass-forming components. The intentional addition of hematite or of Cu2+ colouring ions in a controlled amount is suggested in two cases. SEM-EDX and Raman analysis of the lead antimonate pigments have pointed out different chemical substitutions in their pyrochlore structure, mainly Fe3+ in the Sb5+ site and Ca2+ in the Pb2+ site, the proportion of which being correlated to the pigment shade (from pale yellow to orange–red). Part of these substitutions arises from the chemical reaction of the pigment with the hematite and glass melt during firing. Regarding the black glazes, an unexpected colouring technique involving copper sulphide nanoparticles together with the chromophore Fe3+-S2− is highlighted for Khorsabad (8th century BC) and for Babylon (6th century BC). For Aššur blacks, the study reveals a change in their colouring technique between the 9th and 8th centuries BC, from a colouration with Mn oxides to an enigmatic one that could also have involved copper sulphide nanoparticles.
Highlights
IntroductionBetween the 14th and the 4th century BC, monumental glazed decorations adorned architectural facades of major cities in Elam (south-west of present-day Iran) and in ancient Mesopotamia (present-day Iraq for its most part) [1]
For nearly a millennium, between the 14th and the 4th century BC, monumental glazed decorations adorned architectural facades of major cities in Elam and in ancient Mesopotamia [1]
The in-depth study by optical microscopy, SEM-EDX, and μ-Raman of glaze samples belonging to Aššur (9th to 7th BC), Khorsabad (8th century BC), and Babylon (6th BC) architectural glazed bricks have brought to light some very interesting features of the respective colouring agents of the orange–yellow and black glazes
Summary
Between the 14th and the 4th century BC, monumental glazed decorations adorned architectural facades of major cities in Elam (south-west of present-day Iran) and in ancient Mesopotamia (present-day Iraq for its most part) [1]. The Ishtar Gate of the city of Babylon for instance, reconstituted in the Vorderasiatisches Museum (VAM) in Berlin, or the frieze of the Archers of the city of Susa, preserved in the musée du Louvre in Paris, allow us to appreciate nowadays the monumentality of such constructions These decorations are the mark of a flourishing technological development of glazing on bricks that took place in these pioneer regions of the Ancient Near East from the 14th century BC onwards, shortly after the appearance of the first core formed glass vessels [1–4]. In order to improve our knowledge and to preserve and transmit this history, the physico-chemical study of these glazed decorations is of major interest This contributes to helping museums reconstitute these decors in an approach of cultural and sensory knowledge and to investigate these technical innovations and the transfer of know-how in these regions, including the connection with metallurgy and glass production techniques. Note that the so-called “weathering” of glass refers to its degradation by chemical reaction of the glassy surface with groundwater during burial
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