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Ceramic technology: how to characterise black Fe-based glass-ceramic coatings
Archaeological and Anthropological Sciences ( IF 2.1 ) Pub Date : 2020-07-28 , DOI: 10.1007/s12520-020-01134-x
Eleni Aloupi-Siotis

The study of the ancient black ceramic coating that decorates the surface of Classical and Hellenistic pottery from Attica and other main production centres in the Mediterranean has been the subject of more than three centuries of research. The physicochemical characterisation and analysis of the black glaze/gloss (BG) with the use of a broad spectrum of analytical techniques has gradually revealed its nature as an iron-based glass-ceramic material. At its best, it is coloured by polycrystalline nanoparticles of magnetite or mixed magnetite/hercynite spinels, dispersed in the amorphous K-aluminosilicate phase doped by Fe2+/Fe3+. We discuss the technique to produce the BGc (black glass-ceramic, hereafter), known as the “iron reduction technique”, with emphasis on the 3-stage firing under oxidising-reducing-oxidising (ORO) conditions as well as the latest analytical results through XPS, high-resolution TEM, SR-micro XRD and XANES. The discussion is based on data and research experience accumulated over the years from the application of conventional techniques (such as SEM-EDS and hhXRF) on ancient samples, laboratory reproductions and contemporary full-scale reproduction of similar artefacts. We show that the parameters affecting the quality of the BGc (sheen, colour, micromorphology) depend on the nature of the clay-slip, the application process, the ORO firing scheme and weathering mechanisms due to burial in humid terrestrial or marine environment. The proposed analytical protocol for the routine characterisation of the micromorphology and the analysis of the BGc and the ceramic body involves the use of non-destructive or minutely destructive techniques with special emphasis on the pottery sample classification and documentation.

中文翻译:

陶瓷技术:如何表征黑色铁基玻璃陶瓷涂层

过去三个多世纪的研究一直是对装饰着Attica和地中海其他主要生产中心的古典和古希腊陶器表面的古代黑色陶瓷涂层的研究。使用广泛的分析技术对黑釉/光泽(BG)进行物理化学表征和分析,逐渐揭示出其作为铁基玻璃陶瓷材料的性质。最好的情况是,它被磁铁矿或磁铁矿/水铁矿尖晶石的多晶纳米颗粒着色,分散在掺有Fe2 + / Fe3 +的非晶K-铝硅酸盐相中。我们讨论了生产BGc(以下称为黑玻璃陶瓷)的技术,称为“铁还原技术”,重点介绍了在氧化还原(ORO)条件下进行的三阶段焙烧,以及通过XPS,高分辨率TEM,SR-micro XRD和XANES的最新分析结果。讨论基于多年以来的数据和研究经验,这些经验是由于对古代样本,实验室复制品和当代人工制品的当代全面复制应用常规技术(例如SEM-EDS和hhXRF)而积累的。我们表明,影响BGc质量的参数(光泽,颜色,微观形态)取决于黏土滑移的性质,施工过程,ORO烧成方案以及由于在潮湿的陆地或海洋环境中埋葬而引起的风化机理。
更新日期:2020-07-28
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