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SEM-EDX and FTIR analysis of archaeological ceramic potteries from southern Italy
Microscopy ( IF 1.8 ) Pub Date : 2020-06-26 , DOI: 10.1093/jmicro/dfaa034
Tania Dey 1 , Joseph Coleman Carter 2 , Keith Swift 2
Affiliation  

Sherds of ancient ceramics potteries, dating back to the 7th-century BC and excavated from southern Italy, were analyzed in terms of microstructure and porosity (SEM), elemental composition (EDX), chemical bonding and mineralogical components (FTIR) in order to establish correlation with firing temperature, firing condition and provenance. Si/Al ratio from EDX analysis showed three major categories of raw materials (illite, kaolinite and montmorillonite), suggesting difference in provenance. Uniformly sized silica nanoparticle (0.7 μm diameter) and trace amount of silver is being reported for the first time in one sample. Anorthite mineral and quartz inclusion was detected by FTIR in certain samples. All samples showed a prominent band for Si-O stretching, which shifted from 1062 cm-1, broadened and appeared as doublet, relative to processing temperature. FTIR results proved incomplete dihydroxylation and undissociated carbonate in three samples, indicated a firing temperature of 700-800 C, whereas other samples were fired above 900 °C. Only one sample among these three showed bloating pores in between interconnecting glassy matrix in SEM image, indicating a firing temperature of 1100-1200 °C. Absence of magnetite along with significant Fe and Mn content indicated the formation of jacobsite, an iron manganese spinel complex, MnFe2O4, which is responsible for the black gloss effect in two particular samples and can be further confirmed by XRD. Presence of numerous small pores in SEM image of one of these two samples (1.2 μm diameter) was indicative of extended vitrification at higher temperature than the other one. However, magnetite was responsible for black gloss effect in two other samples, proving difference in provenance. Therefore, SEM-EDX and FTIR results can offer valuable insight into the firing conditions, gloss decoration and provenance of ancient ceramic potteries.

中文翻译:

意大利南部考古陶瓷的 SEM-EDX 和 FTIR 分析

对可追溯到公元前 7 世纪并从意大利南部出土的古代陶瓷陶器碎片进行了微观结构和孔隙率 (SEM)、元素组成 (EDX)、化学键和矿物成分 (FTIR) 分析,以建立与烧制温度、烧制条件和产地有关。EDX 分析的 Si/Al 比显示三大类原材料(伊利石、高岭石和蒙脱石),表明来源不同。在一个样品中首次报道了均匀大小的二氧化硅纳米颗粒(直径为 0.7 微米)和痕量银。在某些样品中通过 FTIR 检测到钙长石矿物和石英包裹体。所有样品都显示出明显的 Si-O 拉伸带,从 1062 cm-1 偏移,变宽并出现双峰,相对于加工温度。FTIR 结果证明三个样品中的二羟基化不完全和未解离的碳酸盐表明烧制温度为 700-800 C,而其他样品烧制温度高于 900 °C。在这三个样品中,只有一个样品在 SEM 图像中的相互连接的玻璃基质之间显示出膨胀的孔隙,表明烧制温度为 1100-1200°C。不存在磁铁矿以及显着的 Fe 和 Mn 含量表明形成了铁锰尖晶石复合物 MnFe2O4,它是造成两个特定样品中黑色光泽效果的原因,并且可以通过 XRD 进一步证实。在这两个样品之一(直径为 1.2 μm)的 SEM 图像中存在大量小孔表明在比另一个样品更高的温度下玻璃化时间延长。然而,磁铁矿是另外两个样品中黑色光泽效果的原因,证明来源不同。因此,SEM-EDX 和 FTIR 结果可以提供对古代陶瓷的烧制条件、光泽装饰和出处的宝贵见解。
更新日期:2020-06-26
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