Major to trace element imaging and analysis of iron age glasses using stage scanning in the analytical dual beam microscope (tandem)

Major to trace element imaging and analysis of iron age glasses using stage scanning in the analytical dual beam microscope (tandem)
复制标题

主要使用分析双光束显微镜(串联)中的阶段扫描对铁器时代玻璃进行微量元素成像和分析

DOI:
10.1186/s40494-022-00707-4
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发表时间:
2022
期刊:
影响因子:
2.5
通讯作者:
C. Pearce
C. Pearce
中科院分区:
化学2区
文献类型:
--
作者:
E. Vicenzi;T. Lam;Jamie L. Weaver;A. Herzing;J. McCloy;R. Sjöblom;C. Pearce

文献摘要

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1500年前在瑞典乌普萨拉附近的布罗堡山堡发生的铁器时代玻璃化事件≈期间形成的暗色和透明硅酸盐玻璃,使用配备微型X射线荧光(μXRF)光谱仪的扫描电子显微镜进行了分析。通过恒速阶段扫描,采集了相关的微束X射线荧光和电子束诱导能谱(EDS)X射线图。这一结合程序代表了文化遗产界对由金属、陶瓷或无机/有机混合材料组成的考古标本进行分析研究的一种新方法,其中主要和微量元素成分在空间中以微米级分辨率登记到厘米长的区域。使用概览图像来选择与多光谱阴极发光(CL)成像相关的EDS光束扫描图以及共定位的定量EDS和μXRF点分析。铁、钙、镁、钛、磷、锰、锆、锌、Y等元素在深色玻璃中富集,而硅、铝、钾、钠、钡、锶、Rb、镓等元素在透明玻璃中富集。未熔融物质主要由石英(SiO_2)以及少量磷灰石(Ca5(PO4)3[Cl,OH])和锆石(ZrSiO4)组成。多变量统计分析用于测量高方差分量的面积分数,而低方差分量表示相混合物。计算的玻璃成分的熔体粘度之间的差异与现场和实验室观察结果一致。结合大面积能谱和μX射线荧光成像显示,在知情选择更高空间分辨率和更高灵敏度的后续研究方面,例如使用同步加速器分析进行的研究,具有重要的前景。图形摘要
Dark and clear silicate glasses formed during an iron age vitrification event ≈ 1500 years ago at the Broborg hillfort near Uppsala, Sweden have been analyzed using a scanning electron microscope equipped with a micro-X-ray fluorescence (μXRF) spectrometer. Correlated µXRF and electron beam-induced energy dispersive spectrometry (EDS) X-ray maps were collected via stage-scanning at constant velocity. This coupled procedure represents a new approach for the cultural heritage community to conduct analytical studies of archaeometric specimens composed of metal, ceramic, or mixed inorganic/organic materials, where major and trace element compositions are registered in space for areas up to the centimeter-length scale at micrometer-scale resolution. Overview images were used to select areas for EDS beam scan maps correlated with multispectral cathodoluminescence (CL) imaging and co-located quantitative EDS and μXRF point analysis. Fe, Ca, Mg, Ti, P, Mn, Zr, Zn, and Y are enriched in the dark glass, while Si, Al, K, Na, Ba, Sr, Rb, and Ga are enriched in the clear glass. Unmelted material is comprised predominately of quartz (SiO 2 ) along with trace apatite (Ca 5 (PO 4 ) 3 [Cl,OH]) and zircon (ZrSiO 4 ). Multivariate statistical analysis was used to measure the area fractions of high variance components while lower variance components represented phase mixtures. Differences between calculated melt viscosities for the glass compositions are consistent with field and laboratory observations. Coupled large area EDS and μXRF imaging shows significant promise for informed selection of higher spatial resolution and higher sensitivity follow-up studies, e.g., those performed using synchrotron analysis. Graphical Abstract