Investigation of the X‐ray fluorescence technique in the characterization of Ni coatings applied to historical heritage studies

IF 1.5 4区 物理与天体物理 Q3 SPECTROSCOPY X-Ray Spectrometry Pub Date : 2024-05-04 DOI:10.1002/xrs.3429
Paula Silveira, Hugo Marcelo Veit, Johnny Dias, Tiago Falcade
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Abstract

Historical heritage pieces allow a better comprehension of the characteristics of different civilizations over time. The characterization of such pieces is of paramount importance for their preservation. Energy‐dispersive X‐ray fluorescence (EDXRF) is recommended for this application, mostly because it is non‐destructive and the equipment is portable. However, one of its limitations is the difficulty in separating the signal from the substrate and the coating of multilayered samples, as it does not provide depth resolution. This project investigates the application of EDXRF in the characterization of metallic coatings, in the context of historical heritage. The elemental concentration of electrodeposited Ni coatings onto carbon steel substrates was obtained from EDXRF analyses. The relationship between the layer thickness and the variation of the Kα/Kβ intensity ratio of nickel peaks was exploited and the thicknesses of the coatings were estimated through EDXRF measurements. For comparison, particle‐induced x‐ray emission spectroscopy and scanning electron microscopy of the cross‐section were employed, providing a depth profile of the coatings. The estimated thicknesses from EDXRF analysis were comparable to those observed in the microscopy images for thinner films (up to 8 μm). On the other hand, for thicker films, the thicknesses were underestimated, due to the technique's depth limit and matrix effects, as secondary absorption. Despite these limitations, EDXRF remains valuable for evaluating cultural heritage pieces, often providing sufficient information to address authenticity concerns or to guide restoration processes. A case study was also performed to apply the methodology discussed on historical metallic pieces.
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X 射线荧光技术在历史遗产研究中应用于镍涂层表征的研究
历史遗产可以让人们更好地了解不同文明在不同时期的特征。对这些文物进行鉴定对其保护至关重要。能量色散 X 射线荧光 (EDXRF) 被推荐用于这种应用,主要是因为它是非破坏性的,而且设备便于携带。然而,其局限性之一是难以将信号从多层样品的基底和涂层中分离出来,因为它无法提供深度分辨率。本项目以历史遗产为背景,研究了电离辐射 X 射线荧光光谱在金属涂层表征中的应用。通过 EDXRF 分析获得了碳钢基底上电解沉积镍涂层的元素浓度。利用镀层厚度与镍峰 Kα/Kβ 强度比值变化之间的关系,通过 EDXRF 测量估算了镀层厚度。为了进行比较,还使用了粒子诱导 X 射线发射光谱和横截面扫描电子显微镜,以提供涂层的深度剖面图。对于较薄的薄膜(最厚 8 μm),EDXRF 分析得出的估计厚度与显微镜图像中观察到的厚度相当。另一方面,对于较厚的薄膜,由于该技术的深度限制和基质效应(二次吸收),厚度被低估了。尽管存在这些局限性,EDXRF 对于评估文化遗产仍然很有价值,通常可以提供足够的信息来解决真实性问题或指导修复过程。我们还进行了一项案例研究,将所讨论的方法应用于历史上的金属文物。
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来源期刊
X-Ray Spectrometry
X-Ray Spectrometry 物理-光谱学
CiteScore
3.10
自引率
8.30%
发文量
38
审稿时长
6-12 weeks
期刊介绍: X-Ray Spectrometry is devoted to the rapid publication of papers dealing with the theory and application of x-ray spectrometry using electron, x-ray photon, proton, γ and γ-x sources. Covering advances in techniques, methods and equipment, this established journal provides the ideal platform for the discussion of more sophisticated X-ray analytical methods. Both wavelength and energy dispersion systems are covered together with a range of data handling methods, from the most simple to very sophisticated software programs. Papers dealing with the application of x-ray spectrometric methods for structural analysis are also featured as well as applications papers covering a wide range of areas such as environmental analysis and monitoring, art and archaelogical studies, mineralogy, forensics, geology, surface science and materials analysis, biomedical and pharmaceutical applications.
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