High-resolution X-ray diffraction with no sample preparation.
High-resolution X-ray diffraction with no sample preparation.
复制标题
高分辨率X射线衍射，没有样品制备。
DOI：
10.1107/s2053273317008592
复制
发表时间：
2017-07-01
期刊：
影响因子：
--
通讯作者：
Shortland AJ
中科院分区：
文献类型：
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作者：
Hansford GM;Turner SMR;Degryse P;Shortland AJ
展示了一种新的、高分辨率的X射线衍射技术，它可以对未制备的样品进行完全无损、高质量的X射线衍射分析。该方法在表征文化遗产文物方面显示出巨大的潜力。结果表明，在背反射几何结构中实现的能量色散X射线衍射(EDXRD)即使在高分辨率配置下也对样品的形态和位置非常不敏感。这项技术可以对尚未制备的样品进行高质量的X射线衍射分析，因此是完全无损的。这项实验技术是在英国牛津郡钻石光源同步加速器的B18光束线上实现的。这项研究中的大部分实验都是用预先表征的地质材料进行的，以阐明这项新技术的特点并开发分析方法。结果表明，物相识别，精确的晶胞参数的推导和提取岩石样品和其他样品类型的微结构信息。一个特别的亮点是在未经准备的云母片岩样品中确定了一种特定的白云母多型，避免了通常需要进行这种类型鉴定所需的耗时和困难的准备步骤。这项技术在少量化石和考古样本的应用中也得到了演示。采用高分辨率配置的背反射EDXRD在文化遗产文物的结晶分析方面显示出巨大的潜力，用于科学研究，如起源，以及有助于制定保护战略。讨论了将这项技术从同步加速器转移到博物馆的可能性。避免需要从高价值和稀有物体中提取样本是一个非常重要的优势，也适用于其他潜在的研究领域，如古生物学，以及研究样品送回任务带到地球的陨石和行星材料。
A novel, high-resolution X-ray diffraction (XRD) technique that provides completely non-destructive, high-quality XRD analyses of unprepared samples is demonstrated. The method shows great potential in the characterization of cultural heritage artefacts. It is shown that energy-dispersive X-ray diffraction (EDXRD) implemented in a back-reflection geometry is extremely insensitive to sample morphology and positioning even in a high-resolution configuration. This technique allows high-quality X-ray diffraction analysis of samples that have not been prepared and is therefore completely non-destructive. The experimental technique was implemented on beamline B18 at the Diamond Light Source synchrotron in Oxfordshire, UK. The majority of the experiments in this study were performed with pre-characterized geological materials in order to elucidate the characteristics of this novel technique and to develop the analysis methods. Results are presented that demonstrate phase identification, the derivation of precise unit-cell parameters and extraction of microstructural information on unprepared rock samples and other sample types. A particular highlight was the identification of a specific polytype of a muscovite in an unprepared mica schist sample, avoiding the time-consuming and difficult preparation steps normally required to make this type of identification. The technique was also demonstrated in application to a small number of fossil and archaeological samples. Back-reflection EDXRD implemented in a high-resolution configuration shows great potential in the crystallographic analysis of cultural heritage artefacts for the purposes of scientific research such as provenancing, as well as contributing to the formulation of conservation strategies. Possibilities for moving the technique from the synchrotron into museums are discussed. The avoidance of the need to extract samples from high-value and rare objects is a highly significant advantage, applicable also in other potential research areas such as palaeontology, and the study of meteorites and planetary materials brought to Earth by sample-return missions.