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High-resolution X-ray diffraction with no sample preparation

DOI: 10.1107/S2053273317008592 DOI Help

Authors: G. M. Hansford (University of Leicester) , S. M. R. Turner (University of Leicester) , P. Degryse (K.U. Leuven) , A. J. Shortland (Cranfield University)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Acta Crystallographica Section A Foundations And Advances , VOL 73 , PAGES 293 - 311

State: Published (Approved)
Published: July 2017
Diamond Proposal Number(s): 10145

Open Access Open Access

Abstract: 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 XRD 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-characterised 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.

Journal Keywords: energy-dispersive XRD; back-reflection geometry; sample preparation; non-destructive analysis; cultural heritage artefacts; synchrotron experiments

Subject Areas: Technique Development, Archaeological and Cultural Heritage, Materials

Instruments: B18-Core EXAFS