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Abstract: The analysis of reference materials is a fundamental part of the data analysis process, in particular for XAS experiments. The beamline users and more generally the XAS community can greatly benefit from the availability of a reliable and wide base of reference sample spectra, acquired in standard and well-characterized experimental conditions. On B18, the Core EXAFS beamline at the Diamond Light Source, in the past years we have collected a series of XAS data on well characterized compounds. This work constitutes the base for a reference sample database, available as a data analysis tool to the general XAS community. This data repository aims to complement the bare spectroscopic information with characterisation, preparation, provenance, analysis and bibliographic references, so improving the traceability of the deposited information. This integrated approach is the base of success and wide distribution of data repositories in other fields, and we hope it will provide on one side a precious facility for the training of students and researchers new to the technique, and at the same time encourage the discussion of best practices in the data analysis process. The database will be open to the contribution of experimental data from the user community, and will provide bibliographic reference information and access control.

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Abstract: A combination of X-ray analytical techniques has been used to study the microstructure and corrosion of a 450-year-old cast-iron cannonball fragment from the Mary Rose shipwreck. Using a 3D approach, it has been shown that akaganeite, β-FeO(OH, Cl), starts to appear ˜1.5 mm below the outer surface of the object, occurring selectively around non-contiguous graphite flakes in the microstructure, with no corrosion in graphite-free regions. This spatial analysis has given a new look inside a 450-year-old system, to see how metallographic features interact with local chemical environments to give complex corrosion products, centuries in the making.

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Abstract: Purportedly originating from the late Predynastic–Early Dynastic period of ancient Egyptian civilisation (about 3100 BC), the statuette known as “MacGregor Man” was acquired near the site of Naqada in southern Egypt by the Reverend William MacGregor at the end of the 19th century. The Ashmolean Museum (University of Oxford) subsequently purchased the statuette at the sale of MacGregor’s collection in 1922, and it remains one of the most important items in the museum’s Egyptology collection. However, the authenticity of the statuette has been the focus of fierce scholarly debate since it first came to light. At that time there was little with which the object could be compared and a forger would have little source material to copy: some of its features are consistent with securely provenanced statuettes and figurines that were discovered some time after the appearance of MacGregor Man. Several other aspects have caused others to question whether MacGregor Man is genuine. It is carved from what is widely believed to be a basaltic rock; rare in ancient Egypt and its hardness would have made sculpting such a detailed statue exceedingly difficult with the tools available to ancient stonemasons. Also, there are strong indications that MacGregor Man may have been deliberately damaged, possibly in an effort to artificially “antiquate” the statuette (though other explanations are feasible). Despite the sustained interest in MacGregor Man, no mineralogical analysis of the stone it is sculpted from has been carried out to date. Though it has been visually identified as being most likely a basalt, it has so far been impossible to ascertain even this basic information without removing a sample from and thus damaging the statue. Even a basic understanding of the mineralogy of the sample could prove informative since basaltic composition can be diagnostic for determining the region of its origin. Using energy-dispersive X-ray diffraction (EDXRD) in a back-reflection geometry, a non-destructive technique, high-resolution powder diffraction data from several regions were collected at Diamond Light Source (Didcot, Oxfordshire, U.K.) in February 2019. From these data, despite poor powder averaging (resulting from the large crystallite size), we plan to extract crystallographic information such as the minerals present and unit cell dimensions. This will be compared to published data from known Egyptian basalt samples in an attempt to ascertain whether it is Egyptian in origin. The results of this crystallographic analysis will be presented.

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Abstract: Structural changes of MoO3 thin films deposited on thick copper substrates upon annealing at different temperatures were investigated via ex situ X-Ray Absorption Spectroscopy (XAS). From the analysis of the X-ray Absorption Near-Edge Structure (XANES) pre-edge and Extended X-ray Absorption Fine Structure (EXAFS), we show the dynamics of the structural order and of the valence state. As-deposited films were mainly disordered, and ordering phenomena did not occur for annealing temperatures up to 300 °C. At ~350 °C, a dominant α-MoO3 crystalline phase started to emerge, and XAS spectra ruled out the formation of a molybdenum dioxide phase. A further increase of the annealing temperature to ~500 °C resulted in a complex phase transformation with a concurrent reduction of Mo6+ ions to Mo4+. These original results suggest the possibility of using MoO3 as a hard, protective, transparent, and conductive material in different technologies, such as accelerating copper-based devices, to reduce damage at high gradients.

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Abstract: In this work, the authors investigated MoO3 films with thickness between 30 nm and 1 μm grown at room temperature by solid phase deposition on polycrystalline Cu substrates. Atomic force microscopy, scanning electron microscopy, and scanning tunneling microscopy revealed the presence of a homogenous MoO3 film with a “grainlike” morphology, while Raman spectroscopy showed an amorphous character of the film. Nanoindentation measurements evidenced a coating hardness and stiffness comparable with the copper substrate ones, while Auger electron spectroscopy, x-ray absorption spectroscopy, and secondary electron spectroscopy displayed a pure MoO3 stoichiometry and a work function ΦMoO3 = 6.5 eV, 1.8 eV higher than that of the Cu substrate. MoO3 films of thickness between 30 and 300 nm evidenced a metallic behavior, whereas for higher thickness, the resistance–temperature curves showed a semiconducting character.