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Instruments / Technical Area	Publication Details	Published	Actions
B18-Core EXAFS I11-High Resolution Powder Diffraction I12-JEEP: Joint Engineering, Environmental and Processing	Influence of microstructure on the corrosion of archaeological iron observed using 3D synchrotron micro-tomography H. J. Simon , G. Cibin , C. Reinhard , Y. Liu , E. Schofield , I. C. Freestone Corrosion Science DOI: 10.1016/j.corsci.2019.108132 Diamond Proposal Number(s): [16863, 16328] Show Abstract ▼ 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.	Aug 2019
B18-Core EXAFS I11-High Resolution Powder Diffraction	A Synchrotron-based study of the Mary Rose iron cannonballs Hayley Simon , Giannantonio Cibin , Phil Robbins , Sarah Day , Chiu Tang , Ian Freestone , Eleanor Schofield Angewandte Chemie International Edition 30 DOI: 10.1002/anie.201713120 Diamond Proposal Number(s): [16328] Open Access Show Abstract ▼ Abstract: Post-excavation iron corrosion may be accelerated by the presence of Cl−, leading to conservation methods designed to remove Cl. This study exploits a unique opportunity to assess 35 years of conservation applied to cast-iron cannon shot excavated from the Mary Rose. A combination of synchrotron X-ray powder diffraction (SXPD), absorption spectroscopy (XAS), and fluorescence (XRF) mapping have been used to characterise the impact of conservation on the crystalline corrosion products, chlorine distribution, and speciation. The chlorinated phase akaganeite, β-FeO(OH,Cl), was found on shot washed in corrosion inhibitor Hostacor IT with or without an additional reduction stage. No chlorinated phases were observed on the surface of shot stored in sodium sesquicarbonate (Na2CO3/NaHCO3); however, hibbingite, β-Fe2(OH)3Cl, was present in metal pores. It is proposed that surface β-FeO(OH,Cl) formed in the early stages of active conservation owing to oxidation of β-Fe2(OH)3Cl at near-neutral pH.	Mar 2018

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