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Instruments / Technical Area	Publication Details	Published
I18-Microfocus Spectroscopy	Radiation damage effects in chlorite investigated using microfocus synchrotron techniques William Bower , Carolyn I. Pearce , Andrew D. Smith , Simon M. Pimblott , J. Frederick W. Mosselmans , Richard A. D. Pattrick Acs Earth And Space Chemistry DOI: 10.1021/acsearthspacechem.8b00205 Diamond Proposal Number(s): [9044, 9598] Open Access Show Abstract ▼ Abstract: A detailed understanding of the mechanisms and effects of radiation damage in phyllosilicate minerals is a necessary component of the evaluation of the safety case for a deep geological disposal facility (GDF) for radioactive waste. Structural and chemical changes induced by α-particle damage will affect these mineral’s performance as a reactive barrier material (both in the near and far-field) over timescales relevant to GDF integrity. In this study, two examples of chlorite group minerals have been irradiated at α-particle doses comparable to those predicted to be experienced by the clay buffer material surrounding high level radioactive waste canisters. Crystallographic aberrations induced by the focused 4He2+ ion beam are revealed via high-resolution, microfocus X-ray diffraction mapping. Interlayer collapse by up to 0.5 Å is prevalent across both macro- and micro-crystalline samples, with the macro-crystalline specimen displaying a breakdown of the phyllosilicate structure into loosely-connected, multi-oriented crystallites displaying variable lattice parameters. The damaged lattice parameters suggest a localised breakdown and collapse of the OH- rich, ‘brucite-like’ interlayer. Microfocus Fe K-edge X-ray absorption spectroscopy illustrates this defect accumulation, manifest as a severe damping of the X-ray absorption edge. Subtle Fe2+/Fe3+ speciation changes are apparent across the damaged structures. A trend towards Fe reduction is evident at depth in the damaged structures at certain doses (8.76 x 1015 alpha particles/ cm2). Interestingly, this reductive trend does not increase with radiation dose, indeed at the maximum dose (1.26 x 1016 alpha particles/ cm2) administered in this study, there is evidence for a slight increase in Fe binding energy, suggesting the development of a depth-dependant redox gradient concurrent with light ion damage. At the doses examined here, these damaged structures are likely highly reactive, as sorption capacity will, to an extent, be largely enhanced by lattice disruption and an increase in available ‘edge’ sites.	Feb 2019
B18-Core EXAFS I18-Microfocus Spectroscopy	Radiation damage in biotite mica by accelerated α-particles: A synchrotron microfocus X-ray diffraction and X-ray absorption spectroscopy study William Bower , Carolyn Pearce , Andrew Smith , Simon Pimblott , Fred Mosselmans , Sarah Haigh , James Mckinley , Richard Pattrick American Mineralogist 101, 928 - 942 DOI: 10.2138/am-2016-5280CCBYNCND Diamond Proposal Number(s): [9044, 9598, 9647] Open Access Show Abstract ▼ Abstract: A critical radiation damage assessment of the materials that will be present in a Geological Disposal Facility (GDF) for radioactive waste is a priority for building a safety case. Detailed analysis of the effects of high-energy a -particle damage in phyllosilicates such as mica is a necessity, as these are model structures for both the clay-based backfill material and the highly sorbent components of a crystalline host rock. The a -radiation stability of biotite mica [general formula: K(Mg,Fe)3(Al,Si3O10)(F,OH)2 ] has been investigated using the 5 MV tandem pelletron at the University of Manchester’s Dalton Cumbrian Facility (DCF) and both the microfocus spectroscopy (I18) and core X -ray absorption spectroscopy (B18) beamlines at Diamond Light Source (U.K.). Microfocus X-ray diffraction mapping has demonstrated extensive structural aberrations in the mica resulting from controlled exposure to the focused 4He2+ ion (a-particle) beam. Delivered doses were comparable to a-particle fluences expected in the highly active, near-field of a GDF. At doses up to 6.77 displacements per atom (dpa) in the region of highest particle fluence, biotite mica displays a heterogeneous structural response to irradiation on a micrometer scale, with sequential dilation and contraction of regions of the structure perpendicular to the sheets, as well as a general overall contraction of the phyllosilicate layer spacing. At the peak of ion fluence, the structure collapses under a high point defect density and amorphous areas are pervasive among altered domains of the original lattice. Such structural alterations are likely to affect the material’s capacity to sorb and retain escaped radionuclides over long timescales; increased edge site availability may favor increased sorption while interlayer uptake will likely be reduced due to collapse. Radiation-induced reduction of structural iron at the region of highest structural damage across an a-particle’s track has been demonstrated by Fe K-edge X-ray absorption near edge spectroscopy (XANES) and local structural disorder has been confirmed by analysis of both potassium K-edge XANES and Fe K-edge extended X-ray absorption fine structure analysis. An infrared absorption study of deformations in the OH– stretching region, along with electron probe microanalysis complements the synchrotron data presented here	Apr 2016
I18-Microfocus Spectroscopy	Development of irradiation capabilities to address the challenges of the nuclear industry L. Leay , W. Bower , G. Horne , P. Wady , A. Baidak , M. Pottinger , M. Nancekievill , A. D. Smith , S. Watson , P. R. Green , B. Lennox , J. A. Laverne , S. M. Pimblott Nuclear Instruments And Methods In Physics Research Section B: Beam Interactions With Materials And Atoms 343, 62 - 69 DOI: 10.1016/j.nimb.2014.11.028 Diamond Proposal Number(s): [9044] Show Abstract ▼ Abstract: With the announcement of the U.K. new nuclear build and the requirement to decommission old facilities, researchers require bespoke facilities to undertake experiments to inform decision making. This paper describes development of The University of Manchester’s Dalton Cumbrian Facility, a custom built research environment which incorporates a 5 MV tandem ion accelerator as well as a self-shielded 60Co irradiator. The ion accelerator allows the investigation into the radiolytic consequences of various charged particles, including protons, alpha particles and a variety of heavier (metal and nonmetal) ions, while the 60Co irradiator allows the effects of gamma radiation to be studied. Some examples of work carried out at the facility are presented to demonstrate how this equipment can improve our mechanistic understanding of various aspects of the deleterious effects of radiation in the nuclear industry. These examples include applications in waste storage and reprocessing as well as geological storage and novel surveying techniques. The outlook for future research is also discussed.	Jan 2015

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