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Instruments / Technical Area	Publication Details	Published
I13-2-Diamond Manchester Imaging	4D synchrotron X-ray microtomography of fracture in nuclear graphite after neutron irradiation and radiolytic oxidation J. Wade-zhu , R. Krishna , A. J. Bodey , M. Davies , N. K. Bourne , C. Rau , B. Davies , A. Tzelepi , A. N. Jones , B. J. Marsden , P. M. Mummery Carbon DOI: 10.1016/j.carbon.2020.06.051 Diamond Proposal Number(s): [16668] Show Abstract ▼ Abstract: Herein, the first study is presented using 4D synchrotron X-ray microtomography to capture all stages of crack development in neutron irradiated and radiolytically oxidised nuclear graphite. Employing a novel loading setup, specimens of Gilsocarbon graphite, both unirradiated and irradiated at 301 °C to 19.7 × 1020 neutrons/cm2 (∼2.6 displacements/atom (dpa)), were loaded to generate a crack. All stages of the fracture process were then captured using synchrotron X-ray imaging. Reconstructed tomographic images and 3D segmented crack volumes have been used to observe and analyse the irradiation-induced evolution of the graphite microstructure as well as corresponding changes in the crack initiation, propagation, and arrest behaviour of graphite after neutron irradiation. Close examination of the applied stress-strain curves highlights the suppression of micro-crack-based damage accumulation in irradiated graphite. Moreover, as well as the crack-bridging and deflection mechanisms characteristic of unirradiated graphite, crack arrest in the irradiated graphite is shown to be significantly influenced by crack tip blunting. This change is associated with the growth of the open pore structure of graphite, specifically the enlargement and increased frequency of macro-pores, resulting from the simultaneous radiolytic oxidation of the graphite microstructure during neutron irradiation.	Jul 2020
I13-2-Diamond Manchester Imaging	The Diamond I13 full-field transmission X-ray microscope: a Zernike phase-contrast setup for material sciences Malte Storm , Florian Doring , Shashidhara Marathe , Christian David , Christoph Rau Powder Diffraction 425, 1 - 7 DOI: 10.1017/S0885715620000238 Diamond Proposal Number(s): [19746, 24892] Open Access Show Abstract ▼ Abstract: The I13 transmission X-ray microscope at Diamond Light Source (DLS) has been designed to cover a broad range of energies and field of views. The beamline operates on an undulator source, and a multilayer monochromator can be used to work at a larger bandwidth to enable faster acquisitions. The experimental design includes large working distances for the optics to allow installing in situ sample environments. This paper presents the current state of the experimental system and shows some of the latest results.	Apr 2020
I13-2-Diamond Manchester Imaging	Development of synchrotron pink beam x-ray grating interferometer at the Diamond Light source I13-2 beamline Shashidhara Marathe , Malte Storm , Venkata Sree Charan Kuppilli , Richard Harrison , Gunjan Das , Sven L. M. Schroeder , Silvia Cipiccia , Florian Doring , Christian David , Christoph Rau SPIE Optical Engineering + Applications, 2019 DOI: 10.1117/12.2530698 Diamond Proposal Number(s): [21327] Open Access Show Abstract ▼ Abstract: X-ray Grating Talbot Interferometer (XGTI) is already routinely used for quantitative phase contrast imaging of soft tissue samples. XGTI can be realized using various measurement techniques, depending on the X-ray source used, the required spatial resolution and the speed of acquisition. The phase-stepping measurement technique, which is commonly used for XGTI data acquisition, needs multiple acquisitions for a single projection. For fast imaging the Moiré technique, a single-shot technique, is often preferred. However, it requires two gratings which increases the dose on the sample. We have therefore examined the Spatial Harmonic Imaging (SHI) technique which is low-dose and single-shot, using the I13-2 Diamond-Manchester Beamline at Diamond Light Source (DLS). The DLS I13-2 beamline is equipped with a Double Crystal Monochromator (DCM) and a Multi-Layer Monochromator (MLM) to deliver monochromatic beam, which work at the energy bandwidths (ΔE/E) of 10-4 and 10-2, respectively. However, the disadvantage of using these monochromators, especially for fast imaging, is loss of X-ray flux. It has already been shown that XGTI can work with an energy bandwidth (ΔE/E) of 10-1. Our aim is to develop a single phase grating interferometer with pink beam from an undulator source, with X-ray mirror optics and multiple absorption filters, to obtain maximum possible flux with sufficient coherence and monochromaticity. We demonstrate performance with optimized beamline parameters for a photon energy of 15 keV with some demonstrative image reconstructions.	Oct 2019
I13-1-Coherence I13-2-Diamond Manchester Imaging	New imaging opportunities at the Diamond beamline I13L Christoph Rau , Darren Batey , Silvia Cipiccia , Xiaowen Shi , Shashidhara Marathe , Malte Storm , Andrew J. Bodey , Marie-christine Zdora SPIE Optical Engineering + Applications, 2019 DOI: 10.1117/12.2543799 Open Access Show Abstract ▼ Abstract: The Diamond Beamline I13L is dedicated to micro- and nano- imaging, with two independently operating branchlines. The imaging branch preforms imaging in real space, with In-line phase contrast imaging and grating interferometry at micrometre resolution and full-field transmission microscopy up to 50nm spatial resolution. Highest spatial resolution is achieved on the coherence branchline, where diffraction imaging methods such as Ptychography and Bragg-CDI are performed. The article provides an update about the experimental capabilities at the beamline with an emphasis on the rapidly evolving ptychography capabilities. The latter has evolved to an user-friendly method with non-expert users able to explore their science without any specific a-priory knowledge.	Oct 2019
I13-1-Coherence I13-2-Diamond Manchester Imaging	Fast multi-scale imaging using the beamline I13L at the Diamond Light Source Christoph Rau , Malte Storm , Shashidhara Marathe , Andrew J. Bodey , Marie-christine Zdora , Silvia Cipiccia , Darren Batey , Xiaowen Shi , Sven Schroeder , Gunjan Das , Melanie Loveridge , Ralf Ziesche , Brian Connolly SPIE Optical Engineering + Applications, 2019 DOI: 10.1117/12.2543405 Open Access Show Abstract ▼ Abstract: The DIAMOND beamline I13L is dedicated to multi-scale and multi-modal imaging in real and reciprocal space. The beamline consists of two independently operating experimental stations, located at a distance of more than 200 m from the source. The Imaging Branch performs micro-tomography with in-line phase contrast in the 6-30 keV energy range. In addition, a grating interferometry setup and a full-field microscope for nano-tomography are currently implemented. Other techniques providing high-resolution three-dimensional information, in particular coherent X-ray diffraction, are hosted on the Coherence Branch. All imaging methods are tested to operate with large energy bandwidths and therefore shorter exposure times. To this end, two options are currently used: the so-called ‘pink-beam’ mode using a reflecting mirror and X-ray filters and monochromatic mode using a multilayer monochromator. The operation mode enables science for in-situ and operando studies across a wide range of scientific areas.	Oct 2019
I13-1-Coherence	Refractive hard x-ray vortex phase plates Frank Seiboth , Maik Kahnt , Mikhail Lyubomirskiy , Martin Seyrich , Felix Wittwer , Tobias Ullsperger , Stefan Nolte , Darren Batey , Christoph Rau , Christian G. Schroer Optics Letters 44 DOI: 10.1364/OL.44.004622 Diamond Proposal Number(s): [17460] Show Abstract ▼ Abstract: In this Letter, we report on the creation of hard x-ray beams carrying orbital angular momentum of topological charge −ℏ −ℏ and −3ℏ −3ℏ at a photon energy of 8.2 keV via spiral phase plates made out of fused silica by ultrashort-pulsed laser ablation. The phase plates feature a smooth phase ramp with a 0.5 μm nominal step height and a surface roughness of 0.5 μm. The measured vortex beams show submicrometer-sized donut rings and agree well with numerical modeling. Fused silica phase plates are potentially suited to manipulate the electromagnetic field in highly intense x-ray beams at x-ray free-electron laser sources.	Sep 2019
I13-1-Coherence	Spectroscopic imaging with single acquisition ptychography and a hyperspectral detector Darren Batey , Silvia Cipiccia , Frederic Van Assche , Sander Vanheule , Juriaan Vanmechelen , Matthieu N. Boone , Christoph Rau Scientific Reports 9 DOI: 10.1038/s41598-019-48642-y Diamond Proposal Number(s): [22099] Open Access Show Abstract ▼ Abstract: We present a new method of single acquisition spectroscopic imaging with high spatial resolution. The technique is based on the combination of polychromatic synchrotron radiation and ptychographic imaging with a recently developed energy discriminating detector. We demonstrate the feasibility with a Ni-Cu test sample recorded at I13-1 of the Diamond Light Source, UK. The two elements can be clearly distinguished and the Ni absorption edge is identified. The results prove the feasibility of obtaining high-resolution structural and chemical images within a single acquisition using a polychromatic X-ray beam. The capability of resolving the absorption edge applies to a wide range of research areas, such as magnetic domains imaging and element specific investigations in biological, materials, and earth sciences. The method utilises the full available radiation spectrum and is therefore well suited for broadband radiation sources.	Aug 2019
I13-1-Coherence I18-Microfocus Spectroscopy	Provenance of uranium particulate contained within Fukushima Daiichi Nuclear Power Plant Unit 1 ejecta material Peter G. Martin , Marion Louvel , Silvia Cipiccia , Christopher P. Jones , Darren J. Batey , Keith R. Hallam , Ian A. X. Yang , Yukihiko Satou , Christoph Rau , J. Fred W. Mosselmans , David Richards , Thomas B. Scott Nature Communications 10, 2801 DOI: 10.1038/s41467-019-10937-z Diamond Proposal Number(s): [16701, 16702, 18186] Open Access Show Abstract ▼ Abstract: Here we report the results of multiple analytical techniques on sub-mm particulate material derived from Unit 1 of the Fukushima Daiichi Nuclear Power Plant to provide a better understanding of the events that occurred and the environmental legacy. Through combined x-ray fluorescence and absorption contrast micro-focused x-ray tomography, entrapped U particulate are observed to exist around the exterior circumference of the highly porous Si-based particle. Further synchrotron radiation analysis of a number of these entrapped particles shows them to exist as UO2—identical to reactor fuel, with confirmation of their nuclear origin shown via mass spectrometry analysis. While unlikely to represent an environmental or health hazard, such assertions would likely change should break-up of the Si-containing bulk particle occur. However, more important to the long-term decommissioning of the reactors at the FDNPP (and environmental clean-upon), is the knowledge that core integrity of reactor Unit 1 was compromised with nuclear material existing outside of the reactors primary containment.	Jun 2019

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