ORCID Profile
0000-0001-6111-339X
Current Organisation
University of Oxford
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Publisher: Springer Science and Business Media LLC
Date: 03-12-2021
DOI: 10.1038/S41467-021-27224-5
Abstract: Small ion-irradiation-induced defects can dramatically alter material properties and speed up degradation. Unfortunately, most of the defects irradiation creates are below the visibility limit of state-of-the-art microscopy. As such, our understanding of their impact is largely based on simulations with major unknowns. Here we present an x-ray crystalline microscopy approach, able to image with high sensitivity, nano-scale 3D resolution and extended field of view, the lattice strains and tilts in crystalline materials. Using this enhanced Bragg ptychography tool, we study the damage helium-ion-irradiation produces in tungsten, revealing a series of crystalline details in the 3D s le. Our results lead to the conclusions that few-atom-large ‘invisible’ defects are likely isotropic in orientation and homogeneously distributed. A partially defect-denuded region is observed close to a grain boundary. These findings open up exciting perspectives for the modelling of irradiation damage and the detailed analysis of crystalline properties in complex materials.
Publisher: Springer Science and Business Media LLC
Date: 06-04-2017
DOI: 10.1038/SREP45993
Abstract: Focussed Ion Beam (FIB) milling is a mainstay of nano-scale machining. By manipulating a tightly focussed beam of energetic ions, often gallium (Ga + ), FIB can sculpt nanostructures via localised sputtering. This ability to cut solid matter on the nano-scale revolutionised s le preparation across the life, earth and materials sciences. Despite its widespread usage, detailed understanding of the FIB-induced structural damage, intrinsic to the technique, remains elusive. Here we examine the defects caused by FIB in initially pristine objects. Using Bragg Coherent X-ray Diffraction Imaging (BCDI), we are able to spatially-resolve the full lattice strain tensor in FIB-milled gold nano-crystals. We find that every use of FIB causes large lattice distortions. Even very low ion doses, typical of FIB imaging and previously thought negligible, have a dramatic effect. Our results are consistent with a damage microstructure dominated by vacancies, highlighting the importance of free-surfaces in determining which defects are retained. At larger ion fluences, used during FIB-milling, we observe an extended dislocation network that causes stresses far beyond the bulk tensile strength of gold. These observations provide new fundamental insight into the nature of the damage created and the defects that lead to a surprisingly inhomogeneous morphology.
Publisher: American Association for the Advancement of Science (AAAS)
Date: 02-09-2016
Abstract: Coherent electron dynamics in a periodic array of C 60 molecular targets driven by intense x-ray pulses of femtosecond duration.
Publisher: American Physical Society (APS)
Date: 15-09-2021
Publisher: Springer Science and Business Media LLC
Date: 21-06-2022
DOI: 10.1557/S43578-022-00613-2
Abstract: Understanding the mechanisms of plasticity in structural steels is essential for the operation of next-generation fusion reactors. This work on the deformation behaviour of FeCr, focusses on distinguishing the nucleation of dislocations to initiate plasticity, from their propagation through the material. Fe3Cr, Fe5Cr, and Fe10Cr were irradiated with 20 MeV Fe 3+ ions at room temperature to doses of 0.008 dpa and 0.08 dpa. Nanoindentation was then carried out with Berkovich and spherical indenter tips. Our results show that the nucleation of dislocations is mainly from pre-existing sources, which are not significantly affected by the presence of irradiation defects or Cr%. Yield strength, an indicator of dislocation mobility, increases with irradiation damage and Cr content, while work hardening capacity decreases mainly due to irradiation defects. The synergistic effects of Cr and irradiation damage in FeCr appear to be more important for the propagation of dislocations than for their nucleation.
Publisher: International Union of Crystallography (IUCr)
Date: 19-02-2021
DOI: 10.1107/S1600577520016264
Abstract: Focused ion beam (FIB) techniques are commonly used to machine, analyse and image materials at the micro- and nanoscale. However, FIB modifies the integrity of the s le by creating defects that cause lattice distortions. Methods have been developed to reduce FIB-induced strain however, these protocols need to be evaluated for their effectiveness. Here, non-destructive Bragg coherent X-ray diffraction imaging is used to study the in situ annealing of FIB-milled gold microcrystals. Two non-collinear reflections are simultaneously measured for two different crystals during a single annealing cycle, demonstrating the ability to reliably track the location of multiple Bragg peaks during thermal annealing. The thermal lattice expansion of each crystal is used to calculate the local temperature. This is compared with thermocouple readings, which are shown to be substantially affected by thermal resistance. To evaluate the annealing process, each reflection is analysed by considering facet area evolution, cross-correlation maps of the displacement field and binarized morphology, and average strain plots. The crystal's strain and morphology evolve with increasing temperature, which is likely to be caused by the diffusion of gallium in gold below ∼280°C and the self-diffusion of gold above ∼280°C. The majority of FIB-induced strains are removed by 380–410°C, depending on which reflection is being considered. These observations highlight the importance of measuring multiple reflections to unambiguously interpret material behaviour.
Publisher: Springer Science and Business Media LLC
Date: 12-11-2013
DOI: 10.1038/NCOMMS3774
Abstract: Understanding and controlling the behaviour of dislocations is crucial for a wide range of applications, from nano-electronics and solar cells to structural engineering alloys. Quantitative X-ray diffraction measurements of the strain fields due to in idual dislocations, particularly in the bulk, however, have thus far remained elusive. Here we report the first characterization of a single dislocation in a freestanding GaAs/In0.2Ga0.8As/GaAs membrane by synchrotron X-ray micro-beam Laue diffraction. Our experimental X-ray data agrees closely with textbook anisotropic elasticity solutions for dislocations, providing one of few experimental validations of this fundamental theory. On the basis of the experimental uncertainty in our measurements, we predict the X-ray beam size required for three-dimensional measurements of lattice strains and rotations due to in idual dislocations in the material bulk. These findings have important implications for the in situ study of dislocation structure formation, self-organization and evolution in the bulk.
Publisher: International Union of Crystallography (IUCr)
Date: 2017
DOI: 10.1107/S1600577516017525
Abstract: The proliferation of extremely intense synchrotron sources has enabled ever higher-resolution structures to be obtained using data collected from smaller and often more imperfect biological crystals (Helliwell, 1984). Synchrotron beamlines now exist that are capable of measuring data from single crystals that are just a few micrometres in size. This provides renewed motivation to study and understand the radiation damage behaviour of small protein crystals. Reciprocal-space mapping and Bragg coherent diffractive imaging experiments have been performed on cryo-cooled microcrystals of hen egg-white lysozyme as they undergo radiation damage. Several well established metrics, such as intensity-loss and lattice expansion, are applied to the diffraction data and the results are compared with several new metrics that can be extracted from the coherent imaging experiments. In idually some of these metrics are inconclusive. However, combining metrics, the results suggest that radiation damage behaviour in protein micro-crystals differs from that of larger protein crystals and may allow them to continue to diffract for longer. A possible mechanism to account for these observations is proposed.
Publisher: Elsevier BV
Date: 2023
Publisher: International Union of Crystallography (IUCr)
Date: 06-09-2022
DOI: 10.1107/S1600576722007646
Abstract: Bragg coherent X-ray diffraction imaging (BCDI) allows the 3D measurement of lattice strain along the scattering vector for specific microcrystals. If at least three linearly independent reflections are measured, the 3D variation of the full lattice strain tensor within the microcrystal can be recovered. However, this requires knowledge of the crystal orientation, which is typically attained via estimates based on crystal geometry or synchrotron microbeam Laue diffraction measurements. Presented here is an alternative method to determine the crystal orientation for BCDI measurements using electron backscatter diffraction (EBSD) to align Fe–Ni and Co–Fe alloy microcrystals on three different substrates. The orientation matrix is calculated from EBSD Euler angles and compared with the orientation determined using microbeam Laue diffraction. The average angular mismatch between the orientation matrices is less than ∼6°, which is reasonable for the search for Bragg reflections. The use of an orientation matrix derived from EBSD is demonstrated to align and measure five reflections for a single Fe–Ni microcrystal via multi-reflection BCDI. Using this data set, a refined strain field computation based on the gradient of the complex exponential of the phase is developed. This approach is shown to increase accuracy, especially in the presence of dislocations. The results demonstrate the feasibility of using EBSD to pre-align BCDI s les and the application of more efficient approaches to determine the full lattice strain tensor with greater accuracy.
Publisher: Royal Society of Chemistry (RSC)
Date: 2022
DOI: 10.1039/D1CE01586A
Abstract: Morphology, 3D lattice strain, and dissolution of a Co–Fe microcrystal was monitored using in situ Bragg coherent X-ray diffraction imaging.
Publisher: American Physical Society (APS)
Date: 24-11-2020
Publisher: AIP Publishing
Date: 29-04-2015
DOI: 10.1063/1.4919641
Abstract: For laboratory and synchrotron based X-ray sources, radiation damage has posed a significant barrier to obtaining high-resolution structural data from biological macromolecules. The problem is particularly acute for micron-sized crystals where the weaker signal often necessitates the use of higher intensity beams to obtain the relevant data. Here, we employ a combination of techniques, including Bragg coherent diffractive imaging to characterise the radiation induced damage in a micron-sized protein crystal over time. The approach we adopt here could help screen for potential protein crystal candidates for measurement at X-ray free election laser sources.
Location: United States of America
Location: United Kingdom of Great Britain and Northern Ireland
Start Date: 2019
End Date: 2022
Funder: Engineering and Physical Sciences Research Council
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