DIAD-Dual Imaging and Diffraction Beamline
I11-High Resolution Powder Diffraction
I12-JEEP: Joint Engineering, Environmental and Processing
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Open Access
Abstract: The plumes of Enceladus contain a non-ice component that originates from aqueous processes occurring within the interior 1,2. The ocean of Enceladus is thought to be connected to the surface across a range of time scales. These processes range from the rapid eruption of cryovolcanic plumes to slow crustal convection on geological timescales3,4. In every case, the system will have a temperature and geochemical evolution as it freezes, with the history of evolution recorded in the sequence of mineral precipitation. Analogously to igneous and metamorphic petrology, we can explore the mineralogy and its context to reconstruct the history of that sample. Most importantly, for astrobiological investigations, the formation and cryo-petrological study of inorganic salts can be used to identify sites of recent exposure on the surface.
Synchrotron X-ray techniques allow fast, high-resolution probing of these systems with X-ray light. By exploring large, multi-component samples with multiple techniques, with variable temperature over time we can reveal many emergent processes that may not be predictable with simple phase diagrams.
We use a combination of synchrotron powder X-ray diffraction (PXRD) and X-ray microtomography (µCT) across multiple beamlines at Diamond Light Source (I11, I12 and DIAD). Using a multi-modal approach, we present an in-situ study of the low-temperature phase behaviour of Na-Cl-HCO3 fluids. We employ K11-DIAD (Dual Imaging and Diffraction) to carry out ‘image-guided diffraction’ on an Enceladus-type sample frozen in real-time. DIAD’s unique capabilities allow us not only to study microstructure down to 1 µm but also to carry out spatially resolved XRD and identify solid phases present.
We present, for the first time, the use of dual imaging and diffraction of a Na-Cl-CO₃ solution frozen in real time in 3 dimensions [Figure 1]. DIAD’s imaged guided diffraction provides spatially-resolved XRD, allowing us to probe different regions of our sample and identify the formation of Na2CO₃ hydrates. We show the influence of carbonate chemistry on the sequence of cryogenic precipitation and the development of complex microstructures. These results provide insights into crustal transport processes and will help with interpreting observational data from upcoming Galilean missions.
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Sep 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Jiaxu
Zuo
,
Kutsi
Akcicek
,
Shivansh
Nauriyal
,
Barrie
Dams
,
Stefan
Michalik
,
Thomas
Zillhardt
,
Martin
Ansell
,
Richard
Ball
,
Genoveva
Burca
,
Brian
Sheil
,
James
Marrow
,
Sinan
Acikgoz
Open Access
Abstract: Fibrous plaster (FP) ceilings, prevalent in late 19th- and early 20th-century UK theatres, are suspended using ‘wads’. Wads are hangers made of Plaster of Paris, reinforced with twisted woven jute fabric. Several recent collapses in historic fibrous plaster ceilings have been attributed to tensile failures in wads. To understand the failure mechanisms involved, tensile tests were performed on laboratory-produced wad-like samples at the I12 beamline of the UK Diamond Light Source. The tested samples were designed with a dog bone shape and mounted with clevis-grips at each end, to ensure controlled failures along the gauge length. The beamline offered the opportunity to conduct simultaneous synchrotron X-ray computed tomography (sCT) and diffraction measurements during loading, enabling the monitoring of internal crack formation and strain propagation at the microstructural scale. Simultaneously, acoustic emission (AE) and digital image correlation (DIC) measurements were conducted. Preliminary results from these datasets are discussed in this paper. The datasets will provide useful information to validate the ongoing development of algorithms which can categorise the internal failure mechanisms and damage state of wads using only AE signals.
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Sep 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[34953]
Open Access
Abstract: We use in situ synchrotron X-ray diffraction measurements to monitor the solvothermal crystallization mechanism of the aperiodic metal–organic framework TRUMOF-1. Following an initial incubation period, TRUMOF-1 forms as a metastable intermediate that subsequently transforms into an ordered product with triclinic crystal symmetry. We determine the structure of this ordered phase, which we call msw-TRUMOF-1, and show that it is related to TRUMOF-1 through topotactic reorganization of linker occupancies. Our results imply that the connectivity of TRUMOF-1 can be reorganized, as required for data storage and manipulation applications.
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Sep 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[24327]
Open Access
Abstract: We have assessed the elasto-plastic (sub)surface behaviour of 7050-T7451 aluminium alloy treated by shot peening using S110 steel shots of 300 μm in diameter and two different intensities, namely Almen intensity (A) of 3.4 (low-intensity) and 10.9 (high-intensity). Shot peening (SP) is a cold work process applied in the aerospace industry to enhance the fatigue tolerance of structural components after machining. The local mechanical response within the SP-induced layer was depth profiled at room temperature by performing an X-ray micro-diffraction experiment in transmission geometry at a synchrotron source, during tensile loading of the specimen to rupture. The presence of a SP-induced layer in the specimen is evidenced by compressive longitudinal lattice strains (∼-540 με for low-intensity and ∼-4200 με for high-intensity at 0.1 mm from the surface for the 311 reflection), parallel with respect to the applied load, i.e. perpendicular to the direction of impact of the steel shots, and also by higher values of the Full-Width-at-Half-Maximum (FWHM) of the diffraction peaks than those measured in the bulk material, due to the local plastic deformation induced by shot peening. High-intensity shot peening produced a higher surface roughness (Sa ∼13 μm), and also two times thicker deformed surface layer (∼0.4 mm), than low-intensity shot peening (Sa ∼2 μm and ∼0.2 mm thick deformed layer). For both shot peening conditions, the local yield stress of the surface layer and bulk material were similar, however the severely affected layers exhibit a non-linear elastic behaviour when applying loads lower than the yield stress of the material. Beyond yielding, the presence of SP-induced layers is mainly evidenced by the relatively higher value of the FWHM near-surface compared to the bulk (∼20 % higher for low-intensity and ∼40 % for high-intensity), due to the initial plastic deformation accumulated during shot peening and additional plasticity during loading of the specimen.
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Sep 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[24084]
Abstract: Microstructure-informed crystal plasticity finite element models have shown great promise in predicting plastic and creep deformation in polycrystalline materials. These models can provide substantial insight into the design, fabrication and lifetime assessment of critical metallic components during operation, for instance, in thermal power plants. However, to correctly incorporate damage prediction into models, the microstructural strain simulated at the grain level must be accurately predicted with suitable validation. For this reason, a 3D X-ray Diffraction (3DXRD) experiment was carried out on 316H stainless steel, a material commonly used in thermal power plants, to obtain the per-grain strain response during plastic and creep deformation at 550°C. Several hundred grains within a probed X-ray volume were tracked and measured whilst loading in-situ, obtaining per-grain centre-of-mass positions, crystallographic orientations, and average lattice strain over individual grains. These data were used to calibrate a crystal plasticity model to study the plastic and creep deformation using macroscopic stress-strain and stress-relaxation data. Subsequently, the model was used to predict the average elastic strain in different grains during the cyclic creep experiment, which was validated by 3DXRD datasets. The model results reveal that {100} or {311} grain families are strongly sensitive to microstructure, thereby a polycrystal model that describes specific orientation and neighbourhood characteristics is essential to predict the local response of these grain families. Whereas, self-consistent models are suitable for {110} and {111} grain families. This study shows that only with a suitable calibration of subsurface grain behaviour, crystal plasticity models reveal grain characteristic-dependent micromechanical behaviour.
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Aug 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[29061]
Open Access
Abstract: The mechanisms that govern a previously unexplained hardening effect of a single phase Cu-30wt%Zn
-brass after heating have been investigated. After cold-work, the alloy possesses an increased yield strength and hardening rate only when heat treated to temperatures close to 220 °C, and is otherwise softer. Crystallographic texture and microstructure, explored using electron backscatter diffraction (EBSD), describe the deformation heterogeneity including twin development, as a function of heat treatment. When heated, an increased area fraction of deformation twins is observed, with dimensions reaching a critical size that maximises the resistance to dislocation slip in the parent grains. The effect is shown to dominate over other alloy characteristics including short range order, giving serrated yielding during tensile testing which is mostly eliminated after heating. In-situ X-ray diffraction during tensile testing corroborates these findings; dislocation-related line broadening and lattice strain development between as worked and heated
-brass is directly related to the interaction between the dislocations and the population of deformation twins. The experiments unambiguously disprove that other thermally-induced microstructure features contribute to thermal hardening. Specifically, the presence of recrystallised grains or second phases do not play a role. As these heat treatments match annealing conditions subjected to
-brass during deformation-related manufacturing processes, the results here are considered critical to understand, predict and exploit, where appropriate, any beneficial process-induced structural behaviour.
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Aug 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Kai
Zhang
,
Tim
Wigger
,
Rosa
Pineda
,
Simon A.
Hunt
,
Ben
Thomas
,
Thomas
Kwok
,
David
Dye
,
Gorka
Plata
,
Jokin
Lozares
,
Inaki
Hurtado
,
Stefan
Michalik
,
Michael
Preuss
,
Peter D.
Lee
,
Mohammed A.
Azeem
Diamond Proposal Number(s):
[23749]
Abstract: Microstructure evolution during high-strain rate and high-temperature thermo-mechanical processing of a 44MnSiV6 microalloyed steel is investigated using in situ synchrotron high-energy powder X-ray diffraction. The conditions selected replicate a newly developed near solidus high-strain rate process designed for reducing raw material use during the hot processing of steels. High temperatures (exceeding 1300 °C) and high strain rate
= 9 s-1 processing regimes are explored. The lattice strains and dislocation activity estimated from diffraction observations reveal that the microstructure evolution is primarily driven by dynamic recrystallisation. A steady-state stress regime is observed during deformation, which develops due to intermittent and competing work hardening and recovery processes. The texture evolution during the heating, tension, shear deformation and cooling stages is systematically investigated. The direct observation of phase evolution at high-temperature and high-strain rate deformation enables a comprehensive understanding of new manufacturing processes and provides deep insights for the development of constitutive models for face-centred cubic alloys.
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Aug 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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J. F. S.
Markanday
,
N.
D’souza
,
N. L.
Church
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J. R.
Miller
,
J. J. C.
Pitchforth
,
L. D.
Connor
,
S.
Michalik
,
B.
Roebuck
,
N. G.
Jones
,
K. A.
Christofidou
,
H. J.
Stone
Diamond Proposal Number(s):
[33375]
Abstract: Factors affecting strain-age cracking (SAC) have been quantitatively assessed in a range of Ni-base superalloys with differing γ′ contents. Differences in the amount of γ′ present in the as-built condition of HA282, STAL 15DE, CM247LC, and IN713LC are highlighted. In the as-built condition, γ′ are absent in HA282, but appear as nano-clusters in IN713LC. On heating, γ′ precipitates coherently in the γ phase, increasing the yield strength. The kinetics of precipitation are dependent on the heating rate and precipitation terminates at different temperatures in different alloys. The propensity to SAC is assessed via volume changes accompanying precipitation, increase in elastic modulus accompanying γ′ precipitation, and a loss in ductility/grain boundary cohesive strength with increasing temperature. A marked feature of additively built microstructures is the dramatically low grain boundary cohesive strength at ~800 °C, which is related to the segregation within the terminal liquid film at the grain boundary. The most important factor contributing to SAC is the lack of ductility and reduced grain boundary cohesive strength.
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Aug 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Barbara
Bonechi
,
Margherita
Polacci
,
Fabio
Arzilli
,
Giuseppe
La Spina
,
Jean-Louis
Hazemann
,
Richard A.
Brooker
,
Robert
Atwood
,
Sebastian
Marussi
,
Peter D.
Lee
,
Roy A.
Wogelius
,
Jonathan
Fellowes
,
Mike R.
Burton
Diamond Proposal Number(s):
[28538]
Open Access
Abstract: Transitions in eruptive style during volcanic eruptions strongly depend on how easily gas and magma decouple during ascent. Stronger gas-melt coupling favors highly explosive eruptions, whereas weaker coupling promotes lava fountaining and lava flows. The mechanisms producing these transitions are still poorly understood because of a lack of direct observations of bubble dynamics under natural magmatic conditions. Here, we combine x-ray radiography with a novel high-pressure/high-temperature apparatus to observe and quantify in real-time bubble growth and coalescence in basaltic magmas from 100 megapascals to surface. For low-viscosity magmas, bubbles coalesce and recover a spherical shape within 3 seconds, implying that, for lava fountaining activity, gas and melt remain coupled during the ascent up to the last hundred meters of the conduit. For higher-viscosity magmas, recovery times become longer, promoting connected bubble pathways. This apparatus opens frontiers in unraveling magmatic/volcanic processes, leading to improved hazard assessment and risk mitigation.
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Aug 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[27571]
Open Access
Abstract: Using synchrotron X-ray diffraction, tomography and machine-learning enabled phase segmentation strategy, we have studied under operando conditions the nucleation, co-growth and dynamic interplays among the dendritic and multiple intermetallic phases of a typical recycled Al alloy (Al5Cu1.5Fe1Si, wt.%) in solidification with and without ultrasound. The research has revealed and elucidated the underlying mechanisms that drive the formation of the very complex and convoluted Fe-rich phases with rhombic dodecahedron and 3D skeleton networks (the so-called Chinese-script type morphology). Through statistical microstructural analyses and numerical modelling of the ultrasound melt processing, the research has demonstrated that a short period of ultrasound processing of just 7s in the liquid state is able to reduce the average size of the α-Al dendrites and the Fe-containing intermetallic phases by ∼5 times compared to the cases without ultrasound. This work has provided more new insights on quantitatively understanding of the formation of convoluted morphology of intermetallic phases in 4D domain and the beneficial effects of applying ultrasound to recycled Al alloys, which are directly relevant to industrial practice.
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Aug 2024
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