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Three-dimensional X-ray diffraction (3DXRD) has been used to measure, in-situ, the evolution of $\sim 1800$ grains in a single phase low carbon ferritic steel sample during uniaxial deformation. The distribution of initial residual grain stresses in the material was observed to prevail as plasticity builds, though became less pronounced, and therefore less influential as strain increased. The initial Schmid factor of a grain was found to be strongly correlated to the intergranular stress change and the range of stresses that are permissible; a grain well aligned for easy slip is more likely to exhibit a range of stresses than those orientated poorly for dislocation motion. The orientation path of a grain, however, is not only dependent on its initial orientation, but hypothesised to be influenced by its stress state and the stress state of its grain environment. A grain neighbourhood effect is observed: the Schmid factor of serial adjoining grains influences the stress state of a grain of interest, whereas parallel neighbours are much less influential. This phenomenon is strongest at low plastic strains only, with the effect diminishing as plasticity builds. The influence of initial residual stresses becomes less evident, and grains rotate to eliminate any orientation dependent load shedding. The ability of the BCC ferrite to exhaust such neighbourhood interactions, which would otherwise be detrimental in crystal structures with lower symmetric and fewer slip systems, is considered key to the high ductility possessed by these materials., Comment: 17 pages (+2 supplementary pages), 13 figures (+3 supplementary figures). Preprint submitted to Acta Materialia

Diamond Light Source (DLS), the United Kingdom’s national synchrotron facility, is located on the campus of Rutherford Appleton Lab (RAL) in southern Oxfordshire. DLS is jointly funded by the Scien...

An experimental setup is described that uses a hyperspectral imaging detector to collect time-resolved X-ray diffraction information from a complete discharging AA size battery, using a commercial alkaline Zn–Mn cell as a proof of concept. The work is complemented by time-resolved in situ X-ray computed tomography of an identical battery cell., An experimental technique is described for the collection of time-resolved X-ray diffraction information from a complete commercial battery cell during discharging or charging cycles. The technique uses an 80 × 80 pixel 2D energy-discriminating detector in a pinhole camera geometry which can be used with a polychromatic X-ray source. The concept was proved in a synchrotron X-ray study of commercial alkaline Zn–MnO2 AA size cells. Importantly, no modification of the cell was required. The technique enabled spatial and temporal changes to be observed with a time resolution of 20 min (5 min of data collection with a 15 min wait between scans). Chemical changes in the cell determined from diffraction information were correlated with complementary X-ray tomography scans performed on similar cells from the same batch. The clearest results were for the spatial and temporal changes in the Zn anode. Spatially, there was a sequential transformation of Zn to ZnO in the direction from the separator towards the current collector. Temporally, it was possible to track the transformation of Zn to ZnO during the discharge and follow the corresponding changes in the cathode.

Description, 4D x-ray imaging of transport in porous media shows that hydrodynamic dispersion is larger during cleanup versus contamination., Experimental and field studies reported a significant discrepancy between the cleanup and contamination time scales, while its cause is not yet addressed. Using high-resolution fast synchrotron x-ray computed tomography, we characterized the solute transport in a fully saturated sand packing for both contamination and cleanup processes at similar hydrodynamic conditions. The discrepancy in the time scales has been demonstrated by the nonuniqueness of hydrodynamic dispersion coefficient versus injection rate (Péclet number). Observations show that in the mixed advection-diffusion regime, the hydrodynamic dispersion coefficient of cleanup is significantly larger than that of the contamination process. This nonuniqueness has been attributed to the concentration-dependent diffusion coefficient during the cocurrent and countercurrent advection and diffusion, present in contamination and cleanup processes. The new findings enhance our fundamental understanding of transport processes and improve our capability to estimate the transport time scales of chemicals or pollution in geological and engineering systems.

Three-dimensional X-ray diffraction (3DXRD) is shown to be feasible at the I12 Joint Engineering, Environmental and Processing (JEEP) beamline of Diamond Light Source. As a demonstration, a microstructually simple low-carbon ferritic steel was studied in a highly textured and annealed state. A processing pipeline suited to this beamline was created, using software already established in the 3DXRD user community, enabling grain centre-of-mass positions, orientations and strain tensor elements to be determined. Orientations, with texture measurements independently validated from electron backscatter diffraction (EBSD) data, possessed a $\sim 0.1^\circ$ uncertainty, comparable with other 3DXRD instruments. The spatial resolution was limited by the far-field detector pixel size; the average of the grain centre of mass position errors was determined as $\pm \sim 80 \mu$m. An average per-grain error of $\sim 1 \times 10^{-3}$ for the elastic strains was also measured; this could be reduced in future experiments by improving sample preparation, data collection and analysis techniques. Application of 3DXRD onto I12 shows great potential, where its implementation is highly desirable due the flexible, open architecture of the beamline. User-owned or designed sample environments can be used, thus 3DXRD could be applied to previously unexplored scientific areas., Comment: 13 pages, 10 figures. Published in Journal of Synchrotron Radiation

Alternative and sustainable waste sources are receiving increasing attention as they can be used to produce biofuels with a low carbon footprint. Waste fish oil is one such example and can be considered an abundant and sustainable waste source to produce biodiesel. Ultimately this could lead to fishing communities having their own ‘off-grid’ source of fuel for boats and vehicles. At the industrial level, biodiesel is currently produced by homogeneous catalysis because of the high catalyst activity and selectivity. In contrast, heterogeneous catalysis offers several advantages such as improved reusability, reduced waste and lower processing costs. Here we investigate the phase evolution of two heterogeneous catalysts, CaO and a Ca3Al2O6:CaO (‘C3A:CaO’) composite, under in-situ conditions for biodiesel production from fish oil. A new reactor was designed to monitor the evolution of the crystalline catalyst during the reaction using synchrotron powder x-ray diffraction. The amount of calcium diglyceroxide (CaDG) began to increase rapidly after approximately 30 min, for both catalysts. This rapid increase in CaDG could be linked to ex-situ nuclear magnetic resonance studies which showed that the conversion of fish oil to biodiesel rapidly increased after 30 min. The key to the difference in activity of the two catalysts appears to be that the Ca3Al2O6:CaO composite maintains a high rate of CaDG formation for longer than CaO, although the initial formation rates and reaction kinetics are similar. The Ca for the CaDG mainly comes from the CaO phase. In addition, towards the end of the second test utilising the CaO catalyst (after 120 min), there is a rapid decrease in CaDG and a rapid increase in Ca(OH)2. This was not observed for the Ca3Al2O6:CaO catalyst and this is due to Ca3Al2O6 stabilising the CaO in the composite material. No additional calcium containing intermediate crystalline phases were observed during our in-situ experiment. Overall this specialised in-situ set-up has been shown to be suitable to monitor the phase evolution of heterogeneous crystalline catalysts during the triglycerides transesterification reaction, offering the opportunity to correlate the crystalline phases to activity, deactivation and stability.

Parallel-beam tomography systems at synchrotron facilities have limited field of view (FOV) determined by the available beam size and detector system coverage. Scanning the full size of samples bigger than the FOV requires various data acquisition schemes such as grid scan, 360-degree scan with offset center-of-rotation (COR), helical scan, or combinations of these schemes. Though straightforward to implement, these scanning techniques have not often been used due to the lack of software and methods to process such types of data in an easy and automated fashion. The ease of use and automation is critical at synchrotron facilities where using visual inspection in data processing steps such as image stitching, COR determination, or helical data conversion is impractical due to the large size of datasets. Here, we provide methods and their implementations in a Python package, named Algotom, for not only processing such data types but also with the highest quality possible. The efficiency and ease of use of these tools can help to extend applications of parallel-beam tomography systems.

The fatigue crack retardation mechanisms operating after an overload event are investigated for a bainitic steel using high spatial resolution energy dispersive synchrotron X-ray diffraction. The elastic crack-tip strain fields are mapped at mid-thickness of compact tension samples at R-ratios of 0.1 and 0.4. The same overload stress intensity factor (KOL = 60 MPa m1/2) is applied in each case with the cracks then propagating under the same applied stress intensity range, ΔKapp = 27 MPa m1/2. The competing retardation mechanisms are directly quantified and separated, with the associated fatigue crack growth (FCG) rates then being predicted according to a 2-parameter Walker-type assessment and validated against those measured. The stress intensity factor associated with the overload residual stress field is calculated using a weight function approach. For R=0.1, shielding from residual stress controls retardation when crack growth through the overload plastic zone, rp OL, is small (specifically p OL). For more extensive crack growth, discontinuous crack closure controls the retardation behaviour, with significant load transfer across opposing crack faces being observed at minimum load (for R=0.1). These crack face tractions are associated with the plastic asperity created during overload. The traction forces holding the crack faces open at minimum load are, for the first time, used to directly quantify the associated stress intensity factor, Kmin tract as a function of crack growth. While no crack shielding is expected, nor observed, for R=0.4, the variation in FCG rate after overload is explained by changes in effective R-ratio.

In structural materials, ‘intrinsic’ toughening originates from plastic dissipation of strain energy at the tips of cracks. This depends on a material's microstructure and its stress–strain response. By introducing a spatially-varying distribution of prior strain-hardening into a material, we can modify the stress field which develops around a crack as it is loaded, producing an increased resistance to ductile tearing. We demonstrate this toughening effect using synchrotron X-ray diffraction and digital image correlation measurements of the crack tip region in a ductile ferritic steel. Localised strain-hardening also introduces a residual stress, but this is shown not to contribute significantly to the initiation of tearing in this material.

Premature failure of wind turbine gearbox bearings is an ongoing concern for industry, with sudden overload events potentially contributing towards raceway damage, significantly hindering performance. Subsurface stresses generated along a line contact cause material yielding, and a probable crack initiation site. Currently, the ability to study subsurface plastic zone evolution using non-destructive techniques is limited. Neutron Bragg edge imaging is a novel technique, allowing for two-dimensional mapping of the Bragg edge broadening parameter, indicative of bulk plastic deformation. An experiment on the ENGIN-X strain scanning instrument, at the ISIS neutron source, UK, was setup for Bragg edge transmission imaging, to measure the effect of in situ loading on the raceway of a bearing, scaled-down from a traditional wind turbine gearbox bearing. Results demonstrate a strong correlation between load and the Bragg edge width, and allow for future experimental development in studying, not only the effect of overloads on fatigue life, but also the use of neutron imaging for evaluating plastic deformation in engineering components. Keywords: Time-of-flight, Energy-dispersive imaging, Bragg edge imaging, Neutron radiography, Bearing overload, Subsurface plasticity

The governing mechanistic behaviour of Directed Energy Deposition Additive Manufacturing (DED-AM) is revealed by a combined in situ and operando synchrotron X-ray imaging and diffraction study of a nickel-base superalloy, IN718. Using a unique DAE-AM process replicator, real-space imaging enables quantification of the melt-pool boundary and flow dynamics during solidification. This imaging knowledge was also used to informed precise diffraction measurements of temporally resolved microstructural phases during transformation and stress development with a spatial resolution of 100 µm. The diffraction quantified thermal gradient enabled a dendritic solidification microstructure to be predicted and coupled to the stress orientation and magnitude. The fast cooling rate entirely suppressed the formation of secondary phases or recrystallisation in the solid-state. Upon solidification, the stresses rapidly increase to the yield strength during cooling. This insight, combined with the large solidification range of IN718 suggests that the accumulated plasticity exhausts the ductility of the alloy, causing liquation cracking. This study has revealed additional fundamental mechanisms governing the formation of highly non-equilibrium microstructures during DED-AM.

The Directed Energy Deposition Additive Manufacturing (DED-AM) of SS316L was studied using in situ and operando synchrotron X-ray imaging to quantitively understand the effect of processing parameters on the melt-pool morphology and surface quality. It was found that surface roughness of DED-AM builds can result from melt pool surface perturbations caused by changes in the melt flow and build stage motion perturbations. Process maps are developed that quantitatively correlate build quality to process parameters including powder feed rate, laser power and traverse speed. How the AM process parameters control build efficacy is clarified, and the processing conditions required to dampen surface perturbations leading to roughness were determined.

The effect of Strain Path Changes (SPCs) on the mechanical properties and crystal-level features of deformation for a single phase, ferritic steel has been investigated. SPCs were applied via a two-step deformation process, which included pre-straining via cold rolling, followed by uniaxial tension. The pre-strain magnitude and direction, as well as the tensile direction, varied between the specimens. The role of texture and micromechanics were examined in-situ, via Synchrotron X-Ray Diffraction (SXRD), and ex-situ, via Electron Backscatter Diffraction (EBSD). Abrupt strain paths (i.e. strain paths where the pre-strain and the subsequent loading directions differ; here they are orthogonal) result in a significant ductility reduction, becoming more prevalent for high pre-strain magnitudes. The macroscopic response, as well as the texture configuration were greatly dependent on the pre-strain direction but were insensitive to the direction of uniaxial tension. Increasing pre-strain magnitudes resulted in a stagnation of lattice strain hardening rates in all macroscopic directions and in a significant increase in the Geometrically Necessary Dislocation (GND) densities. This was vastly increased for specimens rolled perpendicular to the as-received prior rolling direction. No correlation was found between the GND density and the grain orientation, eliminating this as a controlling ductility factor for BCC ferrite. Instead, the initial texture, the texture developed in a subsequent pre-strain influences the density of dislocations accumulated in all grains, and ultimately determines ductility.

The authors also thank the Laboratoire Léon Brillouin (France) for beamtime allocation and Sebastien GAUTROT (LLB, France) for his help during the experiments. Vincent Jacquemain, Dr. Jean-Baptiste Marijon, and Dr. Stefan Michalik are acknowledged for their help during the synchrotron campaign at Diamond. A two-phase near- beta titanium alloy (Ti–10V–2Fe–3Al, or Ti-1023) in its as-forged state is employed to illustrate the feasibility of a Bayesian framework to identify single-crystal elastic constants (SEC). High Energy X-ray diffraction (HE-XRD) obtained at the Diamond synchrotron source are used to character- ize the evolution of lattice strains for various grain orientations during in situ specimen loading in the elastic regime. On the other hand, specimen behavior and grain deformation are estimated using the elastic self-consistent (ELSC) homogenization scheme. The XRD data and micromechanical modelling are revisited with a Bayesian framework. The effect of different material parameters (crystallographic and morphological textures, phase volume fraction) of the micromechanical model and the biases intro- duced by the XRD data on the identification of the SEC of the βphase are systematically investigated. In this respect, all the three cubic elastic constants of the βphase ( C11(beta) , C12(beta) , C44(beta) ) in the Ti-1023 alloy have been derived with their uncertainties. The grain aspect ratio in the ELSC model, which is often not considered in the literature, is found to be an important parameter in affecting the identified SEC. The Bayesian inference suggests a high probability for non-spherical grains (aspect ratio of ∼3 . 8+/-0 . 8 ) : C11(beta) = 92 . 6+/-19 . 1 GPa , C12(beta) = 82 . 5+/-16 . 3 GPa , C44(beta) = 43 . 5+/-7 . 1 GPa . The uncertainty obtained by Bayesian approach lies in the range of ~1-3 GPa for the shear modulus mu’ = (C11(beta) −C12(beta) )/2 , and ~7 GPa for the shear modulus mu’’ = C44(beta) , while it is significantly larger in the case of the bulk modulus (C11(beta) +2C12(beta))/3 (~17-24 GPa). This research is supported by the “Région Grand Est” and by the French State through two programs operated by the National Research Agency (ANR), (1) “Investment in the future” referenced by ANR-11-LABX-0 0 08-01 (Laboratory of Excellence “DAMAS”: De- sign of Alloy Metals for low-mAss Structures) and (2) “Plan d’Investissement d’Avenir” (PIA) in the frame of a research pro- gram managed by "Institut de Recherche Technologique Matériaux, Métallurgie, Procédés" (IRT M2P). We acknowledge DIAMOND for provision of synchrotron radiation beamtime at beamline I12-JEEP.

Funder: DST-NRF Centre of Excellence in Palaeosciences, Funder: Palaeontological Scientific Trust, Numerous aspects of early hominin biology remain debated or simply unknown. However, recent developments in high-resolution imaging techniques have opened new avenues in the field of paleoanthropology. More specifically, X-ray synchrotron-based analytical imaging techniques have the potential to provide crucial details on the ontogeny, physiology, biomechanics, and biological identity of fossil specimens. Here we present preliminary results of our X-ray synchrotron-based investigation of the skull of the 3.67-million-year-old Australopithecus specimen StW 573 (‘Little Foot’) at the I12 beamline of the Diamond Light Source (United Kingdom). Besides showing fine details of the enamel (i.e., hypoplasias) and cementum (i.e., incremental lines), as well as of the cranial bone microarchitecture (e.g., diploic channels), our synchrotron-based investigation reveals for the first time the 3D spatial organization of the Haversian systems in the mandibular symphysis of an early hominin.

Thermal runaway of lithium-ion batteries can involve various types of failure mechanisms each with their own unique characteristics. Using fractional thermal runaway calorimetry and high-speed radiography, the response of three different geometries of cylindrical cell (18650, 21700, and D-cell) to different abuse mechanisms (thermal, internal short circuiting, and nail penetration) are quantified and statistically examined. Correlations between the geometry of cells and their thermal behavior are identified, such as increasing heat output per amp-hour (kJ Ah−1) of cells with increasing cell diameter during nail penetration. High-speed radiography reveals that the rate of thermal runaway propagation within cells is generally highest for nail penetration where there is a relative increase in rate of propagation with increasing diameter, compared to thermal or internal short-circuiting abuse. For a given cell model tested under the same conditions, a distribution of heat output is observed with a trend of increasing heat output with increased mass ejection. Finally, internal temperature measurements using thermocouples embedded in the penetrating nail are shown to be unreliable thus demonstrating the need for care when using thermocouples where the temperature is rapidly changing. All data used in this manuscript are open access through the NREL and NASA Battery Failure Databank.

The formation of primary Fe-rich intermetallic compound crystals and the effect of TiB2 and TiC inoculation during solidification of a hypereutectic Al-Fe alloy has been investigated. Both horizontal, near isothermal conditions and vertical, directional thermal gradient conditions were studied using laboratory and synchrotron X-ray radiography. TiB2 and TiC inoculation enhanced formation of Fe-rich intermetallics under all experimental conditions. Near isothermal solidification resulted in the highest intermetallic number density and average formation rate, whilst increasing the thermal gradient reduced both. A model for intermetallic crystal formation is proposed to explain the effect of thermal gradient and cooling rate on the intermetallic number density and average formation rate.

The governing mechanistic behaviour of Directed Energy Deposition Additive Manufacturing (DED-AM) is revealed by a combined in situ and operando synchrotron X-ray imaging and diffraction study of a nickel-base superalloy, IN718. Using a unique process replicator, real-space phase-contrast imaging enables quantification of the melt-pool boundary and flow dynamics during solidification. This imaging knowledge informed precise diffraction measurements of temporally resolved microstructural phases with unprecedented precision during transformation and stress development with a spatial resolution of 100 µm. The diffraction quantified thermal gradient enabled a dendritic solidification microstructure to be predicted and coupled to the stress orientation and magnitude. The fast cooling rate entirely suppressed the formation of secondary phases or recrystallisation in the solid-state. Upon solidification, the stresses rapidly increase to the yield strength during cooling. This insight, combined with IN718’s large solidification range suggests that the accumulated plasticity exhausts the alloy’s ductility, causing liquation cracking. This study has revealed additional fundamental mechanisms governing the formation of highly non-equilibrium microstructures during DED-AM.

Many of the grand challenges in volcanic and magmatic research are focused on understanding the dynamics of highly heterogeneous systems and the critical conditions that enable magmas to move or eruptions to initiate. From the formation and development of magma reservoirs, through propagation and arrest of magma, to the conditions in the conduit, gas escape, eruption dynamics, and beyond into the environmental impacts of that eruption, we are trying to define how processes occur, their rates and timings, and their causes and consequences. However, we are usually unable to observe the processes directly. Here we give a short synopsis of the new capabilities and highlight the potential insights that in situ observation can provide. We present the XRheo and Pele furnace experimental apparatus and analytical toolkit for the in situ X-ray tomography-based quantification of magmatic microstructural evolution during rheological testing. We present the first 3D data showing the evolving textural heterogeneity within a shearing magma, highlighting the dynamic changes to microstructure that occur from the initiation of shear, and the variability of the microstructural response to that shear as deformation progresses. The particular shear experiments highlighted here focus on the effect of shear on bubble coalescence with a view to shedding light on both magma transport and fragmentation processes. The XRheo system is intended to help us understand the microstructural controls on the complex and non-Newtonian evolution of magma rheology, and is therefore used to elucidate the many mobilization, transport, and eruption phenomena controlled by the rheological evolution of a multi-phase magmatic flows. The detailed, in situ characterization of sample textures presented here therefore represents the opening of a new field for the accurate parameterization of dynamic microstructural control on rheological behavior.

As a part of a research into new techniques for purifying recycled aluminium alloys, a novel electromagnetic apparatus had been developed for investigating in real-time the separation mechanisms of detrimental inclusions in aluminium alloy melts under alternating magnetic fields. The magnetic coil was designed based on the Helmholtz coil design. A viewing gap was designed for

© 2017 Elsevier Ltd Synchrotron X-ray microtomography and skeletonisation method were used to study the true 3D network structures and morphologies of the Fe-rich intermetallic phases in recycled Al-5.0%Cu-0.6%Mn alloys with 0.5% and 1.0% Fe. It was found that, the Fe-phases in the 1.0%Fe alloy have node lengths of 5–25 μm; while those in the 0.5%Fe alloy are of 3–17 μm. The Fe-phases in the 1.0%Fe alloy also developed sharper mean curvature with wider distribution than those in the 0.5%Fe alloy. Combining SEM studies of the deeply-etched samples, the true 3D structures of 4 different type Fe phases in both alloys are also revealed and demonstrated.

Ultrasound processing of metal alloys is an environmental friendly and promising green technology for liquid metal degassing and microstructural refinement. However many fundamental issues in this field are still not fully understood, because of the difficulties in direct observation of the dynamic behaviours caused by ultrasound inside liquid metal and semisolid metals during the solidification processes. In this paper, we report a systematic study using the ultrafast synchrotron X-ray imaging (up to 271,554 frame per second) technique available at the Advanced Photon Source, USA and Diamond Light Source, UK to investigate the dynamic interactions between the ultrasonic bubbles/acoustic flow and the solidifying phases in a Bi-8%Zn alloy. The experimental results were complimented by numerical modelling. The chaotic bubble implosion and dynamic bubble oscillations were revealed in-situ for the first time in liquid metal and semisolid metal. The fragmentation of the solidifying Zn phases and breaking up of the liquid-solid interface by ultrasonic bubbles and enhanced acoustic flow were clearly demonstrated and agreed very well with the theoretical calculations. The research provides unambiguous experimental evidence and robust theoretical interpretation in elucidating the dominant mechanisms of microstructure fragmentation and refinement in solidification under ultrasound.

Directed Energy Deposition Additive Manufacturing (DED-AM) is transformative for the production of larger, geometrically complex metallic components. However, the mechanical properties of titanium alloy DED-AM components do not always reach their full potential due to microstructural features including porosity and regions of lack of fusion. Using in situ and operando synchrotron X-ray imaging we gain insights into key laser-matter interaction and microstructural feature formation mechanisms during DED-AM of Ti-6242. Analysis of the process conditions reveals that laser power is dominant for build efficiency while higher traverse speed can effectively reduce lack of fusion regions. We also elucidate the mechanisms underlying several physical phenomena occurring during the deposition of titanium alloys, including the formation of a saddle-shaped melt pool and pore pushing. The findings of this work clarify the transient kinetics behind the DED-AM of titanium alloys and can be used as a guide for optimising industrial additive manufacturing processes.

This study focuses on the microscale fatigue properties of 316L stainless steel. This material is commonly used in the manufacture of medical devices such as stents, which, once implanted, are subjected to hundreds of millions of fatigue cycles. Fatigue testing was carried out on 50 μm, 75 μm, 100 μm and 150 μm 316L specimens with 60 μm thickness. A size effect was shown to exist in the form of a reduced fatigue endurance limit of the 50 μm specimens. In order to determine the cause of this size effect, the outer surfaces and fracture surfaces of failed test specimens were examined using Scanning Electron Microscopy (SEM) techniques. These SEM studies suggest that the process of strain localization was occurring in the specimens and was most pronounced in the 50 μm specimens. The experimentally established surface roughness of the test specimens, measured using white-light interferometry, further confirmed the SEM observation.

Non-destructive imaging techniques provide a unique opportunity to study crack initiation and propagation behaviour in structural materials. To evaluate the applicability of different volumetric imaging techniques, a round bar notched sample of duplex stainless steel was fatigue cracked and studied in situ and ex situ. Neutron and synchrotron X-ray tomography was used along with destructive methods and Bragg edge neutron imaging to evaluate the fatigue crack. Neutron attenuation tomography obtained a three-dimensional image in which the crack was readily identifiable. The neutron tomography, although lower in spatial resolution compared with the X-ray synchrotron tomography and requiring higher acquisition time, is sensitive to the phase chemistry, and has the potential to study engineering size components. Bragg edge neutron transmission imaging allows for the mapping of two-dimensional elastic strains and was used to identify the fatigue crack from the reduction in the strain in the region where the crack propagated. A finite element model of the cracked specimen was used to simulate the average through thickness strain that is measured by the Bragg edge neutron imaging technique. The strains measured in the ferritic phase correspond better with the simulation strains than the strain measured in the austenitic phase. It is concluded that this difference is due to strain partitioning, which is influenced by the strong texture present in the duplex steel.

In this paper, we present some highlighted findings from our recent research on real-time and in situ studies of the fundamentals of ultrasonic melt processing, including (1) ultrasonic bubble implosion, oscillation in liquid and semi-liquid (semi-solid) metals and their interactions with the growing solidifying phases; (2) enhanced acoustic metal flow and their impact on the liquid-solid metal interface. The real time experimental phenomena were interpreted with the aid of calculating the propagation of acoustic pressure in liquid metals using the Helmholtz equation and bubble wall pressure and velocity profile during bubble oscillation using the classical Gilmore model. The research provides unambiguous real-time evidence and robust theoretical interpretation in elucidating the dominant mechanisms of microstructure fragmentation and refinement in solidification under ultrasound.

Fatigue crack growth in the Heat Affected Zone (HAZ) of a welded CrNiMoV steel has been investigated, in situ, using Digital Image Correlation (DIC) and Energy Dispersive X-ray Diffraction (EDXD). Compact tension specimens of welded joint were loaded under tension–tension cyclic loading. The crack tip position and the evolution of the near-tip strains normal to the crack plane were tracked at selected positions for a growing fatigue crack both on the specimen surface using DIC and in the bulk of the specimen using EDXD of synchrotron X-rays. The uncertainty and quality of the DIC measurements were examined with regard to some of the key data processing parameters, including subset size and the size of measurement window; whilst the measurement errors in the EDXD measurements were also estimated. A “characteristic” strain was estimated, in the bulk of the specimen and on the specimen surface, from the average strains captured at selected positions when the propagating fatigue crack tip reached these positions.

Internal flow behaviour during melt-pool-based metal manufacturing remains unclear and hinders progression to process optimisation. In this contribution, we present direct time-resolved imaging of melt pool flow dynamics from a high-energy synchrotron radiation experiment. We track internal flow streams during arc welding of steel and measure instantaneous flow velocities ranging from 0.1 m s−1 to 0.5 m s−1. When the temperature-dependent surface tension coefficient is negative, bulk turbulence is the main flow mechanism and the critical velocity for surface turbulence is below the limits identified in previous theoretical studies. When the alloy exhibits a positive temperature-dependent surface tension coefficient, surface turbulence occurs and derisory oxides can be entrapped within the subsequent solid as result of higher flow velocities. The widely used arc welding and the emerging arc additive manufacturing routes can be optimised by controlling internal melt flow through adjusting surface active elements., Understanding what happens to the liquid in melt pools during welding and metal-based additive manufacturing remains a challenge. Here, the authors directly image internal melt pool dynamics using synchrotron radiation to show surface tension affects flow speed, orientation and surface turbulence.