Search

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.

The performance of Li+ ion batteries (LIBs) is hindered by steep Li+ ion concentration gradients in the electrodes. Although thick electrodes (>= 300 mu m) have the potential for reducing the proportion of inactive components inside LIBs and increasing battery energy density, the Li+ ion concentration gradient problem is exacerbated. Most understanding of Li+ ion diffusion in the electrodes is based on computational modeling because of the low atomic number (Z) of Li. There are few experimental methods to visualize Li+ ion concentration distribution of the electrode within a battery of typical configurations, for example, coin cells with stainless steel casing. Here, for the first time, an interrupted in situ correlative imaging technique is developed, combining novel, full-field X-ray Compton scattering imaging with X-ray computed tomography that allows 3D pixel-by-pixel mapping of both Li+ stoichiometry and electrode microstructure of a LiNi0.8Mn0.1Co0.1O2 cathode to correlate the chemical and physical properties of the electrode inside a working coin cell battery. An electrode microstructure containing vertically oriented pore arrays and a density gradient is fabricated. It is shown how the designed electrode microstructure improves Li+ ion diffusivity, homogenizes Li+ ion concentration through the ultra-thick electrode (1 mm), and improves utilization of electrode active materials.

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.

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.

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.

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 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

© 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.

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.

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.

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.

The highly dynamic behavior of ultrasonic bubble implosion in liquid metal, the multiphase liquid metal flow containing bubbles and particles, and the interaction between ultrasonic waves and semisolid phases during solidification of metal were studied in situ using the complementary ultrafast and high-speed synchrotron X-ray imaging facilities housed, respectively, at the Advanced Photon Source, Argonne National Laboratory, US, and Diamond Light Source, UK. Real-time ultrafast X-ray imaging of 135,780 frames per second revealed that ultrasonic bubble implosion in a liquid Bi-8 wt pctZn alloy can occur in a single wave period (30 kHz), and the effective region affected by the shockwave at implosion was 3.5 times the original bubble diameter. Furthermore, ultrasound bubbles in liquid metal move faster than the primary particles, and the velocity of bubbles is 70 ~ 100 pct higher than that of the primary particles present in the same locations close to the sonotrode. Ultrasound waves can very effectively create a strong swirling flow in a semisolid melt in less than one second. The energetic flow can detach solid particles from the liquid–solid interface and redistribute them back into the bulk liquid very effectively.

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.

An X-ray imaging system has been designed to overcome the challenges from the high flux of white-beam radiation, including degradation of image quality caused by accumulated contamination on the scintillator during intense X-ray exposure., The high flux of the white X-ray beams from third-generation synchrotron light sources can significantly benefit the development of high-speed X-ray imaging, but can also bring technical challenges to existing X-ray imaging systems. One prevalent problem is that the image quality deteriorates because of dust particles accumulating on the scintillator screen during exposure to intense X-ray radiation. Here, this problem has been solved by embedding the scintillator in a flowing inert-gas environment. It is also shown that the detector maintains the quality of the captured images even after days of X-ray exposure. This modification is cost-efficient and easy to implement. Representative examples of applications using the X-ray imaging system are also provided, including fast tomography and multimodal phase-contrast imaging for biomedical and geological samples.

The pre-existing porosity behaviour of globular semi-solid Al–Cu alloys during uniaxial compression is quantified during time-resolved synchrotron tomography at ∼64% and ∼93% solid. At ∼64% solid, both tortuous and round pores exist before deformation, respectively persisting and closing during compression, while at ∼93% solid, pre-existing tortuous pores open under compressive axial strain. It is demonstrated that pore behaviour reflects the immediate grain neighbourhood where the semi-solid alloy acts as a granular material, and that pore opening results from shear-induced dilation during uniaxial compression.

The deformation behaviors of a Zr41.2Ti13.8Cu12.5Ni10Be22.5 bulk metallic glassy alloy under step-controlled tensile loads have been studied in situ and systematically using scanning electron microscopy and synchrotron X-ray diffraction. A circular hole, as a stress concentrator, was introduced in the middle of the gauge length of the sample to facilitate the creation of shear bands in a controllable way at the edge of the hole in situ imaging and diffraction studies could be carried out at the identical loads in a quasi-steady state manner. Pair distribution function was used to calculate the strains of different atomic coordination shells and the relative change of the bond lengths of different atomic pairs. The combined imaging and diffraction studies revealed that (1) the extension of solvent–solvent (Zr–Zr) atomic pairs under tension causes the nucleation of shear bands, and (2) the compressive stress field around the shear band tip effectively slows down the fast propagation of shear bands.

Semi-solid deformation mechanisms are important in a range of manufacturing and natural phenomena, which range from squeeze casting to magma flows. Using fast synchrotron X-ray tomography and a bespoke precision thermomechanical rig, we performed a four-dimensional (3-D plus time) quantitative investigation of the granular behaviour of equiaxed dendritic three-phase materials. This methodology produced new insights into the formation of damage during the isothermal semi-solid compression (� 30% liquid fraction) of an Al–15 wt.%Cu alloy at both a macroscopic and microscopic level. Grain rearrangements, such as translation and rotation, were observed and lead to local dilatancy. The resulting flow of Cu-rich intergranular liquid into the dilated interstices gave rise to a local increase in liquid fraction, followed by rapid void growth above a critical axial strain of � 6.4%. The local normal and shear strain distributions were quantified using digital volume correlation, identifying dilatant shear bands. At a microstructural level, the individual grains were also seen to undergo intragranular deformation, leading to bending and fragmentation of dendrites as grains interlock. 2014 Acta Materialia Inc. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/ licenses/by/3.0/).

To better understand the influence of Fe-rich intermetallics on solidification defect formation, fast in situ synchrotron X-ray tomographic microscopy experiments were performed on a commercial A319 alloy (Al–7.5Si–3.5Cu, wt.%) with 0.2 and 0.6 wt.% Fe. Real-time observations during solidification and semi-solid deformation experiments reveal that β-intermetallics contribute via several different mechanisms to porosity formation and hot tearing susceptibility. While β-intermetallics were not observed to nucleate porosity directly, they do block interdendritic channels, thereby reducing the shrinkage feeding, and increasing pore tortuosity. Pores also grow preferentially along the surface of the β-intermetallics, suggesting that the β-phase has a lower gas–solid interfacial energy than α-Al, thus assisting in increasing pore volume. During uniaxial tension experiments, the ductile failure of the semi-solid, intermetallic-poor, base alloy transitions to a brittle-like failure when a large amount of β-intermetallics are present. In all post-failure microstructures, internal damage was preferentially orientated perpendicular to the loading direction, agreeing with prior experimental and numerical studies., Acta Materialia, 68, ISSN:1359-6454

Novel methods of correlating damage evolution measurement techniques are explored to produce improved constitutive equations that better account for the effect of initial inclusion distributions on damage softening behaviour. Based on ex situ, high resolution, synchrotron tomographic quantification of the three-dimensional interactions of damage formed during hot deformation of free cutting steel, a new parameter to account for the effect of inclusions on damage is proposed. Uniaxial tensile samples deformed at 1100 °C and a strain rate of 0.1 s−1 were interrupted at various strains prior to failure. Ex situ synchrotron X-ray computed tomography (sCT) was then used to quantify the growth of damage in the hot deformation of a leaded free cutting steel. Void growth is related to nucleated microvoids at inclusions. The number and volume fraction of voids were calculated for each tensile sample, allowing quantification of the evolving ductile damage via the measured increase in average void diameter after each strain increment. The equivalent diameter, spacing and volume fraction of inclusions were measured at the different interrupt strains. The local strain and stress state, evaluated using the finite element method at the microscale, were related to the local void populations. There was evidence that after necking the damage localized due to clustered inclusions. Damage localization was confirmed with a three-dimensional micromechanics model of 100 inclusions, whose distribution was taken directly from the sCT results, and a novel approach to extract the damage fraction is presented. A new parameter was introduced to account for inclusion size, spacing and clustering, which was validated against the sCT results.

In the present study, the residual stresses distribution in the Linear Friction Welded (LFW) pieces were studied using Finite Element (FE) simulation and high energy synchrotron X-ray diffraction. Fully-coupled implicit thermo-mechanical analysis simulation procedure was employed, with semi-automatic re-meshing using Python scripting to accommodate large deformation and output contour tracking methods for extracting deformed configurations. Model validated by the multi-detector polychromatic synchrotron X-ray experimental data were used to study the distribution of residual stresses distribution in the Linear Friction Welded (LFW) pieces to provide a general function to describe the residual stresses distribution. A characteristic length scale was found in the plot. © 2013 Elsevier Ltd.

This paper presents a novel experiment to quantify both the initial residual stress state in a specimen and its redistribution due to plasticity induced by in-situ loading. The rate of relaxation of the residual stress with respect to permanent deformation is a measure of the elastic follow-up associated with the residual stress field. Residual stress measurements were made using high energy dispersive X-ray diffraction. Digital image correlation, verified by strain gauges, was used to measure full-field deformation on the specimen. The specimen was loaded and unloaded in-situ incrementally to promote plasticity, allowing the relaxation rate of the residual stress to be quantified. An elastic follow-up factor was calculated for the residual stress field, that indicated loading conditions of the residual stress field between fixed-displacement and fixed-load.

The tensile behavior of TiZrNiCuBe metallic glass was studied using synchrotron X-ray diffraction and scanning electron microscopy. Shear band formation was carefully controlled by the introduction of a stress gradient due to a semi-circular notch. Micro- and atomic-level strains were calculated by the Q -space method and pair distribution function analysis, respectively. The atomic-pair strains for the area near the notch increase exponentially at the final deformation stage. This can be directly linked to the shear-induced dilatation resulting from the shear band formation.

A comparison of X-ray diffraction and radiographic techniques for the location and characterization of protein crystals is demonstrated on membrane protein crystals mounted within lipid cubic phase material., The focus in macromolecular crystallography is moving towards even more challenging target proteins that often crystallize on much smaller scales and are frequently mounted in opaque or highly refractive materials. It is therefore essential that X-ray beamline technology develops in parallel to accommodate such difficult samples. In this paper, the use of X-ray microradiography and microtomography is reported as a tool for crystal visualization, location and characterization on the macromolecular crystallography beamlines at the Diamond Light Source. The technique is particularly useful for microcrystals and for crystals mounted in opaque materials such as lipid cubic phase. X-ray diffraction raster scanning can be used in combination with radiography to allow informed decision-making at the beamline prior to diffraction data collection. It is demonstrated that the X-ray dose required for a full tomography measurement is similar to that for a diffraction grid-scan, but for sample location and shape estimation alone just a few radiographic projections may be required.

Ultrasonic melt processing is a promising technique for microstructural refinement in castings. Several mechanisms have been proposed for the observed effects, including cavitation-induced nucleation, activation of substrates and fragmentation. Until now, however, real-time experimental observations which could clarify any of the above mechanisms are very limited. For the first time we directly observed the fragmentation of primary crystals formed in alloys by ultrasonic cavitation. The primary crystals were extracted from real Al alloys and subjected to ultrasonic processing in water with in situ high-speed filming. The recordings of fragmentation of the primary crystals allowed us to observe the different mechanisms of fragmentation, depending on the mechanical properties and morphology of the primary crystals. The collapse of cavitation bubbles in water is less violent than that in liquid aluminum due to the lower cavitation threshold, viscosity and surface tension. Therefore the fragmentation mechanisms for the primary crystals observed in water should also be present for the same primary crystals in the more violent cavitation situation in liquid aluminum.

A new synchrotron-based technique for elemental imaging that combines radiography and fluorescence spectroscopy has been developed and applied to study the spatial distribution of Ag, Zr and Mo in an Al alloy during heating and melting to 700 and then re-soldification. For the first time, multi-element distributions have been mapped independently and simultaneously, showing the dissolution of Ag- and Zr-rich particles during melting and the inter-dendritic segregation of Ag during re-solidification. The new technique is shown to have wide potential for metallurgical and materials science applications where the dynamics of elemental re-distribution and segregation in complex alloys is of importance.

The present investigation establishes the feasibility of using synchrotron-generated X-ray beams for time-resolved in situ imaging and diffraction of the interior components of an internal combustion engine during its operation. The demonstration experiment was carried out on beamline I12 (JEEP) at Diamond Light Source, UK. The external hutch of the JEEP instrument is a large-scale engineering test bed for complex in situ processing and simulation experiments. The hutch incorporates a large capacity translation and rotation table and a selection of detectors for monochromatic and white-beam diffraction and imaging. These capabilities were used to record X-ray movies of a motorcycle internal combustion engine running at 1850 r.p.m. and to measure strain inside the connecting rod via stroboscopic X-ray diffraction measurement. The high penetrating ability and high flux of the X-ray beam at JEEP allowed the observation of inlet and outlet valve motion, as well as that of the piston, connecting rod and the timing chain within the engine. Finally, the dynamic internal strain within the moving connecting rod was evaluated with an accuracy of ∼50 × 10-6. © 2013 International Union of Crystallography.

Residual and thermal stresses have a considerable effect on the process of brittle fracture. In addition to this, the effect of these stresses on elastic-plastic fracture is known to be significant. This is accounted for in structural integrity assessment methodologies such as R6 Rev 4 and BS 7910:2013 by introducing factors representing the interaction between primary and secondary stresses (those that do and do not contribute towards plastic collapse, respectively). The initiation of ductile tearing in a ferritic pressure vessel steel was studied experimentally. Energy-dispersive X-ray diffraction was used to determine lattice strains in the vicinity of a crack tip in modified compact tension specimens at incremental loading steps until the initiation of ductile tearing. The X-ray diffraction measurements allowed the stress field to be evaluated with a high spatial resolution. At the same time, the pattern of total strain at the surface of the specimen was observed using digital image correlation. Prior to the experiment, two samples were subjected to localised out-of-plane compression ahead of the crack tip to introduce a residual stress field and hence significant crack loading in the absence of external load. Stress and strain field data for cracked specimens, with and without a pre-existing residual stress field, indicated significant differences in the development of plastic strain up to the point of tearing initiation. It is shown that this can only be explained when both residual stress and prior material hardening are taken into account.

Fast synchrotron X-ray microtomography was used to directly observe damage accumulation in a semi-solid Al-15 wt pct Cu alloy with a solid fraction of ~0.75 during isothermal tensile deformation. The evolution of damage was quantified in terms of size distribution of internal and surface-connected damage, strain mapping, and volume change to provide an insight into hot tear formation. A combination of existing void growth, void nucleation, and void coalescence all contribute to the final failure, although each dominates during different stages of deformation. Specifically, internal voids are shown to grow and coalesce from the region of high triaxiality at the center of the gage length outward and prove to be the contributing factor to final failure caused by insufficient liquid feeding.

Anin situenergy-dispersive X-ray diffraction experiment was undertaken on operational titanium electrowinning cells to observe the formation of rutile (TiO2) passivation layers on Magnéli-phase (TinO2n−1;n= 4–6) anodes and thus determine the relationship between passivation layer formation and electrolysis time. Quantitative phase analysis of the energy-dispersive data was undertaken using a crystal-structure-based Rietveld refinement. Layer formation was successfully observed and it was found that the rate of increase in layer thickness decreased with time, rather than remaining constant as observed in previous studies. The limiting step in rutile formation is thought to be the rate of solid-state diffusion of oxygen within the anode structure.

Semi-solid deformation has been directly observed in an Al–12 wt.% Cu alloy through the combination of real-time synchrotron X-ray radiography and a bespoke high-temperature tensile tester over a range of fraction solid from 0.35 to 0.98. During deformation at low and moderate fraction solids, the X-ray radiographs indicate that there is significant feeding of interdendritic liquid in the region of strain localization prior to crack formation. Furthermore, the measured load required to initiate localized tensile deformation was found to be similar over the range of fraction solid 0.35 to 0.66. At higher fraction solids, the radiographic observations are consistent with classical hot tearing behaviour: limited liquid flow due to low permeability; void nucleation and coalescence; and final failure. Based on these results, a three-stage mechanism for semi-solid failure is proposed which includes the effects of liquid flow and micro-neck formation.

Better understanding of the distribution of elastic and plastic strains in deformed polycrystalline, multiphase materials is important for structural engineering. The deformation response depends upon the interaction of grains of different orientations, and the anisotropy associated with each phase. Strain partitioning and tensile-compressive hardening asymmetry arises due to mismatches in modulus and ductility between grains and phases in alloys such as Ti-6Al-4V that displays both strong anisotropy within one phase and significant differences of properties between phases. Simple four-point bent beam samples were studied using the newly available energy-dispersive X-ray diffraction setup at the high energy white-beam synchrotron beamline I12 (JEEP) at Diamond Light Source. Diffraction patterns from the bent polycrystalline Ti6Al4V samples were collected using the new 23-cell "horseshoe" detector and interpreted using Pawley refinement to extract unit cell parameters, thus allowing elastic strain to be determined. The tensile-compressive hardening asymmetry was quantified for the grains oriented with the basal plane perpendicular to the loading direction. Initial evaluation of the performance of the new instrument is reported.

A novel, "single-shot" fluorescence imaging technique has been demonstrated on the B16 beamline at the Diamond Light Source synchrotron using the HEXITEC energy dispersive imaging detector. A custom made furnace with 200μm thick metal alloy samples was positioned in a white X-ray beam with a hole made in the furnace walls to allow the transmitted beam to be imaged with a conventional X-ray imaging camera consisting of a 500 μm thick single crystal LYSO scintillator, mirror and lens coupled to an AVT Manta G125B CCD sensor. The samples were positioned 45° to the incident beam to enable simultaneous transmission and fluorescence imaging. The HEXITEC detector was positioned at 90° to the sample with a 50 μm pinhole 13cm from the sample and the detector positioned 2.3m from pinhole. The geometric magnification provided a field of view of 1.1×1.1mm2 with one of the 80×80 pixels imaging an area equivalent to 13μm2. Al-Cu alloys doped with Zr, Ag and Mo were imaged in transmission and fluorescence mode. The fluorescence images showed that the dopant metals could be simultaneously imaged with sufficient counts on all 80x80 pixels within 60s, with the X-ray flux limiting the fluorescence imaging rate. This technique demonstrated that it is possible to simultaneously image and identify multiple elements on a spatial resolution scale ~10μm or higher without the time consuming need to scan monochromatic energies or raster scan a focused beam of X-rays. Moving to high flux beamlines and using an array of detectors could improve the imaging speed of the technique with element specific imaging estimated to be on a 1s timescale.

Cardiovascular stents are commonly made from 316L stainless steel and are deployed within stenosed arterial lesions using balloon expansion. Deployment involves inflating the balloon and plastically deforming the stent until the required diameter is obtained. This plastic deformation induces static stresses in the stent, which will remain for the lifetime of the device. In order to determine these stresses, finite element models of the unit cells of geometrically different, commercially available balloon expandable stents have been created, and deployment and elastic recoil have been simulated. In this work the residual stresses associated with deployment and recoil are compared for the various stent geometries, with a view to establishing appropriate initial stress states for fatigue loading for the stents. The maximum, minimum, and mean stresses induced in the stent due to systolic/diastolic pressure are evaluated, as are performance measures such as radial and longitudinal recoil.

Grain refinement via semi-solid deformation is desired to obtain superior mechanical properties of cast components. Using quantitative in situ synchrotron X-ray tomographic microscopy, we show an additional mechanism for the reduction of grain size, via liquation assisted transgranular cracking of semi-solid globular microstructures. Here we perform localized indentation of Al-15wt.%Cu globular microstructures, with an average grain size of ∼480 μm, at 555 °C (74% solid fraction). Although transgranular fracture has been observed in brittle materials, our results show transgranular fracture can also occur in metallic alloys in semi-solid state. This transgranular liquation cracking (TLC) occurs at very low contact stresses (between 1.1 and 38 MPa). With increasing strain, TLC continues to refine the size of the microstructure until the grain distribution reaches log-normal packing. The results demonstrate that this refinement, previously attributed to fragmentation of secondary arms by melt-shearing, is also controlled by an additional TLC mechanism., Nature Communications, 6, ISSN:2041-1723

A first attempt at the three-dimensional evaluation of naturally initiated surface connected and internal fatigue cracks is presented. Fatigue crack initiation and growth in air and vacuum environments have been investigated through X-ray microtomography in air and vacuum environments at elevated temperatures (350 °C), accompanied by post-mortem electron microscopy of the fracture surfaces. In vacuum ( 10 −5 mbar), multiple internal and surface-connected crack initiation was observed, but only the surface-connected cracks grew. In contrast, fewer cracks formed in air, these were mostly surface-connected and all were observed to grow. In all instances the initiation features were associated with globular primary α . An improved fatigue life was found in vacuum, which was mostly a consequence of delayed initiation, but was also due to slower fatigue crack propagation. The non-propagation of internal cracks was taken to imply that even the good laboratory vacuum obtained here was insufficient to simulate the conditions obtained for an internal crack in a component. The crack shape evolved towards a semi-circular shape a / c = 1 in air during fatigue crack growth, whilst the vacuum cracks remained semi-elliptical ( a / c ≃ 1.4 ). This was taken to imply that oxide-induced crack closure played a role in fatigue crack growth in air.

In the present study, residual stresses in the Powder Bed Direct Laser Deposition (PB DLD) built parts were investigated using X-ray diffraction strain measurement and finite element simulation. The microstructure and texture of the DLD built parts were studied, indicating that the vertically elongated grains have preferred orientation of (001)-type pointing in the growth direction in the nickel superalloy C263. A conceptual model of residual stress generation was proposed using fictitious thermal expansion based on the argument that residual stresses arise from strain incompatibility that is "frozen in" within the work piece during fabrication.

In this work three-dimensional crystal plasticity finite element models are used to simulate the tensile deformation of a thin 316LVM stainless steel specimen. Such models are of interest for predicting the mechanical response of cardiovascular stents, typically made from thin struts of this material. Detailed experimental analysis of the mechanical response of the specimen during deformation is performed using scanning electron microscopy, digital photogrammetry and orientation imaging microscopy to examine microscale strain distribution, plastic slip and grain reorientation. At the macroscale, the models are found to give good predictions of the stress–strain response of the specimen, and at the microscale the models are found to give good predictions of the strain distribution and the active slip systems in the different grains. The models are less successful in predicting grain reorientations. This, however, is shown to be quite sensitive to the choice of latent hardening ratio.

Mechanical devices are being introduced whose size scale is well below that of conventional mechanical test specimens. The smallest devices have sizes in the nanometer range, though ag ood proportion of structural devices are of the micrometer scale. Development of these products raises the question of how their mechanical behaviour and reliability may be predicted. Conventional macroscopic test data can be used, but these are obtained using specimens whose size is much larger than the devices themselves. There is a risk that performance predictions will be inaccurate, due to the existence of size effects. This paper covers small size scale testing in metallic specimens and devices, concentrating on free- standing specimens. To begin, some examples of micro-scale devices are given. Fabrication methods for small metallic devices are then briefly described. This is followed by a review of experimental observations of mechanical properties in various metallic materials at the micro-scale, highlighting the differences in results from different research groups and the gaps in our current knowledge. A section on computational and predictive modelling is included, in recognition of the role of modelling in device design and testing. Overall, the findings are that size effects are common, particularly in crystalline samples when the grain size is similar to one or more of the specimen dimensions. However, observations of size effects differ between studies and mechanical properties can vary widely, even for the same type of material. As a consequence, the relationships between specific device processing methods, specimen size and material properties must be adequately understood to ensure successful performance.

Synchrotron X-ray microtomography has been utilized for the in-situ observation of steady-state plane-strain fatigue crack growth. A high-resolution experimental configuration and phase contrast imaging technique have enabled the reconstruction of crack images with an isotropic voxel with a 0.7 µm edge. The details of a crack are readily observed, together with evidence of the incidence and mechanical influence of closure. After preliminary investigations of the achievable accuracy and reproducibility, a variety of measurement methods are used to quantify crack-opening displacement (COD) and closure from the tomography data. Utilization of the physical displacements of microstructural features is proposed to obtain detailed COD data, and its feasibility is confirmed. Loss of fracture surface contact occurs gradually up to the maximum load. This is significantly different from tendencies reported where a single definable opening level is essentially assumed to exist. The closure behaviour is found to be attributable mainly to pronounced generation of mode III displacement which may be caused by local crack topology. Many small points of closure still remain near the crack tip, suggesting that the near-tip contact induces crack growth resistance. The effects of overloading are also discussed.

Tests were performed to assess the feasibility of bonding single crystal silicon to copper and aluminium nitride. The application of the bonded component is in a cryocooled monochromator for synchrotron X-ray optics. Aluminium, gold and indium–silver interlayers were tried. Some bonded components were tested by immersion in liquid nitrogen to simulate cooling of the component in service. Although bonds could be formed, they were of insufficient integrity for use in a challenging cryogenic application.

Recent developments of synchrotron X-ray sources and dedicated high-energybeamlines are now enabling strain measurements from large volumes of industrially relevant metallic materials. Such capability is allowing the validation of novel and alternative non-destructive experimental methods of strain measurement or computational models of complex deformation processes. This study describes the first dynamic contact strain measurement of a ball bearing using stroboscopic Energy Dispersive X-ray Diffraction (EDXD). The experiment probed the dynamic contact strain in the outer raceway of a test bearing. The inner raceway of the bearing was attached to a shaft rotating at 150 revolutions per minute and the outer raceway, where the measurements were made, was fixed in a stationary bearing housing. A triggering system was used to synchronise the data acquisition of the EDXD detector with the bearing rotation. Specifically, diffraction data was acquired, stroboscopically, from the material volume within the raceway, in a known location, when the ball was positioned directly below it. A total of 20 seconds of accumulated diffraction signal was recorded, acquiring 2 milliseconds of data per revolution, providing diffraction patterns of sufficient quality for the dynamic contact strain to be measured. Macromechanical stress field was calculated from the micromechanicalstrains measured from five lattice planes. This allowed a comparison of theexperimentally measured stress field and that of finite element (FE) simulations. Good agreement was observed between the finite element results and experimental measurements indicating the applicability of this novel dynamic strain measurement technique for tribological systems.

The effect of a Pulsed Electro Magnetic Field (PEMF) on the solidification of an Al-15 wt%Cu alloy was studied in situ by synchrotron X-ray radiography. Samples were solidified with and without the presence of the PEMF while recording radiographs, enabling observation and quantification of dendrite fragmentation by image analysis. Fragmentation increased with a PEMF and was attributed to induced inter-dendritic flow. © (2013) Trans Tech Publications, Switzerland.