Why Is It So Challenging to Measure Residual Stresses ?

Background: Residual stresses have a "hidden" character because they exist in a material without the presence of any external loads. They cannot easily be added or subtracted in a quantified manner, as is done when measuring applied stresses, and so are much more challenging to measure. Objective: The objective here is to identify and describe the various features that make residual stress measurement methods challenging and to consider the ways that these challenges can be addressed in practice. Methods: Various of the most common residual stress measurements methods are considered and the challenges associated with them are identified and classified. Results: Five major challenges for residual stress measurements, and the approaches used for their resolution, are identified. Conclusions: Despite the various challenges that need to be overcome, residual stress measurements can be successfully undertaken in practice. The most significant feature for success is a highly skilled and knowledge practitioner.

A new direction for tackling phosphorus inefficiency in the UK food system.

The UK food system is reliant on imported phosphorus (P) to meet food production demand, though inefficient use and poor stewardship means P is currently accumulating in agricultural soils, wasted or lost with detrimental impacts on aquatic environments. This study presents the results of a detailed P Substance Flow Analysis for the UK food system in 2018, developed in collaboration with industry and government, with the key objective of highlighting priority areas for system interventions to improve the sustainability and resilience of P use in the UK food system. In 2018 the UK food system imported 174.6 Gg P, producing food and exportable commodities containing 74.3 Gg P, a P efficiency of only 43%. Three key system hotspots for P inefficiency were identified: Agricultural soil surplus and accumulation (89.2 Gg P), loss to aquatic environments (26.2 Gg P), and waste disposal to landfill and construction (21.8 Gg P). Greatest soil P accumulation occurred in grassland agriculture (85% of total accumulation), driven by loadings of livestock manures. Waste water treatment (12.5 Gg P) and agriculture (8.38 Gg P) account for most P lost to water, and incineration ashes from food system waste (20.3 Gg P) accounted for nearly all P lost to landfill and construction. New strategies and policy to improve the handling and recovery of P from manures, biosolids and food system waste are therefore necessary to improve system P efficiency and reduce P accumulation and losses, though critically, only if they effectively replace imported mineral P fertilisers.

Core Imaging Library - Part I: a versatile Python framework for tomographic imaging.

We present the Core Imaging Library (CIL), an open-source Python framework for tomographic imaging with particular emphasis on reconstruction of challenging datasets. Conventional filtered back-projection reconstruction tends to be insufficient for highly noisy, incomplete, non-standard or multi-channel data arising for example in dynamic, spectral and in situ tomography. CIL provides an extensive modular optimization framework for prototyping reconstruction methods including sparsity and total variation regularization, as well as tools for loading, preprocessing and visualizing tomographic data. The capabilities of CIL are demonstrated on a synchrotron example dataset and three challenging cases spanning golden-ratio neutron tomography, cone-beam X-ray laminography and positron emission tomography. This article is part of the theme issue 'Synergistic tomographic image reconstruction: part 2'.

Completing the picture through correlative characterization.

Natural and manufactured materials rely on complex hierarchical microstructures to deliver a suite of interesting properties. To predict and tailor their performance requires a joined-up knowledge of their multiphase microstructure, interfaces, chemistry and crystallography from the nanoscale to the macroscale. This Perspective reflects on how recent developments in correlative characterization can bring together multiple image modalities and maps of the local chemistry, structure and functionality to form rich multimodal and multiscale correlated datasets. The automated collection and digitization of multidimensional data is an essential part of the picture for developing multiscale modelling and 'big data'-driven machine learning approaches. These are needed to both improve our understanding of existing materials and exploit high-throughput combinatorial synthesis, processing and testing methods to develop materials with bespoke properties.

Phosphorus stocks and flows in an intensive livestock dominated food system.

Current use and management of phosphorus (P) in our food systems is considered unsustainable and considerable improvements in the efficiency of P use are required to mitigate the environmental impact of poor P stewardship. The inherent low P use efficiency of food production from animals means food systems dominated by livestock agriculture can pose unique challenges for improving P management. This paper presents the results of a substance flow analysis for P in the Northern Ireland (NI) food system for the year 2017 as a case study for examining P stewardship in a livestock dominated agricultural system. Imported livestock feed was by far the largest flow of P into the NI food system in 2017 (11,700 t ± 1300 t) and P from livestock excreta the largest internal flow of P (20,400 ± 1900t). The P contained in livestock slurries and manures alone that were returned to agricultural land exceeded total crop and grass P requirement by 20% and were the largest contributor to an annual excess soil P accumulation of 8.5 ± 1.4 kg ha-1. This current livestock driven P surplus also limits the opportunities for P circularity and reuse from other sectors within the food system, e.g. wastewater biosolids and products from food processing waste. Management of livestock P demand (livestock numbers, feed P content) or technological advancements that facilitate the processing and subsequent export of slurries and manures are therefore needed.

Comparison of grain to grain orientation and stiffness mapping by spatially resolved acoustic spectroscopy and EBSD.

Our aim was to establish the capability of spatially resolved acoustic spectroscopy (SRAS) to map grain orientations and the anisotropy in stiffness at the sub-mm to micron scale by comparing the method with electron backscatter diffraction (EBSD) undertaken within a scanning electron microscope. In the former the grain orientations are deduced by measuring the spatial variation in elastic modulus; conversely, in EBSD the elastic anisotropy is deduced from direct measurements of the crystal orientations. The two test-cases comprise mapping the fusion zones for large TIG and MMA welds in thick power plant austenitic and ferritic steels, respectively; these are technologically important because, among other things, elastic anisotropy can cause ultrasonic weld inspection methods to become inaccurate because it causes bending in the paths of sound waves. The spatial resolution of SRAS is not as good as that for EBSD (∼100 µm vs. ∼a few nm), nor is the angular resolution (∼1.5° vs. ∼0.5°). However the method can be applied to much larger areas (currently on the order of 300 mm square), is much faster (∼5 times), is cheaper and easier to perform, and it could be undertaken on the manufacturing floor. Given these advantages, particularly to industrial users, and the on-going improvements to the method, SRAS has the potential to become a standard method for orientation mapping, particularly in cases where the elastic anisotropy is important over macroscopic/component length scales.

Time-lapse lab-based x-ray nano-CT study of corrosion damage.

An experimental protocol (workflow) has been developed for time-lapse x-ray nanotomography (nano-CT) imaging of environmentally driven morphological changes to materials. Two case studies are presented. First, the leaching of nanoparticle corrosion inhibitor pigment from a polymer coating was followed over 14 days, while in the second case the corrosion damage to an AA2099 aluminium alloy was imaged over 12 hours. The protocol includes several novel aspects relevant to nano-CT with the use of a combination of x-ray absorption and phase contrast data to provide enhanced morphological and composition information, and hence reveal the best information to provide new insights into the changes of different phases over time. For the pigmented polymer coating containing nominally strontium aluminium polyphosphate, the strontium-rich components within the materials are observed to leach extensively whereas the aluminium-rich components are more resistant to dissolution. In the case of AA2099 it is found that the initial grain boundary corrosion is driven by the presence of copper-rich phases and is then followed by the corrosion of grains of specific orientation.

Determining the Effect of Drying Time on Phosphorus Solubilization from Three Agricultural Soils under Climate Change Scenarios.

Climate projections for the future indicate that the United Kingdom will experience hotter, drier summers and warmer, wetter winters, bringing longer dry periods followed by rewetting. This will result in changes in phosphorus (P) mobilization patterns that will influence the transfer of P from land to water. We tested the hypothesis that changes in the future patterns of drying-rewetting will affect the amount of soluble reactive phosphorus (SRP) solubilized from soil. Estimations of dry period characteristics (duration and temperature) under current and predicted climate were determined using data from the UK Climate Projections (UKCP09) Weather Generator tool. Three soils (sieved <2 mm), collected from two regions of the United Kingdom with different soils and farm systems, were dried at 25°C for periods of 0, 2, 4, 5, 6, 8, 10, 15, 20, 25, 30, 60, and 90 d, then subsequently rewetted (50 mL over 2 h). The solubilized leachate was collected and analyzed for SRP. In the 2050s, warm period temperature extremes >25°C are predicted in some places and dry periods of 30 to 90 d extremes are predicted. Combining the frequency of projected dry periods with the SRP concentration in leachate suggests that this may result overall in increased mobilization of P; however, critical breakpoints of 6.9 to 14.5 d dry occur wherein up to 28% more SRP can be solubilized following a rapid rewetting event. The precise cause of this increase could not be identified and warrants further investigation as the process is not currently included in P transfer models.

A comparison of different approaches for imaging cracks in composites by X-ray microtomography.

X-ray computed tomography (CT) has emerged as a key imaging tool in the characterization of materials, allowing three-dimensional visualization of an object non-destructively as well as enabling the monitoring of damage accumulation over time through time-lapse imaging. However, small defects and cracks can be difficult to detect, particularly in composite materials where low-contrast, plate-like geometries of large area can compromise detectability. Here, we investigate a number of strategies aimed at increasing the capability of X-ray CT to detect composite damage such as transverse ply cracking and delamination, looking specifically at a woven glass fibre-reinforced three-dimensional composite. High-resolution region of interest (ROI) scanning, in situ loading, phase contrast and contrast agents are examined systematically as strategies for improving the defect detectability. Spatial resolution, contrast, signal-to-noise ratio, full width at half maximum, user friendliness and measurement time are all considered. Taken together, the results suggest that high-resolution ROI scanning combined with the increased contrast resulting from staining give the highest defect detectability. This article is part of the themed issue 'Multiscale modelling of the structural integrity of composite materials'.

Dynamic damage in carbon-fibre composites.

The Taylor test is used to determine damage evolution in carbon-fibre composites across a range of strain rates. The hierarchy of damage across the scales is key in determining the suite of operating mechanisms and high-speed diagnostics are used to determine states during dynamic loading. Experiments record the test response as a function of the orientation of the cylinder cut from the engineered multi-ply composite with high-speed photography and post-mortem target examination. The ensuing damage occurs during the shock compression phase but three other tensile loading modes operate during the test and these are explored. Experiment has shown that ply orientations respond to two components of release; longitudinal and radial as well as the hoop stresses generated in inelastic flow at the impact surface. The test is a discriminant not only of damage thresholds but of local failure modes and their kinetics. This article is part of the themed issue 'Multiscale modelling of the structural integrity of composite materials'.

How changing root system architecture can help tackle a reduction in soil phosphate (P) levels for better plant P acquisition.

The readily available global rock phosphate (P) reserves may run out within the next 50-130 years, causing soils to have a reduced P concentration which will affect plant P uptake. Using a combination of mathematical modelling and experimental data, we investigated potential plant-based options for optimizing crop P uptake in reduced soil P environments. By varying the P concentration within a well-mixed agricultural soil, for high and low P (35.5-12.5 mg L(-1) respectively using Olsen's P index), we investigated branching distributions within a wheat root system that maximize P uptake. Changing the root branching distribution from linear (evenly spaced branches) to strongly exponential (a greater number of branches at the top of the soil) improves P uptake by 142% for low-P soils when root mass is kept constant between simulations. This causes the roots to emerge earlier and mimics topsoil foraging. Manipulating root branching patterns, to maximize P uptake, is not enough on its own to overcome the drop in soil P from high to low P. Further mechanisms have to be considered to fully understand the impact of P reduction on plant development.

Fracture mechanics by three-dimensional crack-tip synchrotron X-ray microscopy.

To better understand the relationship between the nucleation and growth of defects and the local stresses and phase changes that cause them, we need both imaging and stress mapping. Here, we explore how this can be achieved by bringing together synchrotron X-ray diffraction and tomographic imaging. Conventionally, these are undertaken on separate synchrotron beamlines; however, instruments capable of both imaging and diffraction are beginning to emerge, such as ID15 at the European Synchrotron Radiation Facility and JEEP at the Diamond Light Source. This review explores the concept of three-dimensional crack-tip X-ray microscopy, bringing them together to probe the crack-tip behaviour under realistic environmental and loading conditions and to extract quantitative fracture mechanics information about the local crack-tip environment. X-ray diffraction provides information about the crack-tip stress field, phase transformations, plastic zone and crack-face tractions and forces. Time-lapse CT, besides providing information about the three-dimensional nature of the crack and its local growth rate, can also provide information as to the activation of extrinsic toughening mechanisms such as crack deflection, crack-tip zone shielding, crack bridging and crack closure. It is shown how crack-tip microscopy allows a quantitative measure of the crack-tip driving force via the stress intensity factor or the crack-tip opening displacement. Finally, further opportunities for synchrotron X-ray microscopy are explored.

Employing temporal self-similarity across the entire time domain in computed tomography reconstruction.

There are many cases where one needs to limit the X-ray dose, or the number of projections, or both, for high frame rate (fast) imaging. Normally, it improves temporal resolution but reduces the spatial resolution of the reconstructed data. Fortunately, the redundancy of information in the temporal domain can be employed to improve spatial resolution. In this paper, we propose a novel regularizer for iterative reconstruction of time-lapse computed tomography. The non-local penalty term is driven by the available prior information and employs all available temporal data to improve the spatial resolution of each individual time frame. A high-resolution prior image from the same or a different imaging modality is used to enhance edges which remain stationary throughout the acquisition time while dynamic features tend to be regularized spatially. Effective computational performance together with robust improvement in spatial and temporal resolution makes the proposed method a competitive tool to state-of-the-art techniques.

Exploration of fs-laser ablation parameter space for 2D/3D imaging of soft and hard materials by tri-beam microscopy.

Tri-beam microscopes comprising a fs-laser beam, a Xe+ plasma focused ion beam (PFIB) and an electron beam all in one chamber open up exciting opportunities for site-specific correlative microscopy. They offer the possibility of rapid ablation and material removal by fs-laser, subsequent polishing by Xe-PFIB milling and electron imaging of the same area. While tri-beam systems are capable of probing large (mm) volumes providing high resolution microscopical characterisation of 2D and 3D images across exceptionally wide range of materials and biomaterials applications, presenting high quality/low damage surfaces to the electron beam can present a significant challenge, especially given the large parameter space for optimisation. Here the optimal conditions and artefacts associated with large scale volume milling, mini test piece manufacture, serial sectioning and surface polishing are investigated, both in terms of surface roughness and surface quality for metallic, ceramic, mixed complex phase, carbonaceous, and biological materials. This provides a good starting place for those wishing to examine large areas or volumes by tri-beam microscopy across a range of materials.

Region-of-interest tomography using filtered backprojection: assessing the practical limits.

There are many cases where it is desirable to reconstruct at high resolution a small volume from a larger sample. Here we describe the outcomes of a reconstruction trial based on real samples aimed at delineating the practical limits to which a small region of interest can be viewed from a large sample. Our approach has been to artificially truncate the sinograms of whole sample scans to simulate region of interest tomography. A simple filtered back projection algorithm has been applied, with the sinograms extended laterally in a simple manner to make up for the truncated portions. The impact of the degree of truncation (from 0% down to 99%), the number of projections used, as well as the position of the region of interest, on the faithfulness of the reconstruction is evaluated for a range of sample types. We have assessed the nature of, and extent to which, artefacts are introduced and the degree to which simple strategies can minimize them to an acceptable level without the need for complex reconstruction algorithms, projection stitching strategies or very large detectors. It is found that for a wide range of objects the effect of truncation on feature detection is negligible and that excellent images can be reconstructed if the number of projections is calculated not on the basis of the number of pixels on the camera, but on the number of pixels that would be required to scan the whole sample at the chosen pixel resolution. This paper demonstrates that in many cases more sophisticated reconstruction strategies are not necessary.

Macro-, meso- and microstructural characterization of metallic lattice structures manufactured by additive manufacturing assisted investment casting.

Cellular materials are recognized for their high specific mechanical properties, making them desirable in ultra-lightweight applications. Periodic lattices have tunable properties and may be manufactured by metallic additive manufacturing (AM) techniques. However, AM can lead to issues with un-melted powder, macro/micro porosity, dimensional control and heterogeneous microstructures. This study overcomes these problems through a novel technique, combining additive manufacturing and investment casting to produce detailed investment cast lattice structures. Fused filament fabrication is used to fabricate a pattern used as the mold for the investment casting of aluminium A356 alloy into high-conformity thin-ribbed (~ 0.6 mm thickness) scaffolds. X-ray micro-computed tomography (CT) is used to characterize macro- and meso-scale defects. Optical and scanning electron (SEM) microscopies are used to characterize the microstructure of the cast structures. Slight dimensional (macroscale) variations originate from the 3D printing of the pattern. At the mesoscale, the casting process introduces very fine (~ 3 µm) porosity, along with small numbers of (~ 25 µm) gas entrapment defects in the horizontal struts. At a microstructural level, both the (~ 70 µm) globular/dendritic grains and secondary phases show no significant variations across the lattices. This method is a promising alternative means for producing highly detailed non-stochastic metallic cellular lattices and offers scope for further improvement through refinement of filament fabrication.

Correction of artefacts associated with large area EBSD.

There is an increasing requirement for the acquisition of large two (2D) or three (3D) dimensional electron back scattered diffraction (EBSD) maps. It is a well-known, but largely neglected fact, that EBSD maps may contain distortions. These include long-range distortions, which can be caused by the interaction of the electron beam with the sample geometry and it can also arise from sample or beam drift. In addition there are shorter range artefacts arising from topographical features, such as curtaining. The geometrical distortions can be minimised by careful SEM calibrations and sample alignment. However, the long-range distortions become increasingly prevalent when acquiring large area 2D EBSD maps which take a long time to acquire and thus are especially prone to drift. These distortions are especially evident in serial section tomography (SST) when 2D maps are stacked on top of one another to produce 3D maps. Here we quantify these distortions for large area EBSD data by referencing them to secondary electron (SE) images for 3D-EBSD data acquired on a WCCo hardmetal. Long-range distortions (due to drift) equating to around 10µm across a 200µm x 175 µm area map, and short-range distortions (due to topographical effects) as large as 3 µm over a distance of 40 µm were observed. Methods for correcting these distortions are then proposed. This study illustrates the benefits and necessity of such corrections if morphological features are to be properly interpreted when collecting large 3D EBSD datasets, for example by mechanical sectioning, serial block face SEM ultramicrotomy, laser sectioning, FIB-SEM tomography, PFIB spin milling, etc.

3D characterisation of dry powder inhaler formulations: Developing X-ray micro computed tomography approaches.

Carrier-based dry powder inhaler (DPI) formulations need to be accurately characterised for their particle size distributions, surface roughnesses, fines contents and flow properties. Understanding the micro-structure of the powder formulation is crucial, yet current characterisation methods give incomplete information. Commonly used techniques like laser diffraction (LD) and optical microscopy (OM) are limited due to the assumption of sphericity and can give variable results depending on particle orientation and dispersion. The aim of this work was to develop new three dimensional (3D) powder analytical techniques using X-ray computed tomography (XCT) that could be employed for non-destructive metrology of inhaled formulations. α-lactose monohydrate powders with different characteristics have been analysed, and their size and shape (sphericity/aspect ratio) distributions compared with results from LD and OM. The three techniques were shown to produce comparable size distributions, while the different shape distributions from XCT and OM highlight the difference between 2D and 3D imaging. The effect of micro-structure on flowability was also analysed through 3D measurements of void volume and tap density. This study has demonstrated for the first time that XCT provides an invaluable, non-destructive and analytical approach to obtain number- and volume-based particle size distributions of DPI formulations in 3D space, and for unique 3D characterisation of powder micro-structure.

Mitigating diffuse phosphorus transfer from agriculture according to cost and efficiency.

Potential options for mitigating phosphorus (P) transfer from agriculture to water in England and Wales (E&W) were collated across a range of farm systems to assess their potential effectiveness in reducing mass of P transferred and potential cost (pounds sterling [ pound]) to the farming industry. A simple model framework (called PEASE) incorporating a number of assumptions was used to identify 15 methods for mitigating inputs of P to agricultural systems, 19 methods for preventing mobilization of P, and six methods for controlling the transport of P to streams. The scope for largest reductions in P inputs was to grassland and horticulture. Potential reductions in P mobilization were up to 1.2 kg P ha(-1). Reductions in P transfer associated with transport mitigation were larger than those associated with input and mobilization methods (up to 2.2 kg P ha(-1)). The largest estimated reductions were achieved by installing buffer zones and constructed wetlands, the former being very cost effective ( pound3-5 kg(-1) P saved). Plots of cost curves helped identify where the combined and cumulative P transfer reductions were attainable; these were approximately 0.2 kg ha(-1) for uplands, 0.6 kg ha(-1) for outdoor pigs, 0.9 kg ha(-1) for intensive dairy, and 2.2 kg ha(-1) for arable examples. We concluded that established catchment-scale evidence for mitigation is sparse, especially for specific farm systems in E&W. Sensitivities and uncertainties in the approach, especially associated with expert coefficients, are noted. This approach is nonetheless considered useful for prioritizing where and how best options might be most effectively targeted for least cost but greatest benefit.

Characterization of phosphorus sources in rural watersheds.

Correct identification of P sources in rural watersheds is critical for the development of cost-effective measures to combat agriculturally-driven eutrophication. The chemical composition of various storm runoff types (field surface runoff, field drain outfalls, roads, farmyards, and septic tanks) and the receiving streams in three micro (<10 km(2)) watersheds of varying agricultural intensity were monitored over a 2-yr period. Mean weekly stream soluble reactive phosphorus (SRP) and total phosphorus (TP) concentrations increased from 29 and 69 microg L(-1), respectively in the watershed with the lowest intensity agriculture to 382 and 503 microg L(-1), respectively in the watershed with high intensity agriculture and a village sewage treatment works. Concentrations of TP in storm runoff varied by up to two orders of magnitude reflecting the complex origins, routing, and composition of contributing source areas. Application of the DESPRAL test suggested field runoff TP concentrations were influenced by both P and organic matter in soil. However, runoff from impervious surfaces (farmyard and roads), and/or influenced by septic tank discharges, was significantly more concentrated (0.08-16 mg TP L(-1), mean >>1 mg L(-1)) than surface and subsurface runoff from cultivated land and pasture (0.02-3.6 mg TP L(-1), mean <1 mg L(-1)), and/or contained a significantly greater proportion (>50% vs. <50%) of P in dissolved forms. It is concluded that P sources associated with the functioning of rural communities (impervious surfaces, detergents, and wastewater) may be more ecologically relevant than those associated with agriculture and should be better quantified and controlled to avoid localized eutrophication impacts.