Dr Tan Sui

Despite the elaborate varieties of iridescent colors in biological species, most of them are reflective. Here we show the rainbow-like structural colors found in the ghost catfish (Kryptopterus vitreolus), which exist only in transmission. The fish shows flickering iridescence throughout the transparent body. The iridescence originates from the collective diffraction of light after passing through the periodic band structures of the sarcomeres inside the tightly stacked myofibril sheets, and the muscle fibers thus work as transmission gratings. The length of the sarcomeres varies from ~1 μm from the body neutral plane near the skeleton to ~2 μm next to the skin, and the iridescence of a live fish mainly results from the longer sarcomeres. The length of the sarcomere changes by ~80 nm as it relaxes and contracts, and the fish shows a quickly blinking dynamic diffraction pattern as it swims. While similar diffraction colors are also observed in thin slices of muscles from non-transparent species such as the white crucian carps, a transparent skin is required indeed to have such iridescence in live species. The ghost catfish skin is of a plywood structure of collagen fibrils, which allows more than 90% of the incident light to pass directly into the muscles and the diffracted light to exit the body. Our findings could also potentially explain the iridescence in other transparent aquatic species, including the eel larvae (Leptocephalus) and the icefishes (Salangidae).

In this work, novel bioinspired polyurethane (PU) scaffolds were fabricated via freeze casting for PU-based Pancreatic Ductal Adenocarcinoma (PDAC) model. In order to reproduce the tumour micro-environment that facilitates cellular kinetics, the PU scaffolds were surface modified with extracellular matrix (ECM) proteins including collagen and fibronectin (Col and FN). Synchrotron-based small- and wide-angle X-ray scattering (SAXS/WAXS) techniques were applied to probe structural evolution during in situ mechanical testing. Strains at macroscopic, nano-, and lattice scales were obtained to investigate the effects of ECM proteins and pancreatic cell activities to PU scaffolds. Significant mechanical strengthening across length scales of PU scaffolds was observed in specimens surface modified by FN. A model of stiffness modulation via enhanced interlamellar recruitment is proposed to explain the multi-scale strengthening mechanisms. Understanding multi-scale deformation mechanisms of a series of PU scaffolds opens an opportunity in developing a novel pancreatic cancer model for studying cancer evolution and predicting outcomes of drug/treatments.

Despite the long-established rocking-chair theory of lithium-ion batteries (LIBs), developing novel characterization methodology with higher spatiotemporal resolution facilitates a better understanding of the solid electrolyte interphase studies to shape the reaction mechanisms. In this work, we develop a Xenon ion plasma focused ion beam (Xe+ PFIB)-based characterization technique to probe the cross-sectional interface of both ternary cathode and graphite anode electrodes, with the focus on revealing the chemical composition and distribution underneath the electrode surface by in-depth analysis of secondary ions. Particularly, the lithium fluoride is detected in the pristine cathode prior to contact with the electrolyte, reflecting that the electrode degradation is in the form of the loss of lithium inventory during electrode preparation. This degradation is related to the hydrolysis of the cathode material and the decomposition of the PVDF binder. Through the quantitative analysis of the transition-metal degradation products, manganese is found to be the dominant element in the newly formed inactive fluoride deposition on the cathode, while no transition metal signal can be found inside the anode electrode. These insights at high resolution implemented via a PFIB-based characterization technique not only enrich the understanding of the degradation mechanism in the LIBs but also identify and enable a high-sensitivity methodology to obtain the chemical survey at the subsurface, which will help remove the capacity-fade observed in most LIBs.

In this manuscript, we elucidated, for the first time, the substructural mechanisms present in our recently developed bioinspired polyurethane-based pancreatic tissue models. Different protein coatings of the model, i.e., collagen and fibronectin were examined. More specifically, analysis took place by combined real-time synchrotron X-ray scattering techniques and confocal laser scanning microscopy, to quantify the structural alteration of uncoated-polyurethane (PU) and protein-coated PU as well as the time-resolved structural reorganisation occurring at the micro-, nano- and lattice length scales during in situ micromechanical testing. We demonstrate that a clear increase of stiffness at the lamellar level following the fibronectin-PU modification, which is linked to the changes in the mechanics of the lamellae and interlamellar cohesion. This multi-level analysis of structural-mechanical relations in this polyurethane-based pancreatic cancer tissue model opens an opportunity in designing mechanically robust cost-effective tissue models not only for fundamental research but also for treatment screening.

Precipitation hardened Copper-Chromium-Zirconium (CuCrZr) alloy is a prime candidate for divertor components in future European DEMOnstration (DEMO) fusion reactors. To develop the DEMO Design Criteria for In-vessel Components (DDC-IC), the failure criterion of CuCrZr needs to be investigated. Hence, the effects of stress triaxiality and loading strain rate on the fracture of solution heat treated and annealed CuCrZr alloys were studied using digital-imaging-correlation and electron microscopy techniques. It was found that an increase in the stress triaxiality caused a significant decrease of over 50% in the equivalent strain to fracture. On the other hand, increasing applied strain rate from 1.3 × 10−5 s−1to 8.6 × 10−3 s−1 had no considerable effects on the yield stress and elongation. However, higher flow stresses and a larger number density of voids were observed under the highest applied strain rate of 8.6 × 10−3 s−1. Fracture surface analysis showed that the failure model was dominated by void growth and coalescence for all the tests. This work has been performed within the Engineering Data and Design Integration (EDDI) sub-project of the EUROfusion Materials work package and aimed to contribute to the development of the DEMO Design Criteria for In-vessel Components.

A green electrical energy source is suggested in this study to reduce carbon emissions for application in wearable flexible smart sensors/electronics/medical devices. Fish scales of Rohu fish are used to produce electricity by designing and fabricating triboelectric nanogenerators 2 which need only human motion instead of a battery to produce electricity for self powered sensors and IoT devices. These fish scales are available in abundance in a fish market as a waste material globally. These scales are transparent, flexible, non-toxic, biodegradable, biocompatible, and cheaper (free of cost) material. A very simple design, fabrication, and operation technique is proposed in this study. The various characterization techniques SEM, EDX, FTIR, and XRD are performed on the fish scale because triboelectricity generation depends upon the material composition and surface morphology. The SEM results show a distinct surface pattern of the scale which is helpful for triboelectric charge generation. The EDX shows the basic elemental composition in which Carbon, Nitrogen, and Oxygen are dominant. Further, the FTIR spectrum shows the presence of different bio proteins including keratin, collagens, chitin, etc. Thermogravimetric analysis shows that a fish scale-based fabricated device is capable of working under 200 0 C. A comparative analysis of the triboelectric performance of fish scale with other already reported biomaterials eggshell membrane, dog hair, and bombax ceiba tree cotton is also presented in this study along with highly tribonegative material PTFE. The results of this study help to estimate the position of the novel fish scale material in the triboelectric series. The electrical output of this fish scale-based device is used to light up 90 commercial green LEDs which is equivalent to 180V. The current of value 1.7µA has been measured across the 1MΩ resistor. To present the potential application of the fabricated device, a digital calculator is Switch ON using electricity produced from the fish scale based device.

Objective Dental erosion is a common oral condition caused by chronic exposure to acids from intrinsic/extrinsic sources. Repeated acid exposure can lead to the irreversible loss of dental hard tissues (enamel, dentine, cementum). Dentine can become exposed to acid following severe enamel erosion, crown fracture, or gingival recession. Causing hypersensitivity, poor aesthetics, and potential pulp involvement. Improving treatments that can restore the structural integrity and aesthetics are therefore highly desirable. Such developments require a good understanding of how acid demineralisation progresses where relatively little is known in terms of intertubular dentine (ITD) and peritubular dentine (PTD) microstructure. To obtain further insight, this study proposes a new in vitro method for performing demineralisation studies of dentine. Methods Advanced high-speed synchrotron X-ray microtomography (SXM), with high spatial (0.325 µm) and temporal (15 min) resolution, was used to conduct the first in vitro, time-resolved 3D (4D) study of the microstructural changes in the ITD and PTD phases of human dentine samples (~0.8×0.8×5 mm) during 6 h of continuous acid exposure.

•Through-thickness residual stress distribution in three dimensions is evaluated.•High-resolution residual strain is mapped by neutron Bragg edge imaging.•Location-dependent reference lattice spacing is first applied on neutron imaging.•Correlation between microstructure, residual stress and micro-hardness is studied. Eurofer97 steel is a primary structural material for applications in fusion reactors. Laser welding is a promising technique to join Eurofer97 plasma-facing components and overcome remote handling and maintenance challenges. The interaction of the induced residual stress and the heterogeneous microstructure degrades the mechanical performance of such fusion components. The present study investigates the distribution of residual stresses of as-welded and post-heat treated Eurofer97 joints. The mechanistic connections between microstructure, material properties, and residual stress are also studied. The neutron diffraction is used to study the through-thickness residual stress distribution in three directions, and neutron Bragg edge imaging (NBEI) is applied to study the residual strain in high spatial resolution. The microstructures and micro-hardness are characterised by electron backscatter diffraction and nanoindentation, respectively. The M-shaped residual stress distribution through the thickness of the as-welded weldment is observed by neutron diffraction line scans over a region of 1.41 × 10 mm2. These profiles are cross-validated over a larger area (∼56 × 40 mm2) with the higher spatial resolution by NBEI. The micro-hardness value in the fusion zone of the as-welded sample almost doubles from 2.75 ± 0.09 GPa to 5.06 ± 0.29 GPa due to a combination of residual stress and cooling-induced martensite. Conventional post weld heat treatment (PWHT) is shown to release ∼ 90% of the residual stress but not fully restore the microstructure. By comparing its hardness with that of stress-free samples, it is found that the microstructure is the primary contribution to the hardening. This study provides insight into the prediction of structural integrity for critical structural components of fusion reactors.

Triboelectric nanogenerators (TENG) are playing a vital role in generation of eco-friendly, cost effective power in self-powered form. Herein, a novel contact-separation mode based TENG is fabricated using waste biomaterial onion tunic (OT) as dielectric layer. Moreover, nanocomposite of OT with tin oxide SnOx (x = 1-2) (OT/SnOx composite), and tin oxide (SnO2) nanoparticles (NPs) are synthesized by chemical bath deposition (CBD) method, and used for making active dielectric layers for TENG. For comparative analysis, the biomaterials egg shell membrane (ESM), garlic tunic (GT), almond peel (ALM), bombax ceiba fibers (BOM), calotropis fibers (CALO) and highly electronegative inorganic material polytetrafluoroethylene (PTFE) have also been used as TENG dielectric layers. The synthesized materials are characterized by Fourier Transform Infrared spectroscopy (FTIR), X-Ray diffraction (XRD), Scanning Electron Microscopy (SEM) with Energy dispersive X-ray spectroscopy (EDX) and Thermogravimetric Analysis (TGA). The average particle size of SnO2 NPs and OT/SnOx is in the range of 17-24 nm and 50-60 nm, respectively. The highest output voltage of 19V is produced by TENG combination of SnO2 NPs-PTFE followed by OT/SnOx composite-PTFE (16.6V) and least voltage (10.7V) produced by BOM – PTFE as active dielectric TENG layers by manual tapping of 4-5 Hz. The extensive experimentation observation of single TENG output voltage peaks help in deciding the position in the triboseries of materials used in this study. This triboseries reflects that all biomaterials, NPs and OT/SnOx composite are highly electropositive in nature with respect to PTFE. The fabricated TENGs also tested to power tens of green Light emitting diodes (LEDs), small digital wrist watch and successfully produce range of voltages from mechanical energy of different human activities like walking, running, and jumping.

The plasma-facing components of future fusion reactors, where the Eurofer97 is the primary structural material, will be assembled by laser-welding techniques. The heterogeneous residual stress induced by welding can interact with the microstructure, resulting in a degradation of mechanical properties and a reduction in joint lifetime. Here, a Xe+ plasma focused ion beam with digital image correlation (PFIB-DIC) and nanoindentation is used to reveal the mechanistic connection between residual stress, microstructure, and microhardness. This study is the first to use the PFIB-DIC to evaluate the time-resolved multiscale residual stress at a length scale of tens of micrometers for laser-welded Eurofer97. A nonequilibrium microscale residual stress is observed, which contributes to the macroscale residual stress. The microhardness is similar for the fusion zone and heat-affected zone (HAZ), although the HAZ exhibits around ~30% tensile residual stress softening. The results provide insight into maintaining structural integrity for this critical engineering challenge.

Hot-forming Quenching (HFQ) can lead to significant changes in microstructure of high-strength aluminum alloys for car body sheet. Furthermore, through effective control, desired performance of the alloys can be achieved. Three designed processes, HFQ + Natural Aging (NA) + Simulate Baking (SB), HFQ + Pre-aging (PA) + SB and HFQ + Peak-aging (T6) were applied in this work, and the evolution of precipitated phases was systematically studied using High Resolution Transmission Electron Microscopy-Selected Area Electron Diffraction (HRTEM-SAED). The results revealed the precipitation nature of η phase in 7055 aluminum alloys is that GP zone I evolves into GP zone II, on which η’ phases directly nucleate and multiply, resulting in the transformation from η’ phases into η phases. By comparing the three processes, it is found that HFQ + PA + SB has high-density and finely distributed η’ phases, and grain boundary precipitates are small and discontinuously distributed. By adjusting the pre-aging temperature and time, it can provides a large amount of precipitation nucleation basis for the baking stage and ensure that η’ phase formation with high quantity density. The end product has a tensile strength of 660.1 MPa and a yield strength of 639.4 MPa, which is the most promising sheet material for future car body application.

Many natural materials demonstrate ideal design inspirations for the development of lightweight composite materials with excellent damage tolerance. One notable example is the layered architecture of nacre, which possesses toughness an order of magnitude higher than its constituent parts. Man-made nacre-like ceramic/polymer composites obtained through direct infiltration of polymer in ceramic scaffolds have been shown to produce improved mechanical properties over other composite architectures. Replacing the polymer phase with metal could provide higher damage tolerance but the infiltration of metal into complex ceramic scaffolds is difficult due to the surface tension of molten metal. To address this, bioinspired nacre-like micro-layered (µL) alumina scaffolds with different ceramic fractions from 18 to 85% were infiltrated with aluminium alloy 5083 via pressureless and squeeze casting infiltrations techniques. The scaffolds were created using a bi-directional freeze-casting and one-step densification method. As a result, the µL alumina/aluminium composites displayed significant extrinsic toughening mechanisms with both high strength and toughness. The mechanical performance was highly dependent on the interface, microstructure, and composition. The nacre-like composites with 18% alumina and AlN interface displayed a maximum resistance‐curve toughness up to around 70 MPa.m½ (35 MPa.m½ at the ASTM limit) and a flexural strength around 600 MPa.

Polylactide (PLA)-hydroxyapatite (HAp) composite components have attracted extensive attentions for a variety of biomedical applications. This study seeks to explore how the biocompatible PLA matrix and the bioactive HAp fillers respond to thermo-mechanical environment of a PLA-HAp composite manufactured by 3D printing using Fused Filament Fabrication (FFF). The insight is obtained by in situ synchrotron small- and wide- angle X-ray scattering (SAXS/WAXS) techniques. The thermo-mechanical cyclic loading tests (0-20MPa, 22-56°C) revealed strain softening (Mullins effect) of PLA-HAp composite at both room and elevated temperatures (50°C) due to the increased chain mobility. Above this temperature the deformation behaviour of the soft PLA lamella changes drastically. The thermal test (0-110°C) identified multiple crystallisation mechanisms of the PLA amorphous matrix, including reversible stress-induced large crystal formation at room temperature, reversible coupled stress-temperature-induced PLA crystal formation appearing at around 60°C, as well as irreversible heating-induced crystallisation above 92°C. The shape memory test (0-3.75MPa, 0-70°C) of the PLA-HAp composite demonstrates a fixing ratio (strain upon unloading/strain before unloading) of 65% and rather a ∼100% recovery ratio, showing an improved shape memory property. These findings provide a new framework for systematic characterisation of the thermo-mechanical response of composites, and open up ways towards improved material design and enhanced functionality for biomedical applications.

High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation.

The study area, Woshaxi landslide, is 400 m long and 700 m wide, with an average thickness of approximately 15 m and a volume of 4.2 × 106 m3. The Woshaxi landslide, which is located on the Qinggan River, a tributary of the Yangtze River in the Three Gorges reservoir area, is just 1.5 km from the Qianjiangping landslide. The Qianjiangping landslide following the Three Gorges reservoir impoundment was caused by the combined effects of rainfall and reservoir water-level fluctuation. In this study, the Woshaxi landslide’s deformation characteristics and mechanism are investigated based on deformation monitoring data and a geological survey during the initial impoundment period of the Three Gorges reservoir. Furthermore, based on the characteristics of the combined effects of reservoir water level fluctuation and rainfall in the Three Gorges reservoir area, the stability evolution behavior of the Woshaxi landslide during the initial impoundment period of the Three Gorges reservoir is investigated.

Peritubular dentine (PTD) and intertubular dentine (ITD) were investigated by 3D correlative Focused Ion Beam (FIB)-Scanning Electron Microscopy (SEM)-Energy Dispersive Spectroscopy (EDS) tomography, tapping mode Atomic Force Microscopy (AFM) and scattering-type Scanning Near-Field Optical Microscopy (s-SNOM) mapping. The brighter appearance of PTD in 3D SEM-Backscattered-Electron (BSE) imaging mode and the corresponding higher grey value indicate a greater mineral concentration in PTD (~160) compared to ITD (~152). However, the 3D FIB-SEM-EDS reconstruction and high resolution, quantitative 2D map of the Ca/P ratio (~1.8) fail to distinguish between PTD and ITD. This has been further confirmed using nanoscale 2D AFM map, which clearly visualised biopolymers and hydroxyapatite (HAp) crystallites with larger mean crystallite size in ITD (32 ± 8 nm) than that in PTD (22 ± 3 nm). Correlative microscopy reveals that the principal difference between PTD and ITD arises primarily from the nanoscale packing density of the crystallites bonded together by thin biopolymer, with moderate contribution from the chemical composition difference. The structural difference results in the mechanical properties variation that is described by the parabolic stiffness-volume fraction correlation function introduced here. The obtained results benefit a microstructure-based mechano-chemical model to simulate the chemical etching process that can occur in human dental caries and some of its treatments.

A cost-effective one-step densification process based on bi-directional freeze casting was investigated to produce nacre-like alumina/poly (methyl methacrylate) (PMMA) composites with a unique micro-layered (μL) architecture. This method has the advantage of shorter processing time, as it requires only sintering once instead of twice as in the fabrication of conventional brick-and-mortar (BM) composites via freeze casting. By tuning the processing parameters, composites with different ceramic content and layer thickness were obtained. The resultant mechanical properties of μL composites showed that ceramic content and wall thickness affected mechanical properties significantly. The μL composite with fine ceramic walls (8 μm) and relatively high ceramic fraction (72 vol%) exhibited an exceptional combination of high flexural strength (178 MPa) and fracture toughness (12.5 MPa m1/2). The μL composites were also compared with the conventional BM composites. Although the fracture behaviour of both composites exhibited similar extrinsic toughening mechanisms, the μL composites with longer ceramic walls displayed superior mechanical properties in terms of strength and fracture toughness in comparison with the BM composites comprising short ceramic walls (i.e. bricks), due to the effectiveness of stress transfer of load-bearing ceramic phase within the composites.

Dental caries is one of the most common chronic diseases that affect human teeth. It often initiates in enamel, undermining its mechanical function and structural integrity. Little is known about the enamel demineralisation process caused by dental caries in terms of the microstructural changes and crystallography of the inorganic mineral phase. To improve the understanding of the carious lesion formation process and to help identify efficient treatments, the evolution of the microstructure at the nano-scale in an artificially induced enamel erosion region was probed using advanced synchrotron small-angle and wide-angle X-ray scattering (SAXS and WAXS). This is the first in vitro and time-resolved investigation of enamel demineralisation using synchrotron X-ray techniques which allows in situ quantification of the microstructure evolution over time in a simulated carious lesion. The analysis revealed that alongside the reduction of mineral volume, a heterogeneous evolution of hydroxyapatite (HAp) crystallites (in terms of size, preferred orientation and degree of alignment) could be observed. It was also found that the rate and direction of dissolution depends on the crystallographic orientation. Based on these findings, a novel conceptual view of the process is put forward that describes the key structural parameters in establishing high fidelity ultrastructure-based numerical models for the simulation of the enamel demineralisation process.

Human dentine is a mineralised dental tissue that consists of dentinal tubules surrounded by two distinct dentinal phases: peritubular dentine (PTD) and intertubular dentine (ITD). Dental caries, which manifests itself as a consequence of demineralisation, is one of the most common chronic diseases that affect the function of human teeth. Due to the difference in the packing density of crystallites, PTD and ITD exhibit different reaction rates to acid dissolution. The present study evaluates how the effective Young’s modulus degrades and how the effective stress redistributes in demineralised human dentine as a result of incremental acid dissolution process. An analytical two-layer composite model is proposed and used for the effective Young’s modulus calculation. 3D numerical representative volume elements (RVEs) with different variations in PTD fraction and dentinal tubule density are established to evaluate effective stress redistribution and examine the critical factors that can affect the mechanical performance. The models are then applied on an actual dentine bulk sample. The results reveal how PTD serves as a protection to ITD thus highlight the important role that PTD plays for the structural integrity of dentine. The obtained insights are crucial for advancing the understanding of a variety of natural and therapeutic effects from the mechanical perspective, e.g. the mechanical performance assessment of human dentine subject to complex dynamic processes of de- and re-mineralisation that can occur in human dental caries and dental treatments. It will ultimately inspire the biomimetic design towards strengthening the dentine and dentine-like materials.

The design, operation, and performance of a laboratory-scale X-ray computed tomography arrangement that is capable of elevated-temperature deformation studies of superalloys to 800 °C and possibly beyond are reported. The system is optimized for acquisition of three-dimensional (3D) backprojection images recorded sequentially during tensile deformation at strain rates between 10−4 and 10−2 s−1, captured in situ. It is used to characterize the evolution of damage—for example, void formation and microcracking—in Nimonic 80A and Inconel 718 superalloys, which are studied as exemplar polycrystalline alloys with lesser and greater ductility, respectively. the results indicate that such damage can be resolved to within 30 to 50 μm. Collection of temporally and spatially resolved data for the damage evolution during deformation is proven. Hence, the processes leading to creep fracture initiation and final rupture can be quantified in a novel way.

Based on the incremental method of elastic-plastic mechanics and bilinear projection operators, by combining the strength reduction method with the φ-v inequality, this paper proposes a virtual element method strength reduction technique for slope stability analysis. The deformations of a homogeneous slope and heterogeneous slope are solved under different strength reduction factors, and the mesh dependency problem of the method is discussed. Numerical examples verify the correctness and effectiveness of the proposed method. The results demonstrate that due to the differences in the physical and mechanical properties of soil and rocks, stress becomes concentrated in the contact zone between soil and rocks, and thus, the plastic zone surrounds the rocks. Therefore, it is difficult to form regular connections in a plastic zone, such as a soil slope. This method can be used to analyse the stability of a stony soil slope and to study the effects of particle size, rock content, rock density, and rock spatial distribution on the mechanical behaviour of stony soil slopes.

Nickel superalloys play a pivotal role in enabling power-generation devices on land, sea, and in the air. They derive their strength from coherent cuboidal precipitates of the ordered γ’ phase that is different from the γ matrix in composition, structure and properties. In order to reveal the correlation between elemental distribution, dislocation glide and the plastic deformation of microand nano-sized volumes of a nickel superalloy, a combined in situ nanoindentation compression study was carried out with a scanning electron microscope (SEM) on micro- and nano-pillars fabricated by focused ion beam (FIB) milling of Ni-base superalloy CMSX4. The observed mechanical response (hardening followed by softening) was correlated with the progression of crystal slip that was revealed using FIB nano-tomography and energy-dispersive spectroscopy (EDS) elemental mapping. A hypothesis was put forward that the dependence of material strength on the size of the sample (micropillar diameter) is correlated with the characteristic dimension of the structural units (γ’ precipitates). By proposing two new dislocation-based models, the results were found to be described well by a new parameter-free Hall–Petch equation.

The distinct molecular architecture and thermomechanical properties of polyurethane block copolymers make them suitable for applications ranging from textile fibers to temperature sensors. In the present study, differential scanning calorimetry (DSC) analysis and macroscopic stress relaxation measurements are used to identify the key internal processes occurring in the temperature ranges between −10 °C and 0 °C and between 60 °C and 70 °C. The underlying physical phenomena are elucidated by the small-angle X-ray scattering (SAXS) and wide-angle X-ray scattering (WAXS) study of synchrotron beams, allowing the exploration of the structure-property relationships as a function of temperature. In situ multiscale deformation analysis under uniaxial cyclic thermomechanical loading reveals a significant anomaly in the strain evolution at the nanoscale (assessed via SAXS) in the range between −10 °C and 0 °C owing to the ‘melting’ of the soft matrix. Furthermore, WAXS measurement of crystal strain within the hard regions reveals significant compressive residual strains arising from unloading at ∼60 °C, which are associated with the dynamic shape memory effect in polyurethane at these temperatures.

Residual stresses play a crucial role in determining material properties and behaviour, in terms of structural integrity under monotonic and cyclic loading, and for functional performance, in terms of capacitance, conductivity, band gap, and other characteristics. The methods for experimental residual stress analysis at the macro- and micro-scales are well established, but residual stress evaluation at the nanoscale faces major challenges, e.g. the need for sample sectioning to prepare thin lamellae, by its very nature introducing major modifications to the quantity being evaluated. Residual stress analysis by micro-ring core Focused Ion Beam milling directly at sample surface offers lateral resolution better than 1 μm, and encodes information about residual stress depth variation. We report a new method for residual stress depth profiling at the resolution better than 50 nm by the application of a mathematically straightforward and robust approach based on the concept of eigenstrain. The results are validated by direct comparison with measurements by nano-focus synchrotron X-ray diffraction.