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International audience; Halide perovskites doped with magnetic impurities (such as the transition metals Mn2+, Co2+, Ni2+) are being explored for a wide range of applications beyond photovoltaics, such as spintronic devices, stable light-emitting diodes, single-photon emitters, and magneto-optical devices. However, despite several recent studies, there is no consensus on whether the doped magnetic ions will predominantly replace the octahedral B-site metal via substitution or reside at interstitial defect sites. Here, by performing correlated nanoscale X-ray microscopy, spatially and temporally resolved photoluminescence measurements, and magnetic force microscopy on the inorganic 2D perovskite Cs2PbI2Cl2, we show that doping Mn2+ into the structure results in a lattice expansion. The observed lattice expansion contrasts with the predicted contraction expected to arise from the B-site metal substitution, thus implying that Mn2+ does not replace the Pb2+ sites. Photoluminescence and electron paramagnetic resonance measurements confirm the presence of Mn2+ in the lattice, while correlated nano-XRD and X-ray fluorescence track the local strain and chemical composition. Density functional theory calculations predict that Mn2+ atoms reside at the interstitial sites between two octahedra in the triangle formed by one Cl– and two I– atoms, which results in a locally expanded structure. These measurements show the fate of the transition metal dopants, the local structure, and optical emission when they are doped at dilute concentrations into a wide band gap semiconductor.

Focused ion beam (FIB) techniques are commonly used to machine, analyse and image materials at the micro- and nanoscale. However, FIB modifies the integrity of the sample by creating defects that cause lattice distortions. Methods have been developed to reduce FIB-induced strain, however these protocols need to be evaluated for their effectiveness. Here we use non-destructive Bragg coherent X-ray diffraction imaging to study the in situ annealing of FIB-milled gold microcrystals. We simultaneously measure two non-collinear reflections for two different crystals during a single annealing cycle, demonstrating the ability to reliably track the location of multiple Bragg peaks during thermal annealing. The thermal lattice expansion of each crystal is used to calculate the local temperature. This is compared to thermocouple readings, which are shown to be substantially affected by thermal resistance. To evaluate the annealing process, we analyse each reflection by considering facet area evolution, cross-correlation maps of displacement field and binarised morphology, and average strain plots. The crystal's strain and morphology evolve with increasing temperature, which is likely to be caused by the diffusion of gallium in gold below ~280{\deg}C and the self-diffusion of gold above ~280{\deg}C. The majority of FIB-induced strains are removed by 380-410\degree C, depending on which reflection is being considered. Our observations highlight the importance of measuring multiple reflections to unambiguously interpret material behaviour., Comment: 51 pages, 16 figures

This paper presents the development of novel Carbon-Fibre Reinforced Polymer (CFRP) laminates, tailored for the application of Digital Volume Correlation (DVC) and Computed Tomography (CT) to experimental mechanics analyses of these materials. Analogous to surface-based Digital Image Correlation (DIC), DVC is a relatively novel volumetric method that utilizes CT data to quantify internal three-dimensional (3D) displacements and implicit strain fields. The highly anisotropic and somewhat regular/self-similar microstructures found in well-aligned unidirectional (UD) materials at high fibre volume fractions are intrinsically challenging for DVC, especially along the fibre direction at microstructural length-scales on the order of a few fibre diameters. To permit the application of DVC to displacement and/or strain measurements parallel to the fibre orientation, the matrix was doped with a sparse population of sub-micrometre particles to act as displacement trackers (i.e. fiducial markers). Barium titanate particles (400 nm, ∼1.44 vol. %) were found to offer the most favourable compromise between contrast in CT images and the ability to obtain a homogeneous distribution in 3D space with sufficient particle compactness for local DVC analyses. This property combination was selected following an extensive Micro-focus Computed Tomography (µCT)-based qualitative assessment on a wide test matrix, that included 38 materials manufactured with a range of possible particle compositions, mean sizes and concentrations. By comparing the tensile behaviour of the particle-adapted material alongside its particle-free counterpart, we demonstrate through the application of in situ Synchrotron Radiation Computed Tomography (SRCT) that the macro- and micromechanical responses of the newly developed CFRP are consistent with standard production materials indicating its suitability as a model system for mechanistic investigations. ispartof: Journal Of Composite Materials vol:55 issue:14 status: Published online

This paper presents an experimental demonstration and validation of high-resolution three-dimensional experimental strain measurement using Digital Volume Correlation (DVC) on Carbon Fibre-Reinforced Polymers, via through-thickness strain analysis under a state of pure bending. To permit the application of DVC to displacements and/or strain measurements parallel to the fibre direction in well-aligned unidirectional materials at high volume fractions, a methodology was developed for the insertion of sparse populations of 400 nm BaTiO3 particles within the matrix to act as displacement trackers (i.e. fiducial markers). For this novel material system, measurement sensitivity and noise are considered, along with the spatial filtering intrinsic to established DVC data processing. In conjunction with Micro-focus Computed Tomography, the technique was applied to a simple standard specimen subjected to a four-point flexural test, which resulted in a linear strain distribution through the beam thickness. The high-resolution, fibre-level strain distributions (imaged at a voxel resolution of ∼0.64 µm) were compared against the classical beam theory (Euler–Bernoulli) in incrementally decreasing averaging schemes and different sub-set sizes. Different sampling and averaging strategies are reported, showing that DVC outputs can be obtained that are in very good agreement with the analytical solution. A practical lower limit for the spatial resolution of strain is discerned for the present materials and methods. This study demonstrates the effectiveness of DVC in measuring local strains parallel to the fibre direction, with corresponding potential for calibration and validation of micromechanical models predicting various fibre-dominated damage mechanisms.

Solid-state welding offers distinct advantages for joining reactive materials, such as magnesium (Mg) and its alloys. This study investigates the effect of linear friction welding (LFW) on the microstructure and mechanical properties of cast AZ91 (Mg–9Al–1Zn) and AZ91–2Ca alloys, which (to the best knowledge of the authors) has not been reported in the literature. Using the same set of LFW process parameters, similar alloy joints—namely, AZ91/AZ91 and AZ91–2Ca/AZ91–2Ca—were manufactured and found to exhibit integral bonding at the interface without defects, such as porosity, inclusions, and/or cracking. Microstructural examination of the AZ91/AZ91 joint revealed dissolution of the Al-rich second phase in the weld zone, while the Mn containing phases remained and were refined. In the AZ91–2Ca/AZ91–2Ca joint, the weld zone retained Ca- and Mn-rich phases, which were also refined due to the LFW process. In both joint types, extensive recrystallization occurred during LFW, as evidenced by the refinement of the grains from ~1000 µm in the base materials to roughly 2–6 µm in the weld zone. These microstructural changes in the AZ91/AZ91 and AZ91–2Ca/AZ91–2Ca joints increased the hardness in the weld zone by 32%. The use of digital image correlation for strain mapping along the sample gage length during tensile testing revealed that the local strains were about 50% lower in the weld zone relative to the AZ91 and AZ91–2Ca base materials. This points to the higher strength of the weld zone in the AZ91/AZ91 and AZ91–2Ca/AZ91–2Ca joints due to the fine grain size, second phase refinement, and strong basal texture. Final fracture during tensile loading of both joints occurred in the base materials.

Terahertz metamaterials with strain-sensitive junctions are introduced to identify structurally compromised regions of composite materials. Spatially mapping the local polarimetric metamaterial response visualizes and records regions of stress extrema experienced by visibly opaque materials.

The measuring of internal stress has not only a great scientific aspect, but is particularly important for nondestructive description of component or products in industry. It is expected that exceeding of local mechanical limits in the material can have catastrophic consequences. In this paper is mapped the deformation field of amorphous material under the nanoindenter tip using diffraction in Debye-Scherrer geometry. Using the FEM analysis, it was modeled the deformation field in such material. There is a great match in between measured and calculated data. The result is pointing out on large limits of internal stresses measuring by conventional standard methods.

Interfaces have been reported to significantly strengthen and toughen metallic materials. However, there has been a long-standing question on whether interface-affected-zone (IAZ) exists, and how it might behave. Here we report in situ high-resolution strain mapping near interfaces in a copper–bronze heterogeneous laminate, which revealed the existence of IAZs. Defined as the zone with strain gradient, the IAZ was found to form by the dislocations emitted from the interface. The IAZ width remained largely constant with a magnitude of a few micrometers with increasing applied strain. Interfaces produced both back stress strengthening and work hardening, which led to both higher strength and higher ductility with decreasing interface spacing until adjacent IAZs started to overlap, after which a tradeoff between strength and ductility occurred, indicating the existence of an optimum interface spacing for the best mechanical properties. These findings are expected to help with designing laminates and other heterogeneous metals and alloys for superior mechanical properties.

Free-standing semiconductor nanowires constitute an ideal material system for the direct manipulation of electrical and optical properties by strain engineering. In this study, we present a direct quantitative correlation between electrical conductivity and nanoscale lattice strain of individual InAs nanowires passivated with a thin epitaxial In0.6Ga0.4As shell. With an in situ electron microscopy electromechanical testing technique, we show that the piezoresistive response of the nanowires is greatly enhanced compared to bulk InAs, and that uniaxial elastic strain leads to increased conductivity, which can be explained by a strain-induced reduction in the band gap. In addition, we observe inhomogeneity in strain distribution, which could have a reverse effect on the conductivity by increasing the scattering of charge carriers. These results provide a direct correlation of nanoscale mechanical strain and electrical transport properties in free-standing nanostructures.

Nanobeam electron diffraction strain mapping has been used to measure the strain evolution in stainless steel under in situ deformation. As the amount of deformation increases, the leading dislocation of a planar slip band leaves behind a residual strain in the form of a small lattice expansion. Dislocation analysis confirmed that the dislocations involved were type. While the characteristic residual strain of planar slip has often been observed, it has never before been directly measured. Our results provide a view into the dynamic mechanisms of planar slip, and showcase the possibilities of multidimensional in situ imaging.

We proposed a method for mapping full-field shearing strain distributions in x and y direction. Displacements and strain maps of living osteocytes can be estimated from phase maps recorded by a digital holographic microscopy.

The ongoing trend toward miniaturization has led to an increased interest in the magnetoelectric effect, which could yield entirely new device concepts, such as electric field-controlled magnetic data storage. As a result, much work is being devoted to developing new robust room temperature (RT) multiferroic materials that combine ferromagnetism and ferroelectricity. However, the development of new multiferroic devices has proved unexpectedly challenging. Thus, a better understanding of the properties of multiferroic thin films and the relation with their microstructure is required to help drive multiferroic devices toward technological application. This review covers in a concise manneradvancedanalytical imaging methods based on (scanning) transmission electron microscopy which can potentially be used to characterize complex multiferroic materials. It consists of a first broad introduction to the topic followed by a section describing the so-called phase-contrast methods, which can be used to map the polar and magnetic order in magnetoelectric multiferroics at different spatial length scales down to atomic resolution. Section 3 is devoted to electron nanodiffraction methods. These methods allow measuring local strains, identifying crystal defects and determining crystal structures, and thus offer important possibilities for the detailed structural characterization of multiferroics in the ultrathin regime or inserted in multilayers or superlattice architectures. Thereafter, in Section 4, methods are discussed which allow for analyzing local strain, whereas in Section 5 methods are addressed which allow for measuring local polarization effects on a length scale of individual unit cells. Here, it is shown that the ferroelectric polarization can be indirectly determined from the atomic displacements measured in atomic resolution images. Finally, a brief outlook is given on newly established methods to probe the behavior of ferroelectric and magnetic domains and nanostructures during in situ heating/electrical biasing experiments. These in situ methods are just about at the launch of becoming increasingly popular, particularly in the field of magnetoelectric multiferroics, and shall contribute significantly to understanding the relationship between the domain dynamics of multiferroics and the specific microstructure of the films providing important guidance to design new devices and to predict and mitigate failures.

Nanoscale strain mapping by four-dimensional scanning transmission electron microscopy (4D-STEM) relies on determining the precise locations of Bragg-scattered electrons in a sequence of diffraction patterns, a task which is complicated by dynamical scattering, inelastic scattering, and shot noise. These features hinder accurate automated computational detection and position measurement of the diffracted disks, limiting the precision of measurements of local deformation. Here, we investigate the use of patterned probes to improve the precision of strain mapping. We imprint a "bullseye" pattern onto the probe, by using a binary mask in the probe-forming aperture, to improve the robustness of the peak finding algorithm to intensity modulations inside the diffracted disks. We show that this imprinting leads to substantially improved strain-mapping precision at the expense of a slight decrease in spatial resolution. In experiments on an unstrained silicon reference sample, we observe an improvement in strain measurement precision from 2.7% of the reciprocal lattice vectors with standard probes to 0.3% using bullseye probes for a thin sample, and an improvement from 4.7% to 0.8% for a thick sample. We also use multislice simulations to explore how sample thickness and electron dose limit the attainable accuracy and precision for 4D-STEM strain measurements., 29 pages, 7 figures; revision 1

International audience; This paper reports the fabrication of arrays of vertical piezoelectric nanowires which are individually contacted at their base, and demonstrates that an electrical response to strain can be obtained from individual nanowires from the array, without external biasing exploiting the piezotronic effect. Such a technology could thus be used for the fabrication of self-powered sensors for mechanical strain mapping, where each individually contacted nanowire would act as the strain sensing equivalent of a pixel. Lateral mapping resolutions in the micrometer range can be obtained. Here, the hydrothermal method was used to grow vertical ZnO nanowires selectively between two electrodes that had been patterned beforehand. For the sake of demonstration, nanowires deflection was produced by subjecting the array of nanowires to an incident lateral gas flow of controlled rate, which was switched on and off repeatedly across the sample while electrical response was measured. Different experimental configurations were tested in terms of flow rate, flow orientation, or nanowire position with respect to tube outlet. Experiments were carried out with compressed nitrogen and air. The experimental results are fully consistent with the piezoelectric and piezotronic response which can be expected with this geometry. Moreover, it is shown that the electrical response under nitrogen flow is a linear function of flow rate and that its sign provides information about flow direction. These results demonstrate the very promising prospects of this new technology for high-resolution mapping, with potential applications in gas or liquid flow sensing, fingerprints detection or human-machine interfaces.

This manuscript describes the effects of alterations in biochemical composition on structural morphology and the mechanical behaviour of technical fibres of hemp used for composite applications. First, the strength and apparent Young’s modulus distribution of technical fibres of hemp of 96 hemp samples, corresponding to 32 different hemp accessions cultivated in 3 locations, were analysed using Weibull distribution. From these, 2 samples (one with high and one with low fibre strength) were selected for further analysis. Next, full-field strain measurement at the micro-scale during tensile loading via digital image correlation analysis was used for evaluating both, the stress-strain behaviour at a global scale and the local mechanical behaviour heterogeneity at a micro-scale, along a technical fibre of hemp. The analysis reveals 2 typical types of tensile stress-strain curves, and a complex and very irregular pattern of strain concentrations, which are associated to the technical fibre strength. The non-linear behaviour of the stress-strain curve is explained by the development of shear strain at the elementary fibre (botanically defined as the individual cell) interphases. Micro tomography and biochemical analysis of the technical fibre microstructure showed that alterations in cell wall composition, in particular substitution of pectin, leads to changes in the non-linear behaviour of technical fibres of hemp under tensile loading.

For the determination of the shear properties such as strength, strain and modulus of unidirectionally reinforced composites, nearly a dozen measurement techniques exist, several of which have found their way into standards. One non-standardized method for sheet materials is the 10° off-axis tensile test of unidirectional coupons. The current work focuses on the experimental investigation of tensile testing of CFRP-UD coupon specimens using the 10° off-axis test and DIC strain mapping to measure the full-field deformation response. A sensitivity analysis on the measured stresses, strains and moduli is performed by varying the aspect ratio of the specimens and the location of strain measurement. Test related uncertainties such as the loading angle and specimen preparation details are investigated and quantified with the help of these full-field DIC measurements.

Directed energy deposition (DED) of two high-carbon high speed steel alloys Febal-C-Cr-Mo-V and Febal−x-C-Cr-Mo-V-Wx was performed by using a 4 kW Nd:YAG laser source. The purpose of additive manufacturing was design and evaluation of thermally stable - high temperature wear resistant alloys. High temperature (500 °C) pin-on-disc tests were conducted to investigate the effect of carbides phase fraction on friction and wear. Strain scanning of the powder and additively manufactured materials was carried out by Neutron diffraction. Microstructures of both alloys consisted of a martensitic matrix with networks of primary and eutectic carbides. Micro-hardness (0.5 HV) measurement of all multilayer laser deposits, showed a micro-hardness greater than 700 HV, with no detrimental effect of repetitive laser thermal cycling. Febal−x-C-Cr-Mo-V-Wx showed a better high temperature wear resistance due to greater phase fraction of VC and Mo2C carbides. Fracture surfaces of post-heat treated tensile samples of Febal-C-Cr-Mo-V and Febal−x-C-Cr-Mo-V-Wx revealed brittle failures with minimal plasticity. Neutron strain mapping of the metal powders and the additively manufactured materials resulted in a weak diffraction signal and peak widening effect. These results could be explained either by an effect of strong crystallographic texture in the bulk or by the presence of nano- or semi-crystalline phases.

The analysis by diffraction of polycrystalline materials can determine the full tensor of the elastic strains within them. Point-by-point maps of elastic strain can thus be obtained in fine-grained engineering alloys, typically using synchrotron X-rays or neutrons. In this paper, a novel approach is presented to calculate the elastic strain energy release rate of a loaded crack from two-dimensional strain maps that are obtained by diffraction. The method is based on a Finite Element approach, which uses diffraction data to obtain the parameters required to calculate the J-integral via the contour integral method. The J integral is robust to uncertainties in the crack tip position and to poor definition of the field in the crack vicinity, and does not rely on theoretical assumptions of the field shape. A validation of the technique is presented using a synthetic dataset from a finite element model. Its experimental application is demonstrated in an analysis of a synchrotron X-ray diffraction strain map for a loaded fatigue crack in a bainitic steel.

International audience; Precession electron diffraction has been used to provide accurate deformation maps of a device structure showing that this technique can provide a spatial resolution of better than 2 nm and a precision of better than 0.02%. The deformation maps have been fitted to simulations that account for thin specimen relaxation. By combining the experimental deformation maps and simulations, we have been able to separate the effects of the stressor and recessed sources and drains and show that the Si3N4 stressor increases the in-plane deformation in the silicon channel from 0.92 to 1.52 +/- 0.02%. In addition, the stress in the deposited Si3N4 film has been calculated from the simulations, which is an important parameter for device design.

We determined inhomogeneity of strains around discontinuities as well as changes in orientation of collagen fibrils under applied load in skin. Second Harmonic Generation (SHG) images of collagen fibrils were obtained at different strain magnitudes. Changes in collagen orientation were analyzed using Fast Fourier Transforms (FFT) while strain inhomogeneity was determined at different distances from hair follicles using Digital Image Correlation (DIC). A parameter, defined as the Collagen Orientation Index (COI), is introduced that accounts for the increasingly ellipsoidal nature of the FFT amplitude images upon loading. We show that the COI demonstrates two distinct mechanical regimes, one at low strains (0%, 2.5%, 5% strain) in which randomly oriented collagen fibrils align in the direction of applied deformation. In the second regime, beginning at 5% strain, collagen fibrils elongate in response to applied deformation. Furthermore, the COI is also found to be linearly correlated with the applied stress indicating that collagen fibrils orient to take the applied load. DIC results indicated that major principal strains were found to increase with increased load at all locations. In contrast, minimum principal strain was dependent on distance from hair follicles. These findings are significant because global and local changes in collagen deformations are expected to be changed by disease, and could affect stem cell populations surrounding hair follicles, including mesenchymal stem cells within the outer root sheath.

Nanowires are a versatile platform to investigate and harness phonon and thermal transport phenomena in nanoscale systems. With this perspective, we demonstrate herein the use of crystal phase and mass disorder as effective degrees of freedom to manipulate the behavior of phonons and control the flow of local heat in silicon nanowires. The investigated nanowires consist of isotopically pure and isotopically mixed nanowires bearing either a pure diamond cubic or a cubic-rhombohedral polytypic crystal phase. The nanowires with tailor-made isotopic compositions were grown using isotopically enriched silane precursors 28SiH4, 29SiH4, and 30SiH4 with purities better than 99.9%. The analysis of polytypic nanowires revealed ordered and modulated inclusions of lamellar rhombohedral silicon phases toward the center in otherwise diamond-cubic lattice with negligible interphase biaxial strain. Raman nanothermometry was employed to investigate the rate at which the local temperature of single suspended nanowires evolves in response to locally generated heat. Our analysis shows that the lattice thermal conductivity in nanowires can be tuned over a broad range by combining the effects of isotope disorder and the nature and degree of polytypism on phonon scattering. We found that the thermal conductivity can be reduced by up to ∼40% relative to that of isotopically pure nanowires, with the lowest value being recorded for the rhombohedral phase in isotopically mixed 28Six30Si1–x nanowires with composition close to the highest mass disorder (x ∼ 0.5). These results shed new light on the fundamentals of nanoscale thermal transport and lay the groundwork to design innovative phononic devices., O.M. acknowledges support from NSERC-Canada (Discovery Grants and Strategic Partnership Grants), the Canada Foundation for Innovation, MRIF Québec (Coopération Québec-Catalogne), Mitacs, and Canada Research Chair. J.A. acknowledges funding from Generalitat de Catalunya 2014 SGR 1638 and the Spanish MINECO coordinated projects VALPEC and ANAPHASE (ENE2017-85087-C3-3-R). ICN2 acknowledges support from the Severo Ochoa Programme (MINECO, Grant No. SEV-2013-0295) and is funded by the CERCA Programme/Generalitat de Catalunya.

This paper focuses on local strain distribution in the microstructure of high silicon ductile iron during cyclic loading. In-situ cyclic test was performed on compact-tension (CT) samples inside the scanning electron microscope (SEM) to record the whole deformation and obtain micrographs for microstructural strain measurement by means of digital image correlation (DIC) technique. Focused ion beam (FIB) milling was used to generate speckle patterns necessary for DIC measurement. The equivalent Von Mises strain distribution was measured in the microstructure at the maximum applied load. The results revealed a heterogeneous strain distribution at the microstructural level with higher strain gradients close to the notch of the CT sample and accumulated strain bands between graphite particles. Local strain ahead of the early initiated micro-cracks was quantitatively measured, showing high strain localization, which decreased by moving away from the micro-crack tip. It could be observed that the peak of strain in the field of view was not necessarily located ahead of the micro-cracks tip which could be because of the (i) strain relaxation due to the presence of other micro-cracks and/or (ii) presence of subsurface microstructural features such as graphite particles that influenced the strain concentration on the surface. The RightsLink Digital Licensing and Rights Management Service (including RightsLink for Open Access) is available (A) to users of copyrighted works found at the websites of participating publishers who are seeking permissions or licenses to use those works, and (B) to authors of articles and other manuscripts who are seeking to pay author publication charges in connection with the submission of their works to publishers.

Measuring elastic strain with nanoscale resolution has historically been very difficult and required a marriage of simulations and experiments. Nano precession electron diffraction provides excellent strain and spatial resolution but has traditionally only been applied to single-crystalline semiconductors. The present study illustrates that the technique can also be applied to polycrystalline materials. The strain resolution was determined to be 0.15% and 0.10% for polycrystalline copper and boron carbide, respectively. Local strain maps were obtained near grain boundaries in boron carbide and dislocations in magnesium and shown to correlate with expected values, thus demonstrating the efficacy of this technique. This study demonstrates that nano precession electron diffraction can be extended from semiconductor devices to polycrystalline metals and ceramics to map nanoscale elastic strain fields with high strain resolution.

Strain analysis from high-resolution transmission electron microscopy (HRTEM) images offers a convenient tool for measuring strain in materials at the atomic scale. In this paper we present a theoretical study of the precision and accuracy of surface strain measurements directly from aberration-corrected HRTEM images. We examine the influence of defocus, crystal tilt and noise, and find that absolute errors of at least 1–2% strain should be expected. The model structures include surface relaxations determined using molecular dynamics, and we show that this is important for correctly evaluating the errors introduced by image aberrations. Electronic supplementary material The online version of this article (doi:10.1186/s40679-017-0047-0) contains supplementary material, which is available to authorized users.

Scanning transmission electron microscopy (STEM) data with atomic resolution can contain a large amount of information about the structure of a crystalline material. Often, this information is hard to extract, due to the large number of atomic columns and large differences in intensity from sublattices consisting of different elements. In this work, we present a free and open source software tool for analysing both the position and shapes of atomic columns in STEM-images, using 2-D elliptical Gaussian distributions. The software is tested on variants of the perovskite oxide structure. By first fitting the most intense atomic columns and then subtracting them, information on all the projected sublattices can be obtained. From this, we can extract changes in the lattice parameters and shape of A-cation columns from annular dark field images of perovskite oxide heterostructures. Using annular bright field images, shifts in oxygen column positions are also quantified in the same heterostructure. The precision of determining the position of atomic columns is compared between STEM data acquired using standard acquisition, and STEM-images obtained as an image stack averaged after using non-rigid registration. © The Author(s) 2017. This article is distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made.

Micropatterns are generated on a vast selection of polymeric substrates for various applications ranging from stretchable electronics to cellular mechanobiological systems. When these patterned substrates are exposed to external loading, strain field is primarily affected by the presence of microfabricated structures and similarly by fabrication-related defects. The capturing of such nonhomogeneous strain fields is of utmost importance in cases where study of the mechanical behavior with a high spatial resolution is necessary. Image-based non-contact strain measurement techniques are favorable and have recently been extended to scanning tunneling microscope and scanning electron microscope images for the characterization of mechanical properties of metallic materials, e.g. steel and aluminum, at the microscale. A similar real-time analysis of strain heterogeneity in elastomers is yet to be achieved during the entire loading sequence. The available measurement methods for polymeric materials mostly depend on cross-head displacement or precalibrated strain values. Thus, they suffer either from the lack of any real-time analysis, spatiotemporal distribution or high resolution in addition to a combination of these factors. In this work, these challenges are addressed by integrating a tensile stretcher with an inverted optical microscope and developing a subpixel particle tracking algorithm. As a proof of concept, the patterns with a critical dimension of 200 mu m are generated on polydimethylsiloxane substrates and strain distribution in the vicinity of the patterns is captured with a high spatiotemporal resolution. In the field of strain measurement, there is always a tradeoff between minimum measurable strain value and spatial resolution. Current noncontact techniques on elastomers can deliver a strain resolution of 0.001% over a minimum length of 5 cm. More importantly, inhomogeneities within this quite large region cannot be captured. The proposed technique can overcome this challenge and provides a displacement measurement resolution of 116 nm and a strain resolution of 0.04% over a gage length of 300 mu m. Similarly, the ability to capture inhomogeneities is demonstrated by mapping strain around a thru-hole. The robustness of the technique is also evaluated, where no appreciable change in strain measurement is observed despite the significant variations imposed on the measurement mesh. The proposed approach introduces critical improvements for the determination of displacement and strain gradients in elastomers regarding the real-time nature of strain mapping with a microscale spatial resolution.

In this paper we present a new approach using highly surface sensitive X-ray diffraction methods for archaeometrical investigation highlighted on the Neolithic Axe of Ahneby. Applying the sin 2 Ψ-method with a scintillation detector and a MAXIM camera setup, both were usually applied for material strain analysis on modern metal fabrics. We can distinguish between different production states of bronze axes: cast, forged and tempered. The method can be applied as a local probe of some 100th of μm 2 or integrative on a square centimeter surface area. We applied established synchrotron radiation based methods of material strain mapping and diffraction on a Neolithic bronze axe as well as replicated material for noninvasive analysis. The main goal of the described investigations was to identify the effects upon the bronze objects of post-cast surface treatment with stone tools and of heat treatment.

Recent advances in X-ray microtomography have created the opportunity to image the interior of materials. Microstructural images that are similar to or about an order of magnitude higher in resolution than those currently obtained with light microscopy can now be obtained in three-dimensions using synchrotron radiation. Local strain mapping is readily enabled by processing these high-resolution tomographic images using either the microstructural tracking technique or the digital volume correlation technique. This article is a review of the methodology behind these techniques and discusses recent experimental research on three-dimensional (3D) strain mapping. Potential future research directions are also outlined.

cited By 6; International audience; Strain mapping is an active area of research in transmission electron microscopy. Here we introduce a dark-field electron holographic technique that shares several aspects in common with both off-axis and in-line holography. Two incident and convergent plane waves are produced in front of the specimen thanks to an electrostatic biprism in the condenser system of a transmission electron microscope. The interference of electron beams diffracted by the illuminated crystal is then recorded in a defocused plane. The differential phase recovered from the hologram is directly proportional to the strain in the sample. The strain can be quantified if the separation of the images due to the defocus is precisely determined. The present technique has the advantage that the derivative of the phase is measured directly which allows us to avoid numerical differentiation. The distribution of the noise in the reconstructed strain maps is isotropic and more homogeneous. This technique was used to investigate different samples: a Si/SiGe superlattice, transistors with SiGe source/drain and epitaxial PZT thin films. © 2015 Elsevier B.V.

Crack Initiation and Propagation During Thermal-Mechanical Fatigue on IN792: Effects of Dwell Time

International audience; The last few years have seen a great deal of progress in the development of transmission electron microscopy based techniques for strain mapping. New techniques have appeared such as dark field electron holography and nanobeam diffraction and better known ones such as geometrical phase analysis have been improved by using aberration corrected ultra-stable modern electron microscopes. In this paper we apply dark field electron holography, the geometrical phase analysis of high angle annular dark field scanning transmission electron microscopy images, nanobeam diffraction and precession diffraction, all performed at the state-of-the-art to five different types of semiconductor samples. These include a simple calibration structure comprising 10-nm-thick SiGe layers to benchmark the techniques. A SiGe recessed source and drain device has been examined in order to test their capabilities on 2D structures. Devices that have.been strained using a nitride stressor have been examined to test the sensitivity of the different techniques when applied to systems containing low values of deformation. To test the techniques on modern semiconductors, an electrically tested device grown on a SOI wafer has been examined. Finally a GaN/AlN superlattice was tested in order to assess the different methods of measuring deformation on specimens that do not have a perfect crystalline structure. The different deformation mapping techniques have been compared to one another and the strengths and weaknesses of each are discussed. (C) 2015 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

International audience; Laue micro-diffraction and simultaneous rainbow-filtered micro-diffraction were used to measure accurately the full strain tensor and the lattice orientation distribution at the sub-micrometre scale in highly strained, suspended Ge micro-devices. A numerical approach to obtain the full strain tensor from the deviatoric strain measurement alone is also demonstrated and used for faster full strain mapping. The measurements were performed in a series of micro-devices under either uniaxial or biaxial stress and an excellent agreement with numerical simulations was found. This shows the superior potential of Laue micro-diffraction for the investigation of highly strained micro-devices.

Super-resolution (SR) software-based techniques aim at generating a final image by combining several noisy frames with lower resolution from the same scene. A comparative study on high-resolution high-angle annular dark field images of InAs/GaAs QDs has been carried out in order to evaluate the performance of the SR technique. The obtained SR images present enhanced resolution and higher signal-to-noise (SNR) ratio and sharpness regarding the experimental images. In addition, SR is also applied in the field of strain analysis using digital image processing applications such as geometrical phase analysis and peak pairs analysis. The precision of the strain mappings can be improved when SR methodologies are applied to experimental images.

Unfortunately, after publication of this article [1], it was noticed that the name of the fifth author was incorrectly displayed as Jakob Schiøz. The correct name is Jakob Schiøtz and can be seen in the corrected author list above. The original article has also been updated to correct this error.

Majorana zero modes (MZMs), prime candidates for topological quantum bits, are detected as zero bias conductance peaks (ZBPs) in tunneling spectroscopy measurements. Implementation of a narrow and high tunnel barrier in the next generation of Majorana devices can help to achieve the theoretically predicted quantized height of the ZBP. We propose a material-oriented approach to engineer a sharp and narrow tunnel barrier by synthesizing a thin axial segment of GaxIn1-xSb within an InSb nanowire. By varying the precursor molar fraction and the growth time, we accurately control the composition and the length of the barriers. The height and the width of the GaxIn1-xSb tunnel barrier are extracted from the Wentzel-Kramers-Brillouin (WKB)-fits to the experimental I-V traces., Comment: See doi: 10.5281/zenodo.5064400 for source data. No changes in this version compared to the previous version

Core-shell ${\text{Ge-Si}}_{x}$${\text{Ge}}_{1\ensuremath{-}x}$ nanowires (NWs) are expected to contain large strain fields due to the lattice mismatch at the core-shell interface. Here we report the measurement of core strain in a NW heterostructure using Raman spectroscopy. We compare the Raman spectra, and the frequency of the Ge-Ge mode measured in individual ${\text{Ge-Si}}_{0.5}$${\text{Ge}}_{0.5}$ core-shells, and bare Ge NWs. We find that the Ge-Ge mode frequency is diameter independent in Ge NWs with a value similar to that of bulk Ge, 300.5 ${\text{cm}}^{\ensuremath{-}1}$. On the other hand, ${\text{Ge-Si}}_{0.5}$${\text{Ge}}_{0.5}$ core-shell nanowires reveal a strain-induced blue shift of the Ge-Ge mode, dependent on the relative core and shell thicknesses. Using lattice dynamical theory we determine the strain in the Ge core and show that the results are in good agreement with values calculated using a continuum elasticity model.

ontributions that were presented at the sixth Size and Strain conference held in Presqu'ile de Giens, France, from 17 to 20 October, 2011. The Size-Strain conference is devoted to the analysis of the microstructure of materials by diffraction. Diffraction (X-rays, neutrons) was recognized very early as a very sensitive tool for analyzing deviations from perfect periodicity in crystals. Indeed, point, line, or planar defects yield distinct signatures in diffraction patterns. In the same way, displacement fields and surfaces induce characteristic features in diffracted intensities. In the field of powder diffraction, Line Profile Analysis (LPA) is an important method to extract microstructural information (size, strain, stacking fault, or dislocation density, etc.) from diffraction lines. More recently, the advent of nanobeams on 3rd generation synchrotrons has opened theway to very local investigations, which go beyond the statistical information given by LPA and bring new insights into the models used for LPA. Coherent X-ray diffraction is also a very promising method, which in the near future should allow strain mapping at the nanoscale. Size-Strain VI is the sixth conference in a series. The previous conferences were held in the following places: 1995 Liptovsky Mikulas (Slovakia), 1998 Freiberg (Germany), 2001 Trento (Italy), 2004 Prague (Czech Republic), and 2007 Garmisch-Partenkirchen (Germany). In close relation to the previous Size-Strain conferences, SS-VI focuses on methodologies for the study of lattice defects, residual stress, and texture in thin films, surfaces, and nanostructures, line-broadening analysis, line-profile fitting, and modeling based on fundamental parameters for applications in materials science problems. Newdevelopments for localmeasurements such asmicrobeam diffraction or coherent diffraction are also of special interest. During the summer of 2011,we received the sad news that Professor Robert Snyder passed away. Bob was a member of our scientific committee and a pioneer of this conference. A special tribute was dedicated to him and his career during the conference. Size-Strain VI gathered 102 attendees from 15 different countries. Sunny weather, a lively atmosphere, and a very good scientific program made this conference a very pleasant experience. Finally, the organizing committee has been instrumental in making things work. We really would like to warmly thank Cathy Paitel, Vanessa Coulet, Stephanie Escoubas, Sophie Girardin, and Stephane Labat for their dedication.Without them, the conference would certainly not have been such a great success.

Lattice images as obtained by high-resolution electron microscopy are used to quantify strain and strain profiles in semiconductor layer structures. Inherent parts of the analysis are the definition of spatial resolution and detection limit on the basis of a quantification of noise. As an application the tetragonal strain in pseudomorphic InxAl1–xAs heterostructures is analyzed. The detection limit is 2.8% strain at a spatial resolution of 0.4 × 0.4 nm2 using a 2σ-criterion. If resolution along the heterostructure is reduced by averaging, even 0.2% strain can be detected at a spatial resolution of 0.4 × 35 nm2. Mit hochauflosender Transmissionselektronenmikroskopie erzeugte Gitterabbildungen werden benutzt, um in Halbleiterschichtstrukturen Gitterverzerrungen und Verzerrungsprofile zu quantifieren. Zu dem Verfahren gehort die Definition der Ortsauflosung und der Nachweisgrenze basierend auf der Quantifizierung des Rauschens. Als Anwendung wird die tetragonale Verzerrung in einer pseudomorphen InxAl1–xAs-Heterostruktur ausgewertet. Hier ist die Nachweisgrenze 2,8% Verzerrung bei einer Ortsauflosung von 0,4 × 0,4 nm2, wenn das 2σ-Kriterium benutzt wird. Bei einer Reduktion der Ortsauflosung durch Mittelung langs der Heterostruktur ist es sogar moglich, eine Verzerrung von 0,2% bei einer Ortsauflosung von 0,4 × 35 nm2 nachzuweisen.

Abstract Micromechanical testing techniques can reveal a variety of characteristics in materials that are otherwise impossible to address. However, unlike to macroscopic testing, these miniaturized experiments are more challenging to realize and analyze, as loading and boundary conditions can often not be controlled to the same extent as in standardized macroscopic tests. Hence, exploiting all possible information from such an experiment seems utmost desirable. In the present work, we utilize dynamic in situ microtensile testing of a nanocrystalline equiatomic CoCrFeMnNi high entropy alloy in conjunction with initial feature tracking to obtain a continuous two-dimensional strain field. This enables an evaluation of true stress–strain data as well as of the Poisson’s ratio and allows to study localization of plastic deformation for the specimen. We demonstrate that the presented image correlation method allows for an additional gain of information in these sophisticated experiments over commercial tools and can serve as a starting point to study deformation states exhibiting more complex strain fields. Graphic abstract

Laser powder bed fusion is an efficient technique for additive manufacturing of metallic materials. The quality of the material produced depends on the optimization of a large range of build parameters and the complex thermo-mechanical build process is prone to inducing detrimental material features such as porosity and residual stresses negatively affecting fatigue resistance and lifetime. Here we apply neutron Bragg edge radiography in a parametric study on printing 316L steel. The parameters concerned are the laser scanning speed and strategy as well as the optional use of support structures. Analyses of the full field single shot wavelength-resolved Bragg edge radiography data enables to characterize local density inhomogeneities, as well as cracks, based on the long wavelength tail of the spectrum and variations of the stress field but also textural features based on the Bragg edge pattern. It is found that in the performed study not only respective differences in the residual stresses due to parameter variation are manifesting but also systematic irregularities due to machine imperfections (e.g. issues with the powder coater) are observed in the printed samples. The study supports the use of the parallel scanning strategy without supports and with the lower utilized scanning speed.

It is widely stated that yield stress extraction from micro-compression testing can be unreliable due to factors such as the pillar taper, pillar-punch misalignment and lateral displacement for example through discrete slip events. This study reports on how these factors can be eradicated when using digital image correlation based strain mapping. This approach is demonstrated through a conventional micropillar compression experiment using the hexagonal MAX phase system Cr2AlC. The use of this approach enables the uncertainty of the extracted yield stress values to be significantly reduced and effectively increases the precision of critical resolved shear stress extraction for basal plane slip from ±52% to ±4% of the mean value. The findings suggest that the statistical variations commonly observed in micro-compression tests may frequently be linked to systematic errors in the stress measurements taken, and that precise evaluation of deformation statistics can only be facilitated if the pillar deformation morphology is closely monitored.

A considerable amount of information can be gained from combined collection of both digital image correlation (DIC) measurements, and of electron backscattered diffraction (EBSD) data from the same area during in-situ deformation experiments. Such data collection remains a challenge, however, due the influence of the surface markers required for DIC on the EBSD data quality. In this work we demonstrate that by careful control of the sample preparation process, a two-step electropolishing method can be used to generate excellent surface markers for DIC where the markers are integral features on the surface. The method does not require any special equipment and can be used to collect high quality EBSD data and DIC data with sub-micron resolution on the same area during repeated loading as part of in-situ deformation experiments. Combined EBSD and DIC measurements are illustrated in this work for samples of Al deformed in tension to a strain of 10%. Due to the integral nature of the surface markers we demonstrate also that it is possible to perform DIC measurements up to large plastic strains, including the necked region within a tensile sample. A comparison of EBSD and DIC data collected from the same area of a tensile-deformed sample shows that although the EBSD data provide excellent information on the lattice rotations developed during deformation, these data cannot be directly used as a measure of local plastic strain on the scale of the deformation microstructure. The ability to collect both EBSD and DIC data during an in-situ experiment provides, therefore, an opportunity to explore further the complex relationship between local plastic strain heterogeneity and EBSD-based measures of crystal lattice rotation.