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In this study, we present a methodology to predict the macroscopic yield surface of metals and metallic alloys with general crystallographic textures. In previous work, we have established the use of partially input convex neural networks (pICNN) as macroscopic yield functions of crystal plasticity simulations. However, this work was performed with an over-abundance of data, and on limited crystallographic textures. Here, we extend this study to approach more realistic material states (i.e., complex crystallographic textures), and consider data-availability as a major driver for our approach. We present our modified framework capable of handling generalized material states and demonstrate its effectiveness on samples with multi-modal textures deformed under plane stress conditions. We further describe an adaptive algorithm for the generation of training data as informed by the shape of yield surfaces to reduce the time for both the generation of training data as well as pICNN training. Finally, we will discuss errors in both training and test datasets, limitations, and future extensibility., Comment: 29 pages, 16 figures

Understanding the nucleation and growth of polycrystalline thin films is a long-standing goal. Polycrystalline films have many grains with different orientations that affect thin-film properties. Numerous studies have been done to determine these grain size and their preferred crystallographic orientation as well as stress in films. However most past studies have either employed an ex-situ methodology or only monitor the development of macroscopic stress in real-time. There has never been any research done on the simultaneous determination of crystallographic texture, grain size, and microscopic stress in polycrystalline thin films. In this study, we simultaneously monitored the generation and temporal evolution of texture, grain size, and internal stress in cathodic arc evaporated Al0.50Ti0.50N thin films using a bespoke deposition apparatus designed for use with 2-dimensional synchrotron x-ray diffraction technique. The influence of the substrate temperature is investigated in terms of the emergence and development of texture, grain size and stress evolution. A dynamic evolution of the crystallographic texture is observed as the overall film thickness varies. We clearly resolved two regime of films growth based on stress evolution. Beyond a threshold grain size (~ 14 nm), the stress scales inversely to the average grain sizes, and as the film thickness increases, immediate compressive stress relaxation was seen. An extensive ex-situ evaluation of thin films using electron microscopies and electron diffraction was performed to support the in-situ x-ray diffraction results.

This paper aims to elucidate the role of interface energy anisotropy in orientation selection during nucleation of new grains in a polycrystalline film growth. An assessment of (heterogeneous) nucleation probability as function of orientation of both the bottom grain and of the nucleus was developed (using the concepts of classical nucleation theory). Novel solutions to the generalized Winterbottom construction were described in cases of very strong anisotropy and arbitrary orientations. In order to demonstrate the effect on the film crystallographic texture, a 2D Monte Carlo algorithm for anisotropic polycrystalline growth was used to simulate growth of films with columnar microstructure. The effect of strength of anisotropy, the deposition rate and initial texture were investigated. Results showed that with larger strength of anisotropy, the nucleation rate is less dependent on the driving force, but more dependent on the initial texture. With certain initial textures, the anisotropic nucleation may even be either impossible or having probability close to one irrespective of the driving force. Depending on the conditions, the anisotropic nucleation could hasten the evolution towards the interface-energy minimizing texture or retard it. Based on these insights, a hypothesis was offered to explain a peculiar texture evolution in electrodeposited nickel., Comment: 18 pages, 14 figures, 1 table Submitted in September 2023 to Computational Materials Science, Elsevier

Plastic inhomogeneity, particularly localised strain, is one of the main mechanisms responsible for failures in engineering alloys. This work studied the spatial arrangement and distribution of microstructure and their influence in the plastic inhomogeneity of Inconel 718 fabricated by additive manufacturing (AM). In particular, the density and spatial distribution of geometrically necessary dislocations (GNDs) and the crystallographic texture components were examined in relation to the spatial plastic deformation. In-situ tensile testing coupled with microscopy and EBSD was performed to understand the evolution of the as-built microstructure and its effect on the spatial and temporal deformation behaviour. Bidirectional scan strategy with no interlayer rotation resulted in highly ordered alternating arrangements of coarse Goss-like {110}<001> textured grains separated by fine Cube-like {100}<001> textured grains. This strategy also resulted in an overall high density of dislocations (in particular GNDs) with a regular pattern: the fine grains contained very high GND density while the coarse grains contained less GNDs but they were oriented to be perpendicular to the scan direction. Although this strategy resulted in a dominant Cube texture that is desirable for isotropy, the Cube texture gradually weakened and the undesirable Goss component increased during plastic deformation. Together with the columnar grain morphology and aligned GND arrangement, such texture evolution caused intense plastic inhomogeneity during deformation. Replacing the bidirectional strategy with a chessboard strategy involving a 67{\deg} layer rotation resulted in a lower GND density and much more random distribution of crystallographic texture and GNDs, with a dominant Cube component (and lower Goss texture) that remained stable throughout plastic deformation, reducing the plastic inhomogeneity.

FePd thin films have been recently considered as promising material for high-density magnetic storage devices. However, it is necessary to find a proper method of fabrication for the (001)-textured and chemically well-ordered alloy. In this paper, we present the detailed investigations of lattice parameters, chemical order degree, grain sizes and crystallographic texture, carried out on FePd alloys with 10 at.% of Cu addition. The initial [Cu(0.2 nm)/Fe(0.9 nm)/Pd(1.1 nm)]x5 multilayers were thermally evaporated in an ultra-high vacuum on MgO(100), Si(100), Si(111) and Si(100) covered by 100 nm thick layer of amorphous SiO2. In order to obtain homogeneous FePd:Cu alloy, the multilayers were annealed in two different ways. First, the samples were rapidly annealed in nitrogen atmosphere at 600oC for 90 seconds. Next, the long annealing in a high vacuum for 1 hour at 700oC was done. This paper focuses on quantitative investigations of the chemical order degree and crystallographic texture of ternary FePd:Cu alloys deposited on four different substrates. In order to obtain both quantities we have taken a novel approach to consider the problem of dopant atoms located in the FePd structure. The studies of the structure were done using X-Ray Diffraction (XRD) performed with synchrotron radiation and pole figures measurements. We have found that the addition of Cu changes the FePd lattice parameters and lattice distortion. We have also shown, that using different substrates it is possible to obtain a FePd:Cu alloy with different chemical order and texture. Moreover, it was observed that texture category is substrate dependent.

The development of the crystallinity and of the crystallographic orientation of isotactic polypropylene (iPP) during rolling deformation and subsequent heat treatment is studied. The experiments are conducted by using X-ray diffraction with an area detector. The evolution of crystallographic orientation is tracked by calculating the pole figures and by applying a quantitative 3D texture component fit method. The rolling orientation after a true strain of -1.5 mainly consists of the (010)[001], (130)[001], and [001]//RD fiber components (RD: rolling direction). The results reveal that the crystallinity drastically decreases during rolling. We suggest that decrystallization (disaggregation) is a deformation mechanism which takes place as a microscopic alternative to crystallographic intralamellar shear depending on the orientation of the lamellae relative to the imposed deformation tensor. Heat treatment after rolling leads to the recrystallization of amorphous material and to a strong enhancement of the fiber orientation component. The recrystallization orientation is explained in terms of an oriented nucleation mechanism where amorphous material aligns along existing crystalline lamellae blocks which prevailed during the preceding deformation.

Eutectic rods of Al2O3 and Y3Al5O12 were grown by a laser-heated float zone method, and their microstructure and crystallographic texture were studied by scanning electron microscopy, electron backscattered diffraction and x-ray diffraction. The composites were found to be highly textured with two twin-related crystallographic orientation relationships between the phases. Electron backscattered diffraction was employed to determine the spatial distribution of the orientational variants within the samples and to define the crystallographic orientation of various microstructural features.

Crystallographic and elastic moduli data are presented which document the degree of texture in several oxide dispersion-strengthened (ODS) nickel-base alloys. The existence of strong crystallographic textures in such multicrystalline alloys is considered important, since the small angle grain boundaries may be partially responsible for creep threshold stresses. Gleiter (1979) has shown that ideal, low energy boundaries will act as vacancy sources only when the applied stress is greater than a threshold stress, while large angle grain boundaries will emit vacancies at all stress levels. The continued operation of a net vacancy in an ODS alloy must be avoided, since it will lead to a localized disruption of the microstructure.

Crystal plasticity finite element simulations are frequently employed to predict the plastic anisotropy of polycrystalline metals based on their crystallographic texture. In age-hardenable aluminium alloys, however, the texture-induced plastic anisotropy is known to affect by precipitation. This paper presents a new modelling approach to incorporate this effect into crystal plasticity constitutive models. The approach focuses on the overall effect of precipitation, which is assumed to result in an additional directional dependency with respect to a global material orientation, superimposed with the texture-induced plastic anisotropy. This additional directional dependency is implemented into a conventional crystal plasticity constitutive model via a modified hardening law that introduces two new parameters, of which only one is treated as a free parameter. To demonstrate the applicability of the new modelling approach, it is applied to an age-hardenable AA6014-T4 aluminium alloy and compared against a state-of-the-art crystal plasticity constitutive model that considers only crystallographic texture. The results demonstrate that the new modelling approach significantly improves the prediction accuracy of the plastic anisotropy for the AA6014-T4 aluminium alloy studied., Comment: as submitted, after one round of review

The crystallographic texture is a key organization feature of many technical and biological materials. In these materials, especially hierarchically structured ones, the preferential alignment of the nano constituents is heavily influencing the macroscopic behaviour of the material. In order to study local crystallographic texture with both high spatial and angular resolution, we developed Texture tomography (TexTOM). This approach allows to model the diffraction data of polycrystalline materials by using the full reciprocal space of the ensemble of crystals and describe the texture in each voxel via a orientation distribution function. This means, it provides 3D reconstructions of the local texture by measuring the probabilities of all crystal orientations. The TexTOM approach addresses limitations associated with existing models: It correlates the intensities from several Bragg reflections, thus reduces ambiguities resulting from symmetry. Further, it yields quantitative probability distributions of local real space crystal orientations without further assumptions on the sample structure. Finally, its efficient mathematical formulation enables reconstructions faster than the time-scale of the experiment. In this manuscript, we present the mathematical model, the inversion strategy and its current experimental implementation. We show characterizations of simulated data as well as experimental data obtained from a synthetic, inorganic model sample, the silica-witherite biomorph. In conclusion, Tex-TOM provides a versatile framework to reconstruct 3D quantitative texture information for polycrystalline samples. In this way, it opens the door for unprecedented insights into the nanostructural makeup of natural and technical materials.

The crystallographic texture of metallic materials is a key microstructural feature that is responsible for the anisotropic behavior, e.g., important in forming operations. In materials science, crystallographic texture is commonly described by the orientation distribution function, which is defined as the probability density function of the orientations of the monocrystal grains conforming a polycrystalline material. For representing the orientation distribution function, there are several approaches such as using generalized spherical harmonics, orientation histograms, and pole figure images . Measuring distances between crystallographic textures is essential for any task that requires assessing texture similarities, e.g. to guide forming processes. Therefore, we introduce novel distance measures based on (i) the Earth Movers Distance that takes into account local distance information encoded in histogram-based texture representations and (ii) a distance measure based on pole figure images. For this purpose, we evaluate and compare existing distance measures for selected use-cases. The present study gives insights into advantages and drawbacks of using certain texture representations and distance measures with emphasis on applications in materials design and optimal process control.

The influence of the microstructure of a polycrystalline material on its macroscopic deformation response is still one of the major problems in materials engineering. For materials characterized by elastic-plastic deformation responses, predictive computational models to characterize crystal-plasticity (CP) have been developed. However, due to their large demand of computational resources, CP simulations cannot be straightforwardly implemented in hierarchical computational models such as FE$^{2}$. This bottleneck intensifies the need for the development of macroscopic simulation tools that can be directly informed by microstructural quantities. Using a 3D Finite-Element solver for CP, we generate a macroscopic yield function database based on general loading conditions and crystallographic texture. We furthermore assume an independence of the yield function to hydrostatic pressure of the yield function. Leveraging the advancement in statistical modeling we describe and apply a machine learning framework for predicting macroscopic yield as a function of crystallographic texture. The convexity of the data-driven yield function is guaranteed by using partially input convex neural networks as the predictive tool. Furthermore, in order to allow for the predicted yield function to be directly incorporated in time-integration schemes, as needed for the Finite Element method, the yield surfaces are interpreted as the boundaries of signed distance function level sets., Comment: 23 pages, 16 figures

Directional wave speeds variations in anisotropic elastic solids enables material characterisation capabilities, such as determination of elastic constants and volumetric measurement of crystallographic texture. However, achieving such measurements is challenging especially on samples with complex geometries. Here we propose the use of Green's Function reconstruction from diffuse ultrasonic wave fields for accurate velocity measurements on components with arbitrary geometries. Strategies for accurate reconstruction, including averaging over an increased number of different source locations, using longer window lengths of diffuse fields, and accurately deconvolving a source-dependent factor, were implemented to achieve satisfactory convergence towards Green's Function. Additionally, low signal intensity challenges from laser interferometers were overcome to enable non-contact measurement of the wave speeds, by making use of simultaneous excitation of sources to increase signal-to-noise ratio and signal normalisation to account for energy dissipation of diffuse fields. With successful demonstration using both phased array and laser receivers, this advancement fundamentally broadens acoustic wave velocity measurement capabilities to a wider range of environments and holds promise for future material characterisation of complex-shaped components.

High-throughput experiments that use combinatorial samples with rapid measurements can be used to provide process-structure-property information at reduced time, cost, and effort. Developing these tools and methods is essential in additive manufacturing where new process-structure-property information is required on a frequent basis as advances are made in feedstock materials, additive machines, and post-processing. Here we demonstrate the design and use of combinatorial samples produced on a commercial laser powder bed fusion system to study 60 distinct process conditions of nickel superalloy 625: five laser powers and four laser scan speeds in three different conditions. Combinatorial samples were characterized using optical and electron microscopy, x-ray diffraction, and indentation to estimate the porosity, grain size, crystallographic texture, secondary phase precipitation, and hardness. Indentation and porosity results were compared against a regular sample. The smaller-sized regions (3 mm x 4 mm) in the combinatorial sample have a lower hardness compared to a larger regular sample (20 mm x 20 mm) with similar porosity (< 0.03 %). Despite this difference, meaningful trends were identified with the combinatorial sample for grain size, crystallographic texture, and porosity versus laser power and scan speed as well as trends with hardness versus stress-relief condition., Comment: 44 pages, 13 figures, 4 tables (not including the supplemental material) submitted to Materials & Design

Crystallographic texture engineering in ceramics is essential to achieve direction-specific properties. Current texture engineering methods are time-consuming, energy extensive, or can lead to unnecessary diffusion of added dopants. Herein, we explore ultrafast high-temperature sintering (UHS) to prepare dense and textured alumina using templated grain growth (TGG). From a slurry containing alumina microplatelets coated with Fe3O4 nanoparticles dispersed in a matrix of alumina nanoparticles, green bodies with oriented microplatelets were prepared using magnetic assisted slip casting (MASC). The effects of the sintering temperature, time and heating rate on the density and microstructure of the obtained ceramics were then studied. We found that TGG occurs for a temperature range between 1640 and 1780 {\deg}C and 10 s sintering time. Sintering at 1700 {\deg}C for 10 s led to dense and textured alumina with anisotropic grains thanks to the Fe3O4 coating, which did not have the time to diffuse. The highest texture and relative density were obtained with a heating rate of ~5,500 {\deg}C/min, leading to texture-dependent anisotropic mechanical properties. This study opens new avenues for fabricating textured ceramics in ultra-short times., Comment: 37 pages, 19 figures, includes main manuscript and abstract

The mechanisms that govern a previously unexplained hardening effect of a single phase Cu-30wt%Zn {\alpha}-brass after heating have been investigated. After cold-work, the alloy possesses an increased yield strength and hardening rate only when heat treated to temperatures close to 220{^\circ}C, and is otherwise softer. Crystallographic texture and microstructure, explored using electron backscatter diffraction (EBSD), describe the deformation heterogeneity including twin development, as a function of heat treatment. When heated, an increased area fraction of deformation twins is observed, with dimensions reaching a critical size that maximises the resistance to dislocation slip in the parent grains. The effect is shown to dominate over other alloy characteristics including short range order, giving serrated yielding during tensile testing which is mostly eliminated after heating. In-situ X-ray diffraction during tensile testing corroborates these findings; dislocation-related line broadening and lattice strain development between as worked and heated {\alpha}-brass is directly related to the interaction between the dislocations and the population of deformation twins. The experiments unambiguously disprove that other thermally-induced microstructure features contribute to thermal hardening. Specifically, the presence of recrystallised grains or second phases do not play a role. As these heat treatments match annealing conditions subjected to {\alpha}-brass during deformation-related manufacturing processes, the results here are considered critical to understand, predict and exploit, where appropriate, any beneficial process-induced structural behaviour.

Surface characteristics are a major contributor to the in-service performance, particularly fatigue life, of additively manufactured (AM) components. Centrifugal disk finishing (CDF) is one of many rigid media, abrasive machining processes employed to smooth the surfaces and edges of AM components. Within the general family of abrasive machining processes currently applied to AM, CDF is moderate in terms of material removal rate and the inertial forces exerted. How CDF alters the underlying microstructure of the processed surface is currently unknown. Here we employ white light profilometry and high-energy X-ray diffraction to characterize surface finish, crystallographic texture, and anisotropic distributions of residual microscale strain as a function of depth in CDF-finished Inconel 718 manufactured with laser powder bed fusion. Surfaces are finished using both unimodal and bimodal finishing media size distributions. We find that CDF will remove surface crystallographic textures (here a {111} fiber texture) from AM components, but generally not alter the bulk texture (here a cube texture). CDF is also found to impart significant amounts of residual microscale strain into the first 100 $\mu$m from the sample surface as evidenced by an approximately 50% increase in diffraction peak widths at 20 $\mu$m from the surface in comparison to 120 $\mu$m.

Scaling superconducting digital circuits requires fundamental changes in the current material set and fabrication process. The transition to 300 mm wafers and the implementation of advanced lithography are instrumental in facilitating mature CMOS processes, ensuring uniformity, and optimizing the yield. This study explores the properties of NbxTi(1-x)N films fabricated by magnetron DC sputtering on 300 mm Si wafers. As a promising alternative to traditional Nb in device manufacturing, NbxTi(1-x)N offers numerous advantages, including enhanced stability and scalability to smaller dimensions, in both processing and design. As a ternary material, NbxTi(1-x)N allows engineering material parameters by changing deposition conditions. The engineered properties can be used to modulate device parameters through the stack and mitigate failure modes. We report characterization of NbxTi(1-x)N films at less than 2% thickness variability, 2.4% Tc variability and 3% composition variability. The films material properties such as resistivity (140-375 {\Omega}cm) and critical temperature Tc (4.6 K - 14.1 K) are correlated with stoichiometry and morphology of the films. Our results highlight the significant influence of deposition conditions on crystallographic texture along the films and its correlation with Tc., Comment: 8 pages 8 figures

Fretting wear is a surface degradation process caused by oscillatory motion and contact slipping. During gross slip, high local stresses and plastic deformation in the surface and subsurface can lead to the creation of a nanosized grained structure called Tribologically Transformed Structure (TTS). The current paper studies the formation of TTS in an alpha-beta Ti-6Al-4V alloy under fretting loading while changing the contact pressure and the number of fretting cycles.Cross-sections of wear scars are observed after polishing and chemical etching. Above a threshold pressure of 300 MPa, TTS appears early in the contact (before 1000 cycles) along with two other structures: a Third Body Layer (TBL) made of compacted debris and a General Deformed Layer (GDL) which is the plastic zone under the TTS. TTS first appears as islands and merges in the middle of the contact after enough cycles. Below 200 MPa, only TBL and GDL are formed. At 200 MPa, only small, localized TTS is found. All structures have the same chemical compositions as the initial bulk material except for the nitrided TBL. TTS has a very high hardness compared to the bulk. TTS was carefully extracted using a Focused Ion Beam (FIB) and its microstructure was observed with a Transmission Electron Microscope (TEM). It shows extreme grain refinement and is composed of two alternated zones. The first zone I is composed of $\alpha$ grains with a size of 20 to 50 nm with crystallographic texture. Zone II comprises nanosized equiaxed grains whose sizes range from 5 to 20 nm without texture. The results made it possible to establish a scenario of the appearance of the TTS according to the conditions of contact pressure and number of fretting cycles.

In the presented research, the intergranular elastic interaction and the second-order plastic incompatibility stress in textured ferritic and austenitic steels were investigated by means of diffraction. The lattice strains were measured inside the samples by the multiple reflection method using high energy X-rays diffraction during uniaxial in situ tensile tests. Comparing experiment with various models of intergranular interaction, it was found that the Eshelby-Kr\"oner model correctly approximates the X-ray stress factors (XSFs) for different reflections hkl and scattering vector orientations. The verified XSFs were used to investigate the evolution of the first and second-order stresses in both austenitic and ferritic steels. It was shown that considering only the elastic anisotropy, the non-linearity of $\sin^2{\psi}$ plots cannot be explained by crystallographic texture. Therefore, a more advanced method based on elastic-plastic self-consistent modeling (EPSC) is required for the analysis. Using such methodology the non-linearities of $\cos^2{\phi}$ plots were explained, and the evolutions of the first and second-order stresses were determined. It was found that plastic deformation of about 1- 2% can completely exchange the state of second-order plastic incompatibility stresses.

Computational experiments are exploited in finding a well-designed processing path to optimize material structures for desired properties. This requires understanding the interplay between the processing-(micro)structure-property linkages using a multi-scale approach that connects the macro-scale (process parameters) to meso (homogenized properties) and micro (crystallographic texture) scales. Due to the nature of the problem's multi-scale modeling setup, possible processing path choices could grow exponentially as the decision tree becomes deeper, and the traditional simulators' speed reaches a critical computational threshold. To lessen the computational burden for predicting microstructural evolution under given loading conditions, we develop a neural network (NN)-based method with physics-infused constraints. The NN aims to learn the evolution of microstructures under each elementary process. Our method is effective and robust in finding optimal processing paths. In this study, our NN-based method is applied to maximize the homogenized stiffness of a Copper microstructure, and it is found to be 686 times faster while achieving 0.053% error in the resulting homogenized stiffness compared to the traditional finite element simulator on a 10-process experiment.

We report the crystallographic texture of ZnO thin films comprising nanorods grown by a microwave irradiation assisted method. Different substrates were used, namely Si, Ge, metal coated Si, PMMA coated Si and ITO coated glass, to examine the respective development of crystallographic texture. The films were characterized by Xray diffraction and scanning electron microscopy, while the texture analysis was done by Xray pole figure analysis using the Schultz reflection method. The ZnO film deposited on Si and Ge showed a mixed texture. On all the other substrates, c axis oriented ZnO films were obtained.

Ferroelectrics have a spontaneous electrical polarization that is arranged into domains and can be reversed by an externally applied field. This high versatility makes them useful in enabling components such as capacitors, sensors, and actuators. The key to tuning their dielectric, piezoelectric, and electromechanical performance is to control the domain structure and the dynamics of the domain walls. In fixed compositions, this is often realized by chemical doping. In addition, structural and microstructural parameters, such as grain size, degree of crystallographic texture or porosity play a key role. A major breakthrough in the field came with the fundamental understanding of the link between the local electric and mechanical driving forces and domain wall motion. Here, the impact of structure and microstructure on these driving forces is reviewed and an engineering toolbox is introduced. An overview of advances in the understanding of domain wall motion on the micro- and nanoscale is provided and discussed in terms of the macroscopic functional performance of polycrystalline ferroelectrics/ferroelastics. In addition, a link to theoretical and computational models is established. The review concludes with a discussion about beyond state-of-the-art characterization techniques, new approaches, and future directions toward non-conventionally ordered ferroelectrics for next-generation nanoelectronics and energy-storage applications.

The artificial tailoring of magnetic anisotropy by manipulation of interfacial morphology and film structure are of fundamental interest from application point of view in spintronic and magnetic memory devices. This letter reports an approach of engineering and enhancing the strength of oblique incidence ion beam erosion (IBE) induced in-plane uniaxial magnetic anisotropy (UMA) by simultaneous modification of film morphology as well as film texture. To meet this objective, Cobalt film and Si substrate have been taken as a model system. Unlike conventional post growth IBE of film, we direct our effort to the sequential deposition and subsequent IBE of the film. Detailed in-situ investigation insights that the film grows in highly biaxially textured polycrystalline state with formation of nanometric surface ripples. The film also exhibits pronounced UMA with easy axis oriented parallel to the surface ripple direction. Remarkably, the induced UMA is about one order of magnitude larger than the reported similar kind of earlier studies. The possibility of imposing in-plane crystallographic texture giving rise to magneto-crystalline anisotropy, along with long-range dipolar interaction throughout ripple crests enhances the strength of the UMA. The present findings can be further extended to systems characterized by different crystallographic structure and magnetic properties and show the general applicability of the present method.

Deciphering the three-dimensional atomic structure of solid-solid interfaces in core-shell nanomaterials is the key to understand their remarkable catalytical, optical and electronic properties. Here, we probe the three-dimensional atomic structures of palladium-platinum core-shell nanoparticles at the single-atom level using atomic resolution electron tomography. We successfully quantify the rich structural variety of core-shell nanoparticles including bond length, coordination number, local bond orientation order, grain boundary, and five-fold symmetry, all in 3D at atomic resolution. Instead of forming an atomically-sharp boundary, the core-shell interface is atomically diffuse with an average thickness of 4.2 A, irrespective of the particle's size, morphology, or crystallographic texture. The high concentration of Pd in the interface is highly related to the electric double layers of the Pd seeds. These results advance our understanding of core-shell structures at the fundamental level, providing potential strategies into nanomaterial manipulation and chemical property regulation., Comment: 41 pages, 18 figures

Intercalation materials are promising candidates for reversible energy storage and are, for example, used as lithium-battery electrodes, hydrogen-storage compounds, and electrochromic materials. An important issue preventing the more widespread use of these materials is that they undergo structural transformations (of up to ~10% lattice strains) during intercalation, which expand the material, nucleate microcracks, and, ultimately, lead to material failure. Besides the structural transformation of lattices, the crystallographic texture of the intercalation material plays a key role in governing ion-transport properties, generating phase separation microstructures, and elastically interacting with crystal defects. In this review, I provide an overview of how the structural transformation of lattices, phase transformation microstructures, and crystallographic defects affect the chemo-mechanical properties of intercalation materials. In each section, I identify the key challenges and opportunities to crystallographically design intercalation compounds to improve their properties and lifespans. I predominantly cite examples from the literature of intercalation cathodes used in rechargeable batteries, however, the identified challenges and opportunities are transferable to a broader range of intercalation compounds., Comment: 13 pages, 5 figures

When compressed, a metallic specimen will generally experience changes to its crystallographic texture due to plasticity-induced rotation. Ultrafast x-ray diffraction techniques make it possible to measure rotation of this kind in targets dynamically compressed over nanosecond timescales to the kind of pressures ordinarily encountered in planetary interiors. The axis and the extent of the local rotation can provide hints as to the combination of plasticity mechanisms activated by the rapid uniaxial compression, thus providing valuable information about the underlying dislocation kinetics operative during extreme loading conditions. We present large-scale molecular dynamics simulations of shock-induced lattice rotation in three model crystals whose behavior has previously been characterized in dynamic-compression experiments: tantalum shocked along its [101] direction, and copper shocked along either [001] or [111]. We find that, in all three cases, the texture changes predicted by the simulations are consistent with those measured experimentally using in situ x-ray diffraction. We show that while tantalum loaded along [101] and copper loaded along [001] both show pronounced rotation due to asymmetric multiple slip, the orientation of copper shocked along [111] is predicted to be stabilized by opposing rotations arising from competing, symmetrically equivalent slip systems., Comment: 28 pages, 21 figures in main article; 4 pages, 5 figures in supplemental material. This article will be submitted to Physical Review Materials

The optimization along the chain processing-structure-properties-performance is one of the core objectives in data-driven materials science. In this sense, processes are supposed to manufacture workpieces with targeted material microstructures. These microstructures are defined by the material properties of interest and identifying them is a question of materials design. In the present paper, we addresse this issue and introduce a generic multi-task learning-based optimization approach. The approach enables the identification of sets of highly diverse microstructures for given desired properties and corresponding tolerances. Basically, the approach consists of an optimization algorithm that interacts with a machine learning model that combines multi-task learning with siamese neural networks. The resulting model (1) relates microstructures and properties, (2) estimates the likelihood of a microstructure of being producible, and (3) performs a distance preserving microstructure feature extraction in order to generate a lower dimensional latent feature space to enable efficient optimization. The proposed approach is applied on a crystallographic texture optimization problem for rolled steel sheets given desired properties.

A physically-informed continuum crystal plasticity model is presented to elucidate the deformation mechanisms and dislocation evolution in body-centered-cubic (bcc) tantalum widely used as a key structural material for mechanical and thermal extremes. We show our unified structural modeling framework informed by mesoscopic dislocation dynamics simulations is capable of capturing salient features of the large inelastic behavior of tantalum at quasi-static (10$^{-3}$ s$^{-1}$) to extreme strain rates (5000 s$^{-1}$) and at room temperature and higher (873K) at both single- and polycrystal levels. We also present predictive capabilities of our model for microstructural evolution in the material. To this end, we investigate the effects of dislocation interactions on slip activities, instability and strain-hardening behavior at the single crystal level. Furthermore, ex situ measurements on crystallographic texture evolution and dislocation density growth are carried out for the polycrystal tantalum specimens at increasing strains. Numerical simulation results also support that our modeling framework is capable of capturing the main features of the polycrystal behavior over a wide range of strains, strain rates and temperatures. The theoretical, experimental and numerical results at both single- and polycrystal levels provide critical insight into the underlying physical pictures for micro- and macroscopic responses and their relations in this important class of refractory bcc materials undergoing severe inelastic deformations.

Thick-section plates made from a recently developed Al-Cu-Mg-Li alloy have been evaluated to understand the influence of microstructure on the anisotropy of tensile strengths after natural and artificial ageing treatment. Pancake-shaped grains with a coarse substructure and strong crystallographic texture with a beta-fibre orientation at the mid-thickness position are observed. In addition, an inhomogeneous distribution of T1 precipitates through the plate thickness has been revealed with the volume fraction of intragranular precipitates ~ 40% higher at the plate centre than the thickness position. Altogether these microstructural features contribute to the in-plane anisotropy of tensile strengths that is ~ 5% higher at the mid-thickness position than the 1/4 thickness position. The variation of ageing-induced T1 precipitates through the plate thickness further contributes to the through-thickness anisotropy that is ~ 3% higher in T8 temper as compared to T3 temper.

A polycrystalline plasticity model, which incorporates the contribution of deformation twinning, is proposed. For this purpose, each material point is treated as a composite material consisting of a parent constituent and multiple twin variants. In the constitutive equations, the twin volume fractions and their spatial gradients are treated as external state variables to account for the contribution of twin boundaries to free energy. The set of constitutive relations is implemented in a spectral solver, which allows solving the differential equations resulting from equilibrium and compatibility conditions. The proposed model is then used to investigate the behavior of a AZ31 magnesium alloy. For the investigated loading conditions, the mechanical behavior is controlled by the joint contribution of basal slip and tensile twinning. Also, according to the numerical results, the development of crystallographic texture, morphological texture and internal stresses is consistent with the experimental observations of the literature.

Metals and alloys fabricated by fusion-based additive manufacturing (AM), or 3D printing, undergo complex dynamics of melting and solidification, presenting challenges to the effective control of grain structure. Herein, we report on the use of high-intensity ultrasound that controls the process of solidification during AM of 316L stainless steel. We find that the use of ultrasound favours the columnar-to-equiaxed transition, promoting the formation of fine equiaxed grains with random crystallographic texture. Moreover, the use of ultrasound increases the number density of grains from 305 mm-2 to 2748 mm-2 despite an associated decrease in cooling rate and temperature gradient in the melt pool during AM. Our assessment of the relationship between grain size and cooling rate indicates that the formation of crystallites during AM is enhanced by ultrasound. Furthermore, the use of ultrasound increases the amount of constitutional supercooling during solidification by lowering the temperature gradient in the bulk of the melt pool, thus creating an environment that favours nucleation, growth, and survival of grains. This new understanding provides opportunities to better exploit ultrasound to control grain structure in AM-fabricated metal products., Comment: Paper published in Additive Manufacturing

A metastable austenitic Fe-Cr-Ni steel was processed by selective laser melting with low power, resulting in nearly random crystallographic texture. In-situ tensile loading and neutron diffraction experiments were undertaken and the results indicate high ductility, despite the presence of porosity, and pronounced strain-induced martensitic transformation. A secondary hardening is observed in the mechanical data due to the martensite carrying significant load, upon its formation. The pronounced martensitic transformation is discussed with respect to the initial and the evolving deformation texture and its affinity for forming martensite under uniaxial tensile loading., Comment: As accepted version to Scripta Materialia

Ultrathin aluminum nitride (AlN) films are of great interest for integration into nanoelectromechanical systems for actuation and sensing. Given the direct relationship between crystallographic texture and piezoelectric response, x-ray diffraction has become an important metrology step. However, signals from layers deposited below the piezoelectric (PZE) AlN thin film may skew the crystallographic analysis and give misleading results. In this work, we compare the use of a Ti or AlN seed layer on the crystallographic quality of PZE AlN. We also analyze the influence of several AlN seed layer thicknesses on the rocking curve FWHM of PZE AlN and demonstrate an larger effect of the AlN seed layer on the {\theta}-2{\theta} AlN <0002> crystallographic peak for increasing AlN seed layer thickness., Comment: 16 pages, 4 figures, 1 table

This study is inspired by the recent development of "virtual material testing laboratory" in which the main equipment is a full field crystal plasticity modeling tool. Ample examples have demonstrated its applications to sheet forming operations. In those applications, the mechanical anisotropy originated from the crystallographic texture can be adequately described, such as r-values and earing. Formability is another important property in sheet metal forming, which has yet not been equipped in these virtual laboratories. Though theoretical models for formability can be dated back to 1885 due to Consid\`{e}re, all popular models at the moment suffer from their respective limitations. In this study, we explore the feasibility of applying full field crystal plasticity model for calculating forming limit diagram, avoiding using additional assumptions or models for determining the forming limits.

Microstructure characterisation has been greatly enhanced through the use of electron backscatter diffraction (EBSD), where rich maps are generated through analysis of the crystal phase and orientation in the scanning electron microscope (SEM). Conventional EBSD analysis involves raster scanning of the electron beam and the serial analysis of each diffraction pattern in turn. For grain shape, crystallographic texture, and microstructure analysis this can be inefficient. In this work, we present Rapid EBSD, a data fusion approach combining forescatter electron (FSE) imaging with static sparse sampling of EBSD patterns. We segment the FSE image into regions of similar colour (i.e. phase and crystal orientation) and then collect representative EBSD data for each segmented region. This enables microstructural assessment to be performed at the spatial resolution of the (fast) FSE imaging whilst including orientation and phase information from EBSD analysis of representative points. We demonstrate the Rapid EBSD technique on samples of a cobalt based superalloy and a strained dual phase titanium alloy, comparing the results with conventional analysis. Rapid EBSD is advantageous for assessing grain size distributions in time-limited experiments., Comment: As peer reviewed once and resubmitted. New comments made in yellow/red

Zirconium alloys are used in the nuclear industry as structural materials, and can be subject to high strain rate loading conditions during forming and in the case of a reactor accident. In this context, the relationship between strain rate dependent mechanical properties, crystallographic texture and deformation modes, such as slip and deformation twinning, are explored in this work. Commercially pure zirconium is deformed to 10 % engineering strain under quasi-static and high strain rate loading, and post-mortem analysis of the samples is performed using electron backscatter diffraction (EBSD) to observe different twin and slip systems activated. Twin types are identified from local intergranular misorientation maps, and active slip systems are identified from long range intragranular misorientation maps. We link characterisation of the mechanical responses, twin types and morphologies, and relative slip system activation as a function of loading mode. We find that variations in strength and hardening can be related to the relative propensity of twinning and the number of active slip systems., Comment: As submitted pre-print

Nanostructured and architectured copper niobium composite wires are excellent candidates for the generation of intense pulsed magnetic fields (>90T) as they combine both high strength and high electrical conductivity. Multi-scaled Cu-Nb wires are fabricated by accumulative drawing and bundling (a severe plastic deformation technique), leading to a multiscale, architectured, and nanostructured microstructure exhibiting a strong fiber crystallographic texture and elongated grain shapes along the wire axis. This paper presents a comprehensive study of the effective elastic behavior of this composite material by three multi-scale models accounting for different microstructural contents: two mean-field models and a full-field finite element model. As the specimens exhibit many characteristic scales, several scale transition steps are carried out iteratively from the grain scale to the macro-scale. The general agreement among the model responses allows suggesting the best strategy to estimate the effective behavior of Cu-Nb wires and save computational time. The importance of crystallographical and morphological textures in various cases is discussed. Finally, the models are validated by available experimental data with a good agreement., Comment: This paper has been published on 6 May 2017 in "International Journal of Solids and Structures"

We report the results of a comparative study of the magnetic microstructure of textured and isotropic $\mathrm{Nd}_2\mathrm{Fe}_{14}\mathrm{B}/\alpha$-$\mathrm{Fe}$ nanocomposites using magnetometry, transmission electron microscopy, synchrotron x-ray diffraction, and, in particular, magnetic small-angle neutron scattering (SANS). Analysis of the magnetic neutron data of the textured specimen and computation of the correlation function of the spin misalignment SANS cross section suggests the existence of inhomogeneously magnetized regions on an intraparticle nanometer length scale, about $40-50 \, \mathrm{nm}$ in the remanent state. Possible origins for this spin disorder are discussed: it may originate in thin grain-boundary layers (where the materials parameters are different than in the $\mathrm{Nd}_2\mathrm{Fe}_{14}\mathrm{B}$ grains), or it may reflect the presence of crystal defects (introduced via hot pressing), or the dispersion in the orientation distribution of the magnetocrystalline anisotropy axes of the $\mathrm{Nd}_2\mathrm{Fe}_{14}\mathrm{B}$ grains. X-ray powder diffraction data reveal a crystallographic texture in the direction perpendicular to the pressing direction -- a finding which might be related to the presence of a texture in the magnetization distribution, as inferred from the magnetic SANS data.

The quaternion Bingham distribution has been used to model preferred crystallographic orientation, or crystallographic texture, in polycrystalline materials in the materials science and geological communities. A primary difficulty in applying the Bingham distribution has been the lack of an efficient method for fitting the distribution parameters with respect to the materials underlying crystallographic symmetry or any statistical sample symmetry due to processing. In this paper we present a symmetrized distribution, based on the quaternion Bingham, which can account for any general combination of crystallographic or sample symmetries. We also introduce a numerical scheme for estimating the parameters of the symmetrized distribution based on the well known expectation maximization algorithm., Comment: Accepted 4/2016 as Short Communication to Journal of Applied Crystallography

The objective of this investigation was to establish whether crystallographic texture played a role in variable ST ductility in 2219-T87 thick plate. The EBSD study involved data collection at NASA Glenn Research Center and ODF analysis of the imported data at NASA Langley Research Center. The most significant result was that through-thickness variations in microtextural characteristics were asymmetrical about the mid-plane of the plate. However, the overall texture intensity was low, such that cross-sectional variations were classified as a second order effect on ST ductility.

A test block of Inconel (IN) 718 was fabricated using electron beam freeform fabrication (EBF(sup 3)) to examine how the EBF(sup 3) deposition process affects the microstructure, crystallographic texture, and mechanical properties of IN 718. Tests revealed significant anisotropy in the elastic modulus for the as-deposited IN 718. Subsequent tests were conducted on specimens subjected to a heat treatment designed to decrease the level of anisotropy. Electron backscatter diffraction (EBSD) was used to characterize crystallographic texture in the as-deposited and heat treated conditions. The anisotropy in the as-deposited condition was strongly affected by texture as evidenced by its dependence on orientation relative to the deposition direction. Heat treatment resulted in a significant improvement in modulus of the EBF(sup 3) product to a level nearly equivalent to that for wrought IN 718 with reduced anisotropy; reduction in texture through recrystallization; and production of a more homogeneous microstructure.

We demonstrate a facile method to produce crystallographically textured, macroporous materials using a combination of modified ice templating and templated grain growth (TGG). The process is demonstrated on alumina and the lead-free piezoelectric material sodium potassium niobate. The method provides macroporous materials with aligned, lamellar ceramic walls which are made up of crystallographically aligned grains. Each method showed that the ceramic walls present a long-range order over the entire sample dimensions and have crystallographic texture as a result of the TGG process. We also present a modification of the March-Dollase equation to better characterize the overall texture of materials with textured but slightly misaligned walls. The controlled crystallographic and morphologic orientation at two different length scales demonstrated here can be the basis of multifunctional materials., Comment: 14 pages, 7 figures, 19 references

We present a thorough research on Ta/Ru-based buffers and their influence on features crucial from the point of view of applications of MTJs, such as critical switching current and thermal stability. We investigate devices consisting of buffer/FeCoB/MgO/FeCoB/Ta/Ru multilayers for three different buffers: Ta 5 / Ru 10 / Ta 3, Ta 5 / Ru 10 / Ta 10 and Ta 5 / Ru 20 / Ta 5 (all thicknesses in nm). In addition, we study systems with a single FeCoB layer deposited above as well as below the MgO barrier. The crystallographic texture and the roughness of the buffers are determined by means of XRD and atomic force microscopy measurements. Furthermore, we examine the magnetic domain pattern, the magnetic dead layer thickness and the perpendicular magnetic anisotropy fields for each sample. Finally, we investigate the effect of the current induced magnetization switching for nanopillar junctions with lateral dimensions ranging from 1 {\mu}m down to 140 nm. Buffer Ta 5 / Ru 10 / Ta 3, which has the thickest dead layer, exhibits a large increase in the thermal stability factor while featuring a slightly lower critical current density value when compared to the buffer with the thinnest dead layer Ta 5 / Ru 20 / Ta 5.

Vibration damping in polycrystalline TbDy alloys was studied at cryogenic temperatures. The material was prepared by cold-rolling to induce crystallographic texture, and was then heat-treated to relieve internal stress. Mechanical hysteretic losses were measured at various strains, frequencies, and loading configurations at 77 K. Some textured TbDy materials demonstrated 22.6% energy dissipation in mechanical measurements at low frequency (0.01 Hz) and a mean logarithmic decrement of 0.23 at a higher frequency (25 kHz). Ultrasonic velocities of longitudinal and shear elastic waves were measured on single and polycrystalline TbDy; little variation in ultrasonic velocities was found evenfor samples with large variation in crystallographic texture and magnetomechanical properties.