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The exceptional mechanical strength of medium/high-entropy alloys has been attributed to hardening in random solid solutions. Here, we evidence non-random chemical mixing in a CrCoNi alloy, resulting from short-range ordering. A data-mining approach of electron nanodiffraction enabled the study, which is assisted by neutron scattering, atom probe tomography, and diffraction simulation using first-principles theory models. Two samples, one homogenized and one heat-treated, are observed. In both samples, results reveal two types of short-range-order inside nanoclusters that minimize the Cr–Cr nearest neighbors (L1 2 ) or segregate Cr on alternating close-packed planes (L1 1 ). The L1 1 is predominant in the homogenized sample, while the L1 2 formation is promoted by heat-treatment, with the latter being accompanied by a dramatic change in dislocation-slip behavior. These findings uncover short-range order and the resulted chemical heterogeneities behind the mechanical strength in CrCoNi, providing general opportunities for atomistic-structure study in concentrated alloys for the design of strong and ductile materials. Non-random chemical mixings that are intrinsic to medium- and high-entropy alloys are difficult to detect and quantify. Here the authors perform a diffraction data-mining analysis, revealing nanoclusters of short-range orders in a CrCoNi alloy, and their impacts on chemical homogeneity and dislocations slip.

Electrochemical intercalation can enable lithium extraction from dilute water sources. However, during extraction, co-intercalation of lithium and sodium ions occurs, and the response of host materials to this process is not fully understood. This aspect limits the rational materials designs for improving lithium extraction. Here, to address this knowledge gap, we report one-dimensional (1D) olivine iron phosphate (FePO 4 ) as a model host to investigate the co-intercalation behavior and demonstrate the control of lithium selectivity through intercalation kinetic manipulations. Via computational and experimental investigations, we show that lithium and sodium tend to phase separate in the host. Exploiting this mechanism, we increase the sodium-ion intercalation energy barrier by using partially filled 1D lithium channels via non-equilibrium solid-solution lithium seeding or remnant lithium in the solid-solution phases. The lithium selectivity enhancement after seeding shows a strong correlation with the fractions of solid-solution phases with high lithium content (i.e., Li x FePO 4 with 0.5 ≤ x < 1). Finally, we also demonstrate that the solid-solution formation pathway depends on the host material’s particle morphology, size and defect content. Lithium extraction from dilute sources could help solve the lithium supply security issue. Here, the authors investigate the Li- and Na- ion co-intercalation behavior in iron phosphate electrodes and demonstrate the lithium selectivity control through intercalation kinetic manipulations.

Solution processable semiconducting polymers have been under intense investigations due to their diverse applications from printed electronics to biomedical devices. However, controlling the macromolecular assembly across length scales during solution coating remains a key challenge, largely due to the disparity in timescales of polymer assembly and high-throughput printing/coating. Herein we propose the concept of dynamic templating to expedite polymer nucleation and the ensuing assembly process, inspired by biomineralization templates capable of surface reconfiguration. Molecular dynamic simulations reveal that surface reconfigurability is key to promoting template–polymer interactions, thereby lowering polymer nucleation barrier. Employing ionic-liquid-based dynamic template during meniscus-guided coating results in highly aligned, highly crystalline donor–acceptor polymer thin films over large area (>1 cm 2 ) and promoted charge transport along both the polymer backbone and the π–π stacking direction in field-effect transistors. We further demonstrate that the charge transport anisotropy can be reversed by tuning the degree of polymer backbone alignment. Controlling macromolecular assembly across length scales during solution coating of semiconducting polymers is still a challenge. Here the authors show a biomineralization inspired dynamic templating method that expedites polymer nucleation and assembly which allows for surface reconfiguration.

A diffraction-based technique is developed for the determination of three-dimensional nanostructures. The technique employs high-resolution and low-dose scanning electron nanodiffraction (SEND) to acquire three-dimensional diffraction patterns, with the help of a special sample holder for large-angle rotation. Grains are identified in three-dimensional space based on crystal orientation and on reconstructed dark-field images from the recorded diffraction patterns. Application to a nanocrystalline TiN thin film shows that the three-dimensional morphology of columnar TiN grains of tens of nanometres in diameter can be reconstructed using an algebraic iterative algorithm under specified prior conditions, together with their crystallographic orientations. The principles can be extended to multiphase nanocrystalline materials as well. Thus, the tomographic SEND technique provides an effective and adaptive way of determining three-dimensional nanostructures.

We designed a clamped beam bending test using a nanoindentation holder with help of transmission electron microscopy (TEM) and focused ion beam specimen fabrication. The microstructure evolution and crack propagation in nanocrystalline TiN were studied by electron imaging and load–displacement measurements during mechanical loading. By measuring the loads under which the crack starts and stops propagating and the time, we obtained the film's fracture toughness using the finite element method and crack propagation speed. Among these, we identified three types of crack propagation pathways, namely bridging, intergranular and a mixed mode of transgranular and intergranular fracture, and the associated microstructure changes. The measured fracture toughness is in agreement with the reported values. Thus, our in situ TEM bending test provides the first direct measurement of fracture toughness in a TEM and a correlation of fracture toughness with fracture toughening mechanisms in nanocrystalline TiN. The method is general and can be applied to other nanocrystalline materials.

Crystals deform by the intermittent multiplication and slip avalanches of dislocations. While dislocation multiplication is well-understood, how the avalanches form, however, is not clear, and the lack of insight in general has contributed to “a mass of details and controversy” about crystal plasticity. Here, we follow the development of dislocation avalanches in the compressed nanopillars of a high entropy alloy, Al 0.1 CoCrFeNi, using direct electron imaging and precise mechanical measurements. Results show that the avalanche starts with dislocation accumulations and the formation of dislocation bands. Dislocation pileups form in front of the dislocation bands, whose giveaway trigs the avalanche, like the opening of a floodgate. The size of dislocation avalanches ranges from few to 10 2  nm in the nanopillars, with the power-law distribution similar to earthquakes. Thus, our study identifies the dislocation interaction mechanism for large crystal slips, and provides critical insights into the deformation of high entropy alloys. Crystal deformation has been the subject of intense studies and debates since the discovery of dislocation in 1934. The paper presents an experimental study via electron imaging of a high entropy alloy to follow dislocation activities that lead to the dislocation avalanche occurring in the material.

Interfaces between correlated complex oxides are promising avenues to realize new forms of magnetism that arise as a result of charge transfer, proximity effects, and locally broken symmetries. We report on the discovery of a noncollinear magnetic structure in superlattices of the ferromagnetic metallic oxide La2/3Sr1/3MnO3 (LSMO) and the correlated metal LaNiO3 (LNO). The exchange interaction between LSMO layers is mediated by the intervening LNO, such that the angle between the magnetization of neighboring LSMO layers varies in an oscillatory manner with the thickness of the LNO layer. The magnetic field, temperature, and spacer thickness dependence of the noncollinear structure are inconsistent with the bilinear and biquadratic interactions that are used to model the magnetic structure in conventional metallic multilayers. A model that couples the LSMO layers to a helical spin state within the LNO fits the observed behavior. We propose that the spin-helix results from the interaction between a spatially varying spin susceptibility within the LNO and interfacial charge transfer that creates localized Ni2+ states. Our work suggests a new approach to engineering noncollinear spin textures in metallic oxide heterostructures.