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Understanding material failure on a fundamental level is a key aspect in the design of robust structural materials, especially for metals and alloys capable to undergo plastic deformation. In the last decade, significant progress is made in quantifying the stresses associated with failure in both experiments and simulations. Nonetheless, the processes occurring on the most essential level of individual dislocations that govern semi-brittle and ductile fracture are still experimentally not accessible, limiting the failure prediction capabilities. Therefore, in the present work, a one-of-a-kind nanoscale fracture experiment is conducted on a single crystalline Cr bending beam in situ in the transmission electron microscope and for the first time quantify the transient strains around individual dislocations, as well as of the whole dislocation network during crack opening. The results reveal the importance of both pre-existing and newly emitted dislocations for crack-tip shielding via their intrinsic strain field and provide guidelines to design more damage tolerant materials.

We describe the development, operation, and application of the 4D Camera-a 576 by 576 pixel active pixel sensor for scanning/transmission electron microscopy which operates at 87,000 Hz. The detector generates data at ∼480 Gbit/s which is captured by dedicated receiver computers with a parallelized software infrastructure that has been implemented to process the resulting 10-700 Gigabyte-sized raw datasets. The back illuminated detector provides the ability to detect single electron events at accelerating voltages from 30 to 300 kV. Through electron counting, the resulting sparse data sets are reduced in size by 10--300× compared to the raw data, and open-source sparsity-based processing algorithms offer rapid data analysis. The high frame rate allows for large and complex scanning diffraction experiments to be accomplished with typical scanning transmission electron microscopy scanning parameters.

Diffusion is one of the most fundamental concepts in materials science, playing a pivotal role in materials synthesis, forming, and degradation. Of particular importance is solid state interdiffusion of metals which defines the usable parameter space for material combinations in the form of alloys. This parameter space can be explored on the macroscopic scale by using diffusion couples. However, this method reaches its limit when going to low temperatures, small scales, and when testing ultrathin diffusion barriers. Therefore, this work transfers the principle of the diffusion couples to small scales by using core-shell nanowires and in situ heating. This allows us to delve into the interdiffusion dynamics of copper and gold, revealing the interplay between diffusion and the disorder-order phase transition. Our in situ TEM experiments in combination with chemical mapping reveal the interdiffusion coefficients of Cu and Au at low temperatures and highlight the impact of ordering processes on the diffusion behavior. The formation of ordered domains within the solid-solution is examined using high-resolution imaging and nanodiffraction including strain mapping. In addition, we examine the effectiveness of ultrathin Al2O3 barrier layers to control interdiffusion of the diffusion couple. Our findings indicate that a 5 nm thick layer serves as an efficient diffusion barrier. This research provides valuable insights into the interdiffusion behavior of Cu and Au on the nanoscale, offering potential applications in the development of miniaturized integrated circuits and nanodevices.

Structural materials used in nuclear reactor environments are subjected to coupled extremes such as high temperature, irradiation, and corrosion which act in concert to degrade their functional performance. Connecting alloy microstructure such as grain boundaries, and accumulating point defects with corrosion attack and pore morphology is critical to understanding underlying mechanisms. We uncover the compositional variations and morphology at multiple length scales in corrosion-damaged Ni-Cr alloy after exposure to oxidants in molten fluoride salts. A complex network of dense corrosion pores is detected by surface-level SEM observations. The corrosion pores take on a 1-dimensional morphology and are enriched with Ni and depleted of Cr 1–5 µm from the pore surface. STEM-EDS and 4D-STEM strain maps acquired simultaneously highlight the local variations in composition and structure of a ≤ 200 nm Cr-rich layer identified from a cross-section taken at the bottom of an isolated corrosion pore between the Ni-Cr alloy matrix and the embedded salt. However, the absence of an observed interface between the Ni-Cr alloy matrix and the FCC-structured Cr-rich layer suggests that Cr plating from the salt did not transpire. These findings support a proposed Cr lattice diffusion mechanism rather than Cr-precipitation from the salt to accommodate temperature transient conditions during sample cooling. Through the development of a 1D phase field model, these results are rationalized by formation energies for the Ni- and Cr-oxidation into the molten salt. This study reveals the locally altered microstructure caused by high temperature corrosion in non-steady-state molten salt nuclear reactor environments.

Diffuse intensities in the electron diffraction patterns of concentrated face-centered cubic solid solutions have been widely attributed to chemical short-range order, although this connection has been recently questioned. This article explores the many nonordering origins of commonly reported features using a combination of experimental electron microscopy and multislice diffraction simulations, which suggest that diffuse intensities largely represent thermal and static displacement scattering. A number of observations may reflect additional contributions from planar defects, surface terminations incommensurate with bulk periodicity, or weaker dynamical effects.

The dealloying corrosion behavior of the FCC Ni20Cr (wt%) in molten LiF-NaF-KF (FLiNaK) salts at 600 °C under varying applied potentials was investigated. Using in-operando electrochemical techniques and a multi-modal suite of characterization methods, we connect electrochemical potential, thermodynamic stability, and electro-dissolution kinetics to the corrosion morphologies. Notably, under certain potential regimes, a micron-scale bicontinuous structure, characterized by a network of interconnected pores and ligaments riched with the composition of the more noble (MN) element, becomes prominent. At other potentials both MN and less noble (LN) elements dealloy but at different rates. The dealloying process consists of lattice and grain boundary diffusion of Cr to the metal/salt interface, interphase Cr oxidation, accompanied by surface diffusion of Ni to form interconnected ligaments. At higher potentials, the bicontinuous porous structure undergoes further surface coarsening. Concurrently, Cr(II), Cr(III), and Ni(II) begin to dissolve, with the dissolution of Ni occurring at a significantly slower rate. When solid-state transport of Cr is exceeded by the interfacial rates, dealloying depths are limited.

The arrangement of crystalline domains in semicrystalline polymers is key to understanding how to optimize the nanostructured morphology for enabling better properties. For example, in polystyrene-b-poly(ethylene oxide) (PS-b-PEO), the degree of crystallinity and arrangement of the crystallites within the PEO phase plays a crucial role in determining the physical properties of the electrolyte. Here, we used four-dimensional scanning transmission electron microscopy to directly visualize the crystal domains within the PEO-rich region of the PS-b-PEO block copolymer and show the relative angle of the domain with respect to the PEO-PS interface. As demonstrated here, our analysis method is applicable to other electron-beam sensitive materials, especially semicrystalline polymers, to unveil their local phase condition and distribution.

The tensile creep behavior of a vacuum arc-melted Nb45Ta25Ti15Hf15 refractory high entropy alloy was investigated over a constant true stress range of 50–300 MPa at a temperature of 1173 K. Creep tests were carried out in both high vacuum (5 × 10−6 torr) and ultrahigh purity Ar gas to examine the environmental effect. The samples tested in vacuum exhibited power law behavior with a stress exponent of 4.1 and exceptional tensile creep ductility, whereas those tested in Ar suffered significant embrittlement due to HfO2 formation at grain boundaries, which was exacerbated at low applied stresses where extended exposure to residual O2 gas resulted in more extensive brittle intergranular fracture. Phase decomposition occurred after long-term thermal exposure, where a second Hf-rich body-centered cubic phase formed predominantly at grain boundaries but did not cause embrittlement. Compared to the equiatomic TaNbHfZrTi (Senkov alloy) and face-centered cubic multiple-principal element alloys, Nb45Ta25Ti15Hf15 has superior creep resistance, especially at high applied stresses, while maintaining excellent creep ductility. Transmission electron microscopy revealed that creep deformation in Nb45Ta25Ti15Hf15 at 1173 K is controlled by cross-kink collisions from screw dislocations that results in dipole drag at lower strain rates and jog drag at higher strain rates.

Exploratory synthesis has been the main generator of new inorganic materials for decades. However, our Edisonian and bias-prone processes of synthetic exploration alone are no longer sufficient in an age that demands rapid advances in materials development. In this work, we demonstrate an end-to-end attempt towards systematic, computer-aided discovery and laboratory synthesis of inorganic crystalline compounds as a modern alternative to purely exploratory synthesis. Our approach initializes materials discovery campaigns by autonomously mapping the synthetic feasibility of a chemical system using density functional theory with AI feedback. Following expert-driven down-selection of newly generated phases, we use solid-state synthesis and in situ characterization via hot-stage X-ray diffraction in order to realize new ternary oxide phases experimentally. We applied this strategy in six ternary transition-metal oxide chemistries previously considered well-explored, one of which culminated in the discovery of two novel phases of calcium ruthenates. Detailed characterization using room temperature X-ray powder diffraction, 4D-STEM and SQUID measurements identifies the structure and composition and confirms distinct properties, including distinct defect concentrations, of one of the new phases formed in our experimental campaigns. While the discovery of a new material guided by AI and DFT theory represents a milestone, our procedure and results also highlight a number of critical gaps in the process that can inform future efforts towards the improvement of AI-coupled methodologies.

We present a study directly measuring the electron‐beam‐induced plasticity of amorphous Al2O3 coatings. Core–shell nanostructures are employed as small‐scale model systems for two‐dimensional coatings made by atomic layer deposition (ALD). Copper nanowires (NWs) are used as substrates for ALD deposition, representing a model system for interconnects commonly found in integrated circuits. Experiments are performed in situ in a transmission electron microscope (TEM) and further analyzed with electron energy loss spectroscopy (EELS). Our in situ TEM tensile experiments reveal the highly plastic behavior of the ALD shell, which withstands a maximum strain of 188%. Comparable samples under beam‐off conditions show a brittle fracture, which underlines the effect of electron irradiation. The electron‐beam‐activated bond switching within the amorphous network enables compensation of the applied tensile strain, leading to viscous flow. By incorporating an intermediate nanocrystalline layer within the Al2O3 shell, the plasticity is suppressed and brittle fracture occurs. This work directly demonstrates the tuning of mechanical properties in amorphous ALD structures through electron irradiation.

High or enriched-purity O2 is used in numerous industries and is predominantly produced from the cryogenic distillation of air, an extremely capital- and energy-intensive process. There is significant interest in the development of new approaches for O2-selective air separations, including the use of metal-organic frameworks featuring coordinatively unsaturated metal sites that can selectively bind O2 over N2 via electron transfer. However, most of these materials exhibit appreciable and/or reversible O2 uptake only at low temperatures, and their open metal sites are also potential strong binding sites for the water present in air. Here, we study the framework CuI-MFU-4l (CuxZn5-xCl4-x(btdd)3; H2btdd = bis(1H-1,2,3-triazolo[4,5-b],[4',5'-i])dibenzo[1,4]dioxin), which binds O2 reversibly at ambient temperature. We develop an optimized synthesis for the material to access a high density of trigonal pyramidal CuI sites, and we show that this material reversibly captures O2 from air at 25 °C, even in the presence of water. When exposed to air up to 100% relative humidity, CuI-MFU-4l retains a constant O2 capacity over the course of repeated cycling under dynamic breakthrough conditions. While this material simultaneously adsorbs N2, differences in O2 and N2 desorption kinetics allow for the isolation of high-purity O2 (>99%) under relatively mild regeneration conditions. Spectroscopic, magnetic, and computational analyses reveal that O2 binds to the copper(I) sites to form copper(II)-superoxide moieties that exhibit temperature-dependent side-on and end-on binding modes. Overall, these results suggest that CuI-MFU-4l is a promising material for the separation of O2 from ambient air, even without dehumidification.

In a scanning transmission electron microscope (STEM), producing a high-resolution image generally requires an electron beam focused to the smallest point possible. However, the magnetic lenses used to focus the beam are unavoidably imperfect, introducing aberrations that limit resolution. Modern STEMs overcome this by using hardware aberration correctors comprised of many multipole elements, but these devices are complex, expensive, and can be difficult to tune. We demonstrate a design for an electrostatic phase plate that can act as an aberration corrector. The corrector is comprised of annular segments, each of which is an independent two-terminal device that can apply a constant or ramped phase shift to a portion of the electron beam. We show the improvement in image resolution using an electrostatic corrector. Engineering criteria impose that much of the beam within the probe-forming aperture be blocked by support bars, leading to large probe tails for the corrected probe that sample the specimen beyond the central lobe. We also show how this device can be used to create other STEM beam profiles such as vortex beams and probes with a high degree of phase diversity, which improve information transfer in ptychographic reconstructions.

The influence of vacuum arc melting and mechanical processing (wrought) versus additive manufacturing (AM) on the creep behavior of multi-principal element alloys (MPEA) is investigated in this study. Annealed wrought and hot isostatically pressed (HIP) AM CrCoNi were creep tested under constant tensile stress of 40 to 200 MPa at temperatures of 1023 to 1173 K. Stress exponents of 4.5 ± 0.2 and 5.9 ± 0.1 and activation energies ranging from 240 to 259 and 320 to 331 kJ/mol were found for wrought and AM CrCoNi, respectively. The results indicate that the AM material exhibits superior creep resistance and inferior creep ductility compared to the wrought alloy. This difference is attributed to the AM material having a higher percentage of Cr-rich oxides, a smaller total low angle grain boundary (LAGB) length on a percentage basis, and a greater total twin boundary (TB) length on a percentage basis. The AM and wrought materials have similar grain sizes; however, the smaller LAGB length and greater TB length in the AM material reduce slip transmission on the other side of the boundaries and contribute to strength. The dislocation structures of the AM and wrought materials consist of individual curved dislocations with dislocation multijunctions and jogs, which is similar to the arrangements previously observed in CrMnFeCoNi.

An additively manufactured (nominally equiatomic) CrCoNi alloy was processed by laser powder bed fusion (LPBF). At ambient temperatures (298 K), this medium-entropy alloy displayed a yield strength, σy of ∼691 ± 9 MPa, and an ultimate tensile strength, σu of ∼926 ± 15.2 MPa; at cryogenic temperatures (77 K), yield and tensile strengths increased respectively to σy ∼ 944 ± 6 MPa and σu ∼ 1382 ± 11 MPa. These strength levels are 57 and 44% higher than that of the wrought alloy, due to strengthening from the solidification cellular structures intertwined with dislocations in the LPBF CrCoNi. The crack-initiation fracture toughness, KJIc was measured to be ∼183.7 ± 28 MPa√m at 298 K; this value marginally decreased by ∼4% to ∼176 ± 11 MPa√m at 77 K. These KJIc values of the LPBF CrCoNi were 11% and 35% lower than the wrought CrCoNi alloy at 298 K and 77 K, respectively. The resistance to crack growth of the LPBF CrCoNi from its hierarchical micro- and meso‑structures was evaluated using nonlinear-elastic fracture mechanics by measuring R-curve behavior in the form of the J-integral as a function of crack extension. The specific features of the hierarchical microstructures at different length-scales provide a basis for the strengthening and toughening properties of this additively manufactured medium-entropy alloy. This correlation between the deformation and the hierarchical microstructures at different length-scales may provide future guidance for improving the fracture toughness properties of medium-entropy alloys.

Nanobeam electron diffraction can probe local structural properties of complex crystalline materials including phase, orientation, tilt, strain, and polarization. Ideally, each diffraction pattern from a projected area of a few unit cells would produce a clear Bragg diffraction pattern, where the reciprocal lattice vectors can be measured from the spacing of the diffracted spots, and the spot intensities are equal to the square of the structure factor amplitudes. However, many samples are too thick for this simple interpretation of their diffraction patterns, as multiple scattering of the electron beam can produce a highly nonlinear relationship between the spot intensities and the underlying structure. Here, we develop a stacked Bloch wave method to model the diffracted intensities from thick samples with structure that varies along the electron beam. Our method reduces the large parameter space of electron scattering to just a few structural variables per probe position, making it fast enough to apply to very large fields of view. We apply our method to SrTiO3/PbTiO3/SrTiO3 multilayer samples, and successfully disentangle specimen tilt from the mean polarization of the PbTiO3 layers. We elucidate the structure of complex vortex topologies in the PbTiO3 layers, demonstrating the promise of our method to extract material properties from thick samples.

The creep behavior of an additively manufactured (AM) yttrium oxide dispersion strengthened (ODS) CrCoNi multi-principal element alloy (MPEA) is investigated in this study. Tests were conducted over a constant tensile stress range of 40–200 MPa and a temperature range of 973–1173 K. A stress exponent of 6.5 ± 0.1 and activation energies in the range of 335–367 kJ/mol were measured. Compared to its non-ODS counterpart and its parent alloy (CrMnFeCoNi), AM ODS CrCoNi has superior creep resistance at all tested stresses and temperatures. The mechanism contributing to the excellent creep resistance of AM ODS CrCoNi is attributed to the interaction of mixed character dislocations with oxide particles. The creep ductility of AM ODS CrCoNi is higher than its non-ODS counterpart due to a large percentage of low angle grain boundaries associated with its columnar grain structure. It was also found that creep ductility is significantly greater at the highest applied stress of 200 MPa compared to lower stresses. The steady state dislocation structure of AM ODS CrCoNi consists of long arrays of dislocations, which is different from that observed in non-ODS CrCoNi which consists of individual curved dislocations.

In this work, we present a modified simultaneous growth and self-aggregation method that produces ceria and silver Janus nanoparticles for the conversion of 4-nitrophenol, a chemical widely used in several industries. The nanoparticles had cerium-to-silver ratios ranging from 0 to 1.35 and well-defined heterodimer morphologies. By controlling the growth conditions, we have manipulated the interface between ceria and silver, maximizing its exposure to the chemical reactants and increasing the reaction rate constants between 2- and 4-fold. Taken together, these results can inform the design rules to achieve better performing hybrid nanocatalysts.

The extraordinary work hardening ability and fracture toughness of the face-centered cubic (fcc) high-entropy alloys render them ideal candidates for many structural applications. Here, the deformation and failure mechanisms of an equiatomic CrCoNi medium-entropyalloy (MEA) were investigated by powerful laser-driven shock experiments. Multiscale characterization demonstrates that profuse planar defects including stacking faults, nanotwins, and hexagonal nanolamella were generated during shock compression, forming a three-dimensional network. During shock release, the MEA fractured by strong tensile deformation and numerous voids was observed in the vicinity of the fracture plane. High defect populations, nanorecrystallization, and amorphization were found adjacent to these areas of localized deformation. Molecular dynamics simulations corroborate the experimental results and suggest that deformation-induced defects formed before void nucleation govern the geometry of void growth and delay their coalescence. Our results indicate that the CrCoNi-based alloys are impact resistant, damage tolerant, and potentially suitable in applications under extreme conditions.

Improving the mechanical strength of ceramic solid electrolytes such as lithium phosphorus sulfide families for pressure-driven dendrite blocking as well as reducing the electronic conductivity to prevent a dendrite formation inside the electrolytes are very important to extend the lifespan of all-solid-state lithium-metal batteries. Here, we propose a low-temperature solution-precipitation process to prepare polymer-solid electrolyte composites for a highly uniform polymer distribution in the electrolyte to enhance their mechanical strength and reduce their electronic conduction. The composites with up to 12 wt % of polymer are prepared, and the composites exhibit high ionic conductivities of up to 0.3 mS/cm. Furthermore, the electrochemical stability of the electrolyte composites on Li striping/plating cycles is investigated. We confirm that the proposed solution-precipitation process makes the composite much more stable than the bare solid electrolyte and causes them to outperform similar composites from the other existing preparation methods, such as mechanical mixing and solution dispersion.

Vacancies are missing atoms in a crystalline material, and occur both at equilibrium (varying with temperature) and out of equilibrium such as when crystalline materials are damaged with radiation or corrosion. While we know of their importance, particularly regarding diffusive mechanisms, it is not straightforward to experimentally measure their concentration or to visualize them directly. Traditionally, measurements such as positron annihilation spectroscopy and to some degree X-ray diffraction can measure average concentrations, but generally lack the ability to visualize or quantify a heterogenous concentration of vacancies that can occur at the level of individual defects and microstructural features. Here, we present a method to map vacancy concentrations and their distribution using local lattice parameter measurements with a high-resolution electron microscope. Our method utilizes a Au thin film as a model to demonstrate the method via four-dimensional scanning transmission electron microscopy (4D-STEM) by correlating the differences between changes in lattice parameter and the volumetric thermal expansion during in situ heating experiments. The vacancy mapping methodology is also applied to non-equilibrium defects accumulated in pure Al via knock-on electron beam irradiation. Our method demonstrates the ability to map point defect concentrations in heterogeneous systems in situ with nanometer spatial resolution. The result is a technique that can provide direct measurements of vacancy concentrations at the level of individual defects in studies of materials in and out of equilibrium.

Crystalline symmetries have played a central role in the identification and understanding of quantum materials. Here we investigate whether an amorphous analogue of a well known three-dimensional strong topological insulator has topological properties in the solid state. We show that amorphous Bi2Se3 thin films host a number of two-dimensional surface conduction channels. Our angle-resolved photoemission spectroscopy data are consistent with a dispersive two-dimensional surface state that crosses the bulk gap. Spin-resolved photoemission spectroscopy shows this state has an anti-symmetric spin texture, confirming the existence of spin-momentum locked surface states. We discuss these experimental results in light of theoretical photoemission spectra obtained with an amorphous topological insulator tight-binding model, contrasting it with alternative explanations. The discovery of spin-momentum locked surface states in amorphous materials opens a new avenue to characterize amorphous matter, and triggers the search for an overlooked subset of quantum materials outside of current classification schemes.

The microstructure of high-entropy alloys with refractory elements and Al as constituents can be considered to be analogous to superalloys. These so-termed refractory high-entropy superalloys (RHSAs) can show remarkable compressive strength up to temperatures exceeding 1200 °C. Here, we examine the microstructure and properties - compressive, tensile, and fracture toughness - of a precipitation-hardened, body-centered cubic, RHSA, Al0.5Nb1.25Ta1.25TiZr, at ambient temperature (RT) to 1200 °C. Two dual-phase microstructures comprising ordered B2 (brittle) and disordered A2 (ductile) phases were produced in this alloy - one with B2 as the matrix, the other with A2 - for evaluation of the mechanical properties. Under compression, both microstructures display RT compressive strengths above 1.5 GPa and considerable ductility exceeding 40% at elevated temperatures; the alloy with the A2 matrix has ∼15% compressive ductility even at RT. However, properties are very different under tensile loading; at all temperatures, both microstructures fail predominately in an intergranular mode in the elastic regime at a fracture stress less than 200 MPa and ductility below 0.15%. The microstructure with the A2 matrix has a KIc fracture toughness of ∼15 MPa√m at RT, although at all temperatures above 800 °C, measured KIc values for both dual-phase microstructures are less than 5 MPa√m. In this study, we investigate the microstructural origin of these mechanical properties, and emphasize the importance of evaluating these alloys in tension.

Metallic alloys have played essential roles in human civilization due to their balanced strength and ductility. Metastable phases and twins have been introduced to overcome the strength-ductility tradeoff in face-centered cubic (FCC) high-entropy alloys (HEAs). However, there is still a lack of quantifiable mechanisms to predict good combinations of the two mechanical properties. Here we propose a possible mechanism based on the parameter κ, the ratio of short-ranged interactions between closed-pack planes. It promotes the formation of various nanoscale stacking sequences and enhances the work-hardening ability of the alloys. Guided by the theory, we successfully designed HEAs with enhanced strength and ductility compared with other extensively studied CoCrNi-based systems. Our results not only offer a physical picture of the strengthening effects but can also be used as a practical design principle to enhance the strength-ductility synergy in HEAs.

Interstitial oxygen embrittles titanium, particularly at cryogenic temperatures, which necessitates a stringent control of oxygen content in fabricating titanium and its alloys. Here, we propose a structural strategy, via grain refinement, to alleviate this problem. Compared to a coarse-grained counterpart that is extremely brittle at 77 K, the uniform elongation of an ultrafine-grained (UFG) microstructure (grain size ~ 2.0 µm) in Ti-0.3wt.%O is successfully increased by an order of magnitude, maintaining an ultrahigh yield strength inherent to the UFG microstructure. This unique strength-ductility synergy in UFG Ti-0.3wt.%O is achieved via the combined effects of diluted grain boundary segregation of oxygen that helps to improve the grain boundary cohesive energy and enhanced dislocation activities that contribute to the excellent strain hardening ability. The present strategy will not only boost the potential applications of high strength Ti-O alloys at low temperatures, but can also be applied to other alloy systems, where interstitial solution hardening results into an undesirable loss of ductility.

Corrosion is a ubiquitous failure mode of materials. Often, the progression of localized corrosion is accompanied by the evolution of porosity in materials previously reported to be either three-dimensional or two-dimensional. However, using new tools and analysis techniques, we have realized that a more localized form of corrosion, which we call 1D wormhole corrosion, has previously been miscategorized in some situations. Using electron tomography, we show multiple examples of this 1D and percolating morphology. To understand the origin of this mechanism in a Ni-Cr alloy corroded by molten salt, we combined energy-filtered four-dimensional scanning transmission electron microscopy and ab initio density functional theory calculations to develop a vacancy mapping method with nanometer-resolution, identifying a remarkably high vacancy concentration in the diffusion-induced grain boundary migration zone, up to 100 times the equilibrium value at the melting point. Deciphering the origins of 1D corrosion is an important step towards designing structural materials with enhanced corrosion resistance.

CrCoNi-based medium- and high-entropy alloys display outstanding damage tolerance, especially at cryogenic temperatures. In this study, we examined the fracture toughness values of the equiatomic CrCoNi and CrMnFeCoNi alloys at 20 kelvin (K). We found exceptionally high crack-initiation fracture toughnesses of 262 and 459 megapascal-meters½ (MPa·m½) for CrMnFeCoNi and CrCoNi, respectively; CrCoNi displayed a crack-growth toughness exceeding 540 MPa·m½ after 2.25 millimeters of stable cracking. Crack-tip deformation structures at 20 K are quite distinct from those at higher temperatures. They involve nucleation and restricted growth of stacking faults, fine nanotwins, and transformed epsilon martensite, with coherent interfaces that can promote both arrest and transmission of dislocations to generate strength and ductility. We believe that these alloys develop fracture resistance through a progressive synergy of deformation mechanisms, dislocation glide, stacking-fault formation, nanotwinning, and phase transformation, which act in concert to prolong strain hardening that simultaneously elevates strength and ductility, leading to exceptional toughness.

Local chemical ordering (LCO) in the CrCoNi medium-entropy alloy was investigated by transmission electron microscopy (TEM) after different annealing treatments and their corresponding mechanical properties by bulk tensile tests and nanoindentation. A cold-rolled alloy was annealed at 1000°C for 0.5 h followed by ice water quenching and then aged at a number of different temperatures (600°C, 700°C, 800°C, 900°C, and 1000°C) under vacuum for 240 h to generate different degrees of chemical ordering. A splat-quenched sample rapidly cooled from the liquid phase was also examined. While bulk mechanical properties did not vary among samples with equivalent grain sizes, nanoindentation tests revealed notable differences. As indicated by the load at first pop-in using a Berkovich tip or the indentation yield strength via continuous stiffness measurements using a 10 μm spherical tip, the nanoindentation tests revealed that the stress for onset of plasticity during indentation varied with heat treatment and peaked in the 900°C aged sample. Energy-filtered TEM characterization indicated the presence of ordering in all specimens, with a higher degree of LCO in the aged samples relative to the splat-quenched and 1000°C-quenched samples. The evolution of LCO during aging was determined to occur on the time scale similar to those of bulk diffusion. The difference in nanoindentation strength was attributed to the difference in dislocation nucleation barriers imposed by different degrees of LCO.

In ultrafast electron diffraction (UED) experiments, accurate retrieval of time-resolved structural parameters, such as atomic coordinates and thermal displacement parameters, requires an accurate scattering model. Unfortunately, kinematical models are often inaccurate even for relativistic electron probes, especially for dense, oriented single crystals where strong channeling and multiple scattering effects are present. This article introduces and demonstrates dynamical scattering models tailored for quantitative analysis of UED experiments performed on single-crystal films. As a case study, we examine ultrafast laser heating of single-crystal gold films. Comparison of kinematical and dynamical models reveals the strong effects of dynamical scattering within nm-scale films and their dependence on sample topography and probe kinetic energy. Applying to UED experiments on an 11 nm thick film using 750 keV electron probe pulses, the dynamical models provide a tenfold improvement over a comparable kinematical model in matching the measured UED patterns. Also, the retrieved lattice temperature rise is in very good agreement with predictions based on previously measured optical constants of gold, whereas fitting the Debye-Waller factor retrieves values that are more than three times lower. Altogether, these results show the importance of a dynamical scattering theory for quantitative analysis of UED and demonstrate models that can be practically applied to single-crystal materials and heterostructures.