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This article reviews recent basic research on two categories of metal-based nanolaminates: those composed of metal/metal constituents and those composed of metal/ceramic constituents. We focus primarily on studies that aim to understand—via experiments, modeling, or both—the biphase interface structure and its role in changing the mechanisms that govern strength and deformability at a fundamental level. We anticipate that, by providing a broad perspective on the latest advances in nanolaminates, this review will aid design of new metallic materials with unprecedented combinations of mechanical and physical properties.

Two-phase nanolaminates are known for their high strength, yet they suffer from loss of ductility. Here, we show that broadening heterophase interfaces into "3D interfaces" as thick as the individual layers breaks this strength-ductility trade-off. In this work, we use micropillar compression and transmission electron microscopy to examine the processes underlying this breakthrough mechanical performance. The analysis shows that the 3D interfaces stifle flow instability via shear band formation through their interaction with dislocation pileups. To explain this observation, we use phase field dislocation dynamics (PFDD) simulations to study the interaction between a pileup and a 3D interface. Results show that when dislocation pileups fall below a characteristic size relative to the 3D interface thickness, transmission across interfaces becomes significantly frustrated. Our work demonstrates that 3D interfaces attenuate pileup-induced stress concentrations, preventing shear localization and offering an alternative way to enhanced mechanical performance.

This study revealed dual functions of the installed Facac ligands: enhancement of framework mechanical stability due to electrostatic interactions; and weaker capillary forces evaluated from free energies of dehydration during water evacuation.

Metal-ceramic nanocomposites exhibit exceptional mechanical properties with a combination of high strength, toughness, and hardness that are not achievable in monolithic metals or ceramics, which make them valuable for applications in fields such as the aerospace and automotive industries. In this study, interpenetrating nanocomposites of three-dimensionally ordered macroporous (3DOM) tungsten-silicon oxycarbide (W-SiOC) were prepared, and their mechanical properties were investigated. In these nanocomposites, the crystalline tungsten and amorphous silicon oxycarbide phases both form continuous and interpenetrating networks, with some discrete free carbon nanodomains. The W-SiOC material inherits the periodic structure from its 3DOM W matrix, and this periodic structure can be maintained up to 1000 °C. In situ SEM micropillar compression tests demonstrated that the 3DOM W-SiOC material could sustain a maximum average stress of 1.1 GPa, a factor of 22 greater than that of the 3DOM W matrix, resulting in a specific strength of 640 MPa/(Mg/m3) at 30 °C. Deformation behavior of the developed 3DOM nanocomposite in a wide temperature range (30-575 °C) was investigated. The deformation mode of 3DOM W-SiOC exhibited a transition from fracture-dominated deformation at low temperatures to plastic deformation above 425 °C.

Centimetre-scale crack-free metal nanolattices are realized, enabling outstanding high tensile strength in low-density materials.

Nanoindentation provides a convenient and high-throughput means for mapping mechanical properties and for measuring the strain rate sensitivity of a material. Here, nanoindentation was applied to the study of microcrystalline cellulose. Constant strain rate nanoindentation revealed a depth dependence of nanohardness and modulus, mostly attributed to material densification. Nanomechanical maps of storage modulus and hardness resolved the shape and size of voids present in larger particles. In smaller, denser particles, however, where storage modulus varied little spatially, there was still some spatial dependence of hardness, which can be explained by cellulose’s structural anisotropy. Additionally, hardness changed with the indentation strain rate in strain rate jump tests. The resulting strain rate sensitivity values were found to be in agreement with those obtained by other techniques in the literature.

The strength and plasticity of metallic composites is reviewed in terms of (1) hierarchical morphologies in metallic nanocomposites, such as Cu–Mo, Zr–Nb, Al–Si, and (2) heterogeneous interface behavior and compositionally graded interfaces in metallic laminates, such as Cu/bronze, Ti/Al, Fe/Cu, Cu/Nb. Hierarchical architectures of multiple phases with varying sizes and morphologies are particularly effective in enhancing yield strength, due to the strong glide dislocation interactions with their nanoscale features; plastic deformability, due to increased strain hardening from microstructure hierarchy. Enhanced toughening is attributed to impedance of crack growth via deflection along interfaces that have relatively low shear strength and bridging via relatively softer microscale composite domains. In laminates, the constraint from an interface affected zone arising from geometrically necessary dislocations can lead to enhanced strain hardening and plasticity.

s Manipulation of the atomic-scale structure of two-dimensional (2D) interfaces have been shown to provide nanocomposites with enhanced strength, deformability, and radiation damage resistance. In comparison with 2D interfaces, here we investigate the mechanical response of nanocomposites containing three-dimensional (3D) Cu/Nb interfaces consisting of a chemical/structural gradient separating pure Cu and Nb layers, through which the lattice mismatch between face-centered cubic Cu and body-centered cubic Nb is accommodated over a distance of several nanometers. It is demonstrated that 3D interfaces increase the yield and flow strength by 50% and 22%, respectively, over composites containing 2D interfaces at similar layer thicknesses. After 14% compressive strain, the onset of shear banding results in co-deformation of both Cu and Nb phases within and outside of the shear band. We conclude with a discussion of the role of interface structure in shear band formation and growth in 3D Cu/Nb.

Porous metals represent a class of materials where the interplay of ligament length, width, node structure, and local geometry/curvature offers a rich parameter space for the study of critical length scales on mechanical behavior. Colloidal crystal templating of three-dimensionally ordered macroporous (3DOM, i.e., inverse opal) tungsten provides a unique structure to investigate the mechanical behavior at small length scales across the brittle–ductile transition. Micropillar compression tests show failure at 50 MPa contact pressure at 30 °C, implying a ligament yield strength of approximately 6.1 GPa for a structure with 5% relative density. In situ SEM frustum indentation tests with in-plane strain maps perpendicular to loading indicate local compressive strains of approximately 2% at failure at 30 °C. Increased sustained contact pressure is observed at 225 °C, although large (20%) nonlocal strains appear at 125 °C. The elevated-temperature mechanical performance is limited by cracks that initiate on planes of greatest shear under the indenter.

The resistance of stainless steels to shear localization is dependent on processing and microstructure. The amount of research evaluating the shear response of additively manufactured (AM) stainless steels compared to traditionally manufactured ones is limited. To address this gap, experiments were performed on directed energy deposition AM as-built and wrought 316L stainless steel using a forced shear technique with a hat-shaped specimen and a Split-Hopkinson pressure bar. The resulting adiabatic shear bands were characterized with electron backscatter diffraction (EBSD) and nanoindentation to quantify the changes in microstructure and deformation hardening across shear band regions and between the wrought and AM materials. Despite significant differences between the wrought and AM materials including the forced shear response, the postmortem states of work hardening due to the shear band deformation are nearly the same. The maximum nanoindentation stresses occurred in the shear band center with similar magnitudes and only minor differences away from the shear band. Although EBSD data cannot be resolved in the shear band center, misorientation trends, particularly grain reference orientation deviation, were found to closely resemble nanoindentation trends. The combination of EBSD misorientation and nanoindentation, which are linked through changes in dislocation density, is a viable protocol to quantify local changes to macroscopically applied deformation.

Development of structural materials for service under extreme conditions is slowed by the lack of high-throughput test protocols. Here, a method that integrates high-throughput nanoindentation mapping with precise temperature control under a vacuum atmosphere is demonstrated. High-entropy alloys (HEAs) may possess the strength and stability required of high-temperature structural materials in next-generation nuclear applications. These alloys, including the compositional variation AlxFeCrNiMn (x = 0, 0.3, 1) presented in this work, have distinct microstructural morphologies, and nanoindentation mapping reveals the mechanical behavior of the distinct phases as a function of temperature up to 400°C. FeCrNiMn (Al = 0) consists of a face-centered cubic (FCC) matrix with body-centered cubic (BCC) precipitates and exhibits significant softening in both phases at elevated temperature. In contrast, both the FCC phase and FCC–BCC phases present in Al0.3FeCrNiMn show approximately 90% retention of the room temperature hardness at 400°C, and AlFeCrNiMn with BCC and B2 structures shows a similar 85% retention of hardness.

The mechanical properties of multilayer films consisting of alternating layers of magnesium and niobium are investigated through micropillar compression experiments across a broad range of temperatures. The data collected from the variable temperature micropillar compression tests and strain rate jump tests are used to gain insight into the operative deformation mechanisms within the material. At higher temperatures, diffusion-based deformation mechanisms are shown to determine the plastic behavior of the multilayers. Diffusion occurs more readily along the magnesium–niobium interface than within the bulk, acting as pathway for magnesium diffusion. When individual layer thicknesses are sufficiently small, diffusion can remain the dominant deformation mechanism down to room temperature. Multilayer strengthening models historically rely solely on dislocation-based arguments; therefore, consideration of diffusion-based deformation in nanolaminates with low melting temperature components offers improved understanding of multilayer behavior. acceptedVersion

Nanostructured ferritic alloys (NFAs) having sub-micron grain size with a high density of nano-oxides (NOs) (size of ∼2–3 nm) are one of the best candidates for structural components in Generation IV nuclear systems. In this study, 14YWT NFA cladding tubes were irradiated in BOR60 reactor up to 7 dpa at 360–370 °C. Detailed microstructural analysis has been conducted using bright field transmission electron microscopy, bright field scanning transmission electron microscopy, energy filtered transmission electron microscopy, energy dispersive X-ray spectroscopy, electron energy loss spectroscopy and transmission Kikuchi diffraction techniques. This revealed cavities, and type dislocation loops, and α′ precipitates forming after irradiation with relationships between cavities and NOs, and α′ precipitates and NOs. Cavities mostly form on the NOs; whereas, α′ precipitates form between the NOs where the point defect concentration is high. Moreover, α′ precipitates are distributed homogenously on and around the dislocation loops which is consistent with the observation that there is no Cr segregation on dislocation loops. Grain boundaries were found to be mostly depleted in Cr; however, the characteristics of each grain boundary determines the Cr behavior and the α′ denuded zone around the grain boundaries. Mechanical properties of the irradiated tubes have been determined by using both low force and high force nanoindentation techniques, resulting in 1.03 ± 0.33 GPa and 0.82 ± 0.20 GPa hardening, respectively. Dispersed barrier hardening calculations and nanoindentation measurements are in good agreement. In this study, 14YWT NFA has been systematically studied after neutron irradiation to better understand its superior performance: low α′ concentration, low swelling and low radiation-induced hardening.

Mg/Nb nanolaminates synthesized through vapor deposition techniques exhibit high flow strength without conventional twinning in Mg. In this work, we investigated the influence of laminated microstructures on deformation mechanisms of Mg nanolayers. Using molecular dynamics simulations, we explored that (0001)-oriented Mg layers transform or re-orient to {10 $$ \bar{1} $$ 0}-oriented Mg layers through nucleation and growth of {10 $$ \bar{1} $$ 2} twins by atomic shuffling, instead of conventional {10 $$ \bar{1} $$ 2} twinning shear. Such a reorientation accommodates in-plane compressive strain and out-of-plane tensile strain when Mg/Nb laminates are subjected to compression parallel to the Mg/Nb interfaces. The nucleation of {10 $$ \bar{1} $$ 2} twins is promoted at the Mg/Nb interface due to the structural change associated with the glide of interface dislocations. The growth of {10 $$ \bar{1} $$ 2} twins is accomplished through migration of basal–prismatic boundaries via nucleation and glide of one-layer and two-layer disconnections associated with atomic shuffling. The results shed light on improving mechanical properties of hexagonal close-packed metals employing laminated structures.

Metal-organic framework (MOF) materials have shown promise in many applications, ranging from gas storage to absorption and catalysis. Because of the high porosity and low density of many MOFs, densification methods such as pelletization and extrusion are needed for practical use and for commercialization of MOF materials. Therefore, it is important to elucidate the mechanical properties of MOFs and to develop methods of further enhancing their mechanical strength. Here, we demonstrate the influence of phase purity and the presence of a pore-reinforcing component on elastic modulus and yield stress of NU-1000 MOFs through nanoindentation methods and finite element simulation. Three types of NU-1000 single crystals were compared: phase-pure NU-1000 prepared with biphenyl-4-carboxylic acid as a modulator (NU-1000-bip), NU-1000 prepared with benzoic acid as a modulator (NU-1000-ben), which results in an additional, denser impurity phase of NU-901, and NU-1000-bip whose mesopores were infiltrated with silica (SiOx(OH)y@NU-1000) by nanocasting methods. By maintaining phase purity and minimizing defects, the elastic modulus could be enhanced by nearly an order of magnitude: phase-pure NU-1000-bip crystals exhibited an elastic modulus of 21 GPa, whereas the value for NU-1000-ben crystals was only 3 GPa. The introduction of silica into the mesopores of NU-1000-bip did not strongly affect the measured elastic modulus (19 GPa) but significantly increased the load at failure from 2000 μN to 3000-4000 μN.

Grain boundaries play an important role in the overall mechanical performance of metals and alloys; however, isolating the effects of individual grain boundaries remains rather challenging experimentally. In this work, wire-feed, electron beam additively manufactured tantalum is studied under shock loading conditions generating incipient spall damage. Three grain boundaries aligned parallel to the shock direction were isolated inside a single sample. Postmortem metallography showed voids preferentially appeared on two of the three grain boundaries which had high misorientation angles > 30° compared to the third grain boundary with a relatively lower misorientation angle

Heavy ion irradiation was performed on coarse and nanocrystalline-grained tungsten (CGW and NGW, respectively) at room temperature (RT) and 1050 K from 0.25 to 4 dpa to simulate radiation damage for fusion energy applications. TEM and nanohardness measurements of irradiated samples were made to quantify the radiation tolerance of these two candidate materials. In this case, TEM is used to quantify the defect morphology at low dpa values and determine the barrier strength coefficients of the different defects using the dispersed barrier hardening (DBH) model. Nanohardness measurements and the determined barrier strength coefficients are then used to estimate the defect morphologies at higher dpa values where quantification with TEM is not reliable. Quantification of the damage at low dpa (0.25 dpa) showed different loop (at RT and 1050 K) and void (at 1050 K) densities and sizes for the two grain sizes. Nanohardness measurements performed on the samples showed a very small change in hardness for RT ion irradiation and a higher but more scattered increase in hardness for 1050 K ion irradiation. Using the Dispersed barrier hardening (DBH) model and the average loop/void density and size, the dislocation barrier (α values) values were shown to be very small (0.003 and 0.03 for the CGW and NCW respectively) for loop damage and of weak to moderate strength (0.13 for NCW and CGW) for void damage. The small barrier strength values for fine grained materials and the limitations of using nanohardness measurements with the DBH model to characterize irradiation damage are discussed.

Here we seek to probe and understand the mechanical behavior of grain boundaries in pure Ta as a model bcc material using micropillar compression experiments. Three high angle grain boundaries are chosen with varying crystal orientations. Multiple bi-crystal pillars are prepared containing a single, nearly vertical grain boundary in the approximate center of the pillar and compared against their single crystalline pillar counterparts. The main phenomenon of interest was slip transmission or strain transfer in the bi-crystals which was considered to occur when slip traces aligned across the grain boundary. This occurred in two of the three bi-crystals. These observations were compared against two slip transmission factors, m ' = cos ( ψ ) cos ( κ ) and L R B = cos ( θ ) cos ( κ ) , where ψ , θ , a n d κ are the angles between the slip vectors, slip plane normals, and the intersection of the slip planes with the grain boundary from the slip systems on either side of the grain boundary. Additionally, transmission was compared against the stress-strain response and overall deformation (i.e., sheared boundary) of the bi-crystal. The transmission factors exhibited a consistent behavior with slip transmission occurring for high transmission factors and not occurring for low transmission factors. For example, slip transmission occurred for m ' ≥ 0.85 and did not occur for m ' ≤ 0.46. The engineering stress-strain response and overall deformation behavior did not show correlations with the presence or absence of slip transmission. High angle boundaries in bcc metals are shown to represent a diverse set of responses in bi-crystalline micropillar compression experiments.

In this work, the deformation mechanisms underlying the room temperature deformation of the pseudomorphic body centered cubic (BCC) Mg phase in Mg/Nb nanolayered composites are studied. Nanolayered composites comprised of 50% volume fraction of Mg and Nb were synthesized using physical vapor deposition with the individual layer thicknesses h of 5, 6.7, and 50 nm. At the lower layer thicknesses of h = 5 and 6.7 nm, Mg has undergone a phase transition from HCP to BCC such that it formed a coherent interface with the adjoining Nb phase. Micropillar compression testing normal and parallel to the interface plane shows that the BCC Mg nanolayered composite is much stronger and can sustain higher strains to failure than the HCP Mg nanolayered composite. A crystal plasticity model incorporating confined layer slip is presented and applied to link the observed anisotropy and hardening in the deformation response to the underlying slip mechanisms.

A large percentage of molecular compounds can crystallize in different hydration states. Although hydrated and anhydrous crystal forms can exhibit different physical properties (e.g., solubility, stability, mechanical strength), establishing the contribution water makes to the properties can be elusive. Anhydrous (UA) and dihydrate (UAD) crystal forms of uric acid share a remarkably similar two-dimensional layer structure, though the presence or absence of water between the layers imparts these crystal forms with dramatically different mechanical properties. The quantitative and qualitative differences in how these two materials respond to uniaxial stress were investigated with nanoindentation and atomic force microscopy (AFM) imaging normal to the layer direction. Overall, UA was found to be both substantially harder and more brittle than UAD. Load–displacement curves and AFM images of the UA crystal surface postindent reveal slip planes in preferred crystallographic directions and oriented crack formati...

FeCrAl ferritic alloys are excellent cladding candidates for accident tolerant fuel systems due to their high resistance to oxidation as a result of formation of a protective Al2O3 scale at high temperatures in steam. In this study, we report the irradiation response of the 10Cr and 13Cr FeCrAl cladding tubes under Fe2+ ion irradiation up to ∼16 dpa at 300 °C. Dislocation loop size, density and characteristics were determined using both two-beam bright field transmission electron microscopy and on-zone scanning transmission electron microscopy techniques. 10Cr (C06M2) tube has a lower dislocation density, larger grain size and a slightly weaker texture compared to the 13Cr (C36M3) tube before irradiation. After irradiation to 0.7 dpa and 16 dpa, the fraction of type sessile dislocations decreases with increasing Cr amount in the alloys. It has been found that there is neither void formation nor α′ precipitation as a result of ion irradiations in either alloy. Therefore, dislocation loops were determined to be the only irradiation induced defects contributing to the hardening. Nanoindentation testing before the irradiation revealed that the average nanohardness of the C36M3 tube is higher than that of the C06M2 tube. The average nanohardness of irradiated tube samples saturated at 1.6–2.0 GPa hardening for both tubes between ∼3.4 dpa and ∼16 dpa. The hardening calculated based on transmission electron microscopy was found to be consistent with nanohardness measurements.

Split-Hopkinson pressure bar dynamic compression experiments were conducted to determine the defect/interface interaction dependence on interface type, bilayer thickness and interface orientation with respect to the loading direction in the Ag-Cu eutectic system. Specifically, the deformation microstructure in alloys with either a cube-on-cube orientation relationship with { 111 } Ag || { 111 } Cu interface habit planes or a twin orientation relationship with { 3 13 } Ag || { 1 12 } Cu interface habit planes and with bilayer thicknesses of 500 nm, 1.1 µm and 2.2 µm were probed using TEM. The deformation was carried by dislocation slip and in certain conditions, deformation twinning. The twinning response was dependent on loading orientation with respect to the interface plane, bilayer thickness, and interface type. Twinning was only observed when loading at orientations away from the growth direction and decreased in prevalence with decreasing bilayer thickness. Twinning in Cu was dependent on twinning partial dislocations being transmitted from Ag, which only occurred for cube-on-cube interfaces. Dislocation slip and deformation twin transfer across the interfaces is discussed in terms of the slip transfer conditions developed for grain boundaries in FCC alloys.

Accumulative roll bonded (ARB) Copper Niobium (Cu-Nb) nano-lamellar composite (NLC) panels were friction stir welded (FSWed) to evaluate the ability to join panels while retaining the nano-lamellar structure. During a single pass of the friction stir welding (FSW) process, the nano-lamellar structure of the parent material (PM) was retained but was observed to fragment into equiaxed grains during the second pass. FSW has been modeled as a severe deformation process in which the material is subjected to an instantaneous high shear strain rate followed by extreme shear strains. The loss of the nano-lamellar layers was attributed to the increased strain and longer time at temperature resulting from the second pass of the FSW process. Kinematic modeling was used to predict the global average shear strain and shear strain rates experienced by the ARB material during the FSW process. The results of this study indicate that through careful selection of FSW parameters, the nano-lamellar structure and its associated higher strength can be maintained using FSW to join ARB NLC panels.

Al/SiC nanolaminates with equal nominal thicknesses of the Al and SiC layers (10, 25, 50 and 100 nm) were manufactured by magnetron sputtering. The mechanical properties were measured at 25 °C and 100 °C by means of nanoindentation and micropillar compression tests and the deformation mechanisms were analyzed by in situ micropillar compression tests in the transmission electron microscope. In addition, finite element simulations of both tests were carried out to ascertain the role played by the strength of the Al layers and by the elastic constraint of the ceramic layers on the plastic flow of Al in the mechanical response. It was found that the mechanical response was mainly controlled by the constraint during nanoindentation or micropillar compression tests of very thin layered (≈10 nm) laminates, while the influence of the strength of Al layers was not as critical. This behavior was reversed, however, for thick layered laminates (100 nm). These mechanisms point to the different effects of layer thickness during nanoindentation and micropillar compression, at both temperatures, and showed the critical role played by constraint on the mechanical response of nanolaminates made of materials with a very large difference in the elasto-plastic properties.

Mathematical models suggest that the strain along the film formed by parallel passes of a nanoindentation probe in contact with the film can be either homogenous or heterogeneous, depending on contact pressure and spacing between passes. In this study, a 1 µm copper thin film was worn with a cono-spherical diamond probe with normal loads ranging from 25 to 800 µN and wear box edge lengths of 40, 60, and 80 µm. The nanoindenter counterface was rastered across the surface to mimic dry sliding wear. To determine potential strain field changes, 10-step quasi-static indents (200–2000 µN) were performed using nanoindentation inside the wear boxes created at various loads to determine if a strain field alteration could be observed in changes in hardness of the copper thin film. It was shown that there was a softening effect in the hardness for normal loads

The heavy-ion irradiation behavior of bulk zirconium-niobium multilayered composites was investigated up to large doses. Multilayers with an average individual layer thicknesses ranging between 15 and 80 nm were synthesized by accumulative roll bonding technique. The irradiation was performed with a defocused 7 MeV Zr2+ ion beam at 500 °C. The maximum dose achieved was ∼145 dpa at the depth of ∼1.5 μm from the irradiated surface. Sub-surface microstructural damage and the chemical redistribution were characterized by transmission electron microscopy and energy dispersive spectroscopy, respectively. Irrespective of the layer thicknesses, the irradiation condition caused layer instability and the extent of damage varied with the dose levels. Doses lesser than ∼60 dpa caused layer fragmentation and greater than ∼60 dpa resulted in layer dissolution. The chemical mixing of layers occur to a depth of ∼1 μm, consuming multiple bi-layer periods. Despite the elevated irradiation temperature (500 °C) and a slightly positive heat of mixing (+6 kJ/mol), no phase separation was observed and single-phase was retained in the mixed region. The results demonstrate that chemical mixing was facilitated by the liquid phase miscibility of Zr and Nb, which propelled the interdiffusion within the thermal spikes towards mixing.

We report phenomenal yield strengths—up to one-fourth of the theoretical strength of silver—recorded in microcompression testing of initially dislocation-free silver micro- and nanocubes synthesized from a multistep seed-growth process. These high strengths and the massive strain bursts that occur upon yield are results of the initially dislocation-free single-crystal structure of the pristine samples that yield through spontaneous nucleation of dislocations. When the pristine samples are exposed to a focused ion-beam to fabricate pillars and then compressed, the dramatic strain burst does not occur, and they yield at a quarter of the strength compared to the pristine counterparts. Regardless of the defect-state of the samples prior to testing, a size effect is apparent—where the yield strength increases as the sample size decreases. Since dislocation starvation and the single-arm-source mechanisms cannot explain a size effect on yield strength in dislocation-free samples, we investigate the dislocation nucleation mechanisms controlling the size effect through careful experimental observations and molecular statics simulations. We find that intrinsic or extrinsic symmetry breakers such as surface defects, edge roundness, external sample shape, or a high vacancy concentration can influence dislocation nucleation, and thus contribute to the size effect on yield strength in initially dislocation-free samples.

Recent advances in spherical nanoindentation protocols have proven very useful for capturing the grain-scale mechanical response of different metals. This is achieved by converting the load–displacement response into an effective indentation stress–strain response which reveals latent information such as the elastic–plastic transition or indentation yield strength and work-hardening behavior and subsequently correlating the response with the material structure (e.g., crystal orientation) at the indentation site. Using these protocols, we systematically study and quantify the microscale mechanical effects of He, W, and He + W ion irradiation on commercially pure, polycrystalline tungsten. The indentation stress–strain response is correlated with the crystal orientation from electron backscatter diffraction, the defect structure from transmission electron microscopy micrographs, and the stopping range of ions in matter calculations of displacement damage and He concentration. He-implanted grains show a much higher indentation yield strength and saturation stress compared to W-ion-irradiated grains for the same displacement damage. There is also good agreement between the dispersed barrier hardening model with a barrier strength of 0.5–0.8 and void models (Bacon–Kochs–Scattergood and Osetsky–Bacon models) with the experimentally observed changes in indentation strength due to the presence of He bubbles. This finding indicates that a high density (~ 9 × 1023 m−3) and concentration (~ 1.5 at.%) of small (~ 1 nm diameter) He bubbles can be moderate to strong barriers to dislocation slip in tungsten.

Three methods were used to measure the mechanical properties of $${\text{U}}_{3}{\text{Si}}$$ , $${\text{U}}_3{\text{Si}}_{2}$$ , and USi. Quasi-static and continuous stiffness measurement nanoindentation were used to determine hardness and Young’s modulus, and microindentation was used to evaluate the bulk hardness. Hardness and Young’s modulus of the three U-Si compounds were both observed to increase with Si content. Finally, finite elements modelling was used to validate the nanoindentation data calculated for $${\text{U}}_{3}{\text{Si}}_{2}$$ and estimate its yield strength.

Mechanical properties of thin films are often obtained solely from nanoindentation. At the same time, such measurements are characterized by a substantial amount of uncertainty, especially when mean pressure or hardness are used to infer uniaxial yield stress. In this work we demonstrate that indentation with a pyramidal flat tip (frustum) indenter near the free edge of a sample can provide a significantly better estimate of the uniaxial yield strength compared to frequently used Berkovich indenter. This is first demonstrated using a numerical model for a material with an isotropic pressure sensitive yield criterion. Numerical simulations confirm that the indenter geometry provides a clear distinction of the mean pressure at which a material transitions to inelastic behavior. The mean critical pressure is highly dependent on the plastic Poisson ratio ν p so that at the 1% offset of normalized indent depth, the critical pressure p m c normalized to the uniaxial yield strength σ 0 is 1 m c /σ 0 0 ν p 0.5 . Choice of a frustum over Berkovich indenter reduces uncertainty in hardness by a factor of 3. These results are used to interpret frustum indentation experiments on nanoporous (NP) Copper with struts of typical diameter of 45 nm. An estimate of the yield strength of NP Copper is obtained 230 MPa σ 0 300 MPa. Edge indentation further allows one to obtain in-plane strain maps near the critical pressure. Comparison of the experimentally obtained in-plane strain maps of NP Cu during deformation and the strain field for different plastic Poisson ratios suggest that this material has a plastic Poisson ratio of the order of 0.2–0.3. However, existing constitutive models may not adequately capture post-yield behavior of NP metals.

The mechanisms of strain transfer across Ag/Cu interfaces were determined by a combination of in situ and ex situ TEM straining experiments and molecular dynamics simulations. Minimizing the magnitude of the Burgers vector of the residual dislocation generated in the interface was the dominant factor for determining the outcome of dislocation and deformation twin interactions with both non-coherent twin and cube-on-cube interfaces. This included the unexpected finding, due to the loading condition, of deformation twin activation in the Cu layer due to the intersection of deformation twins in Ag with the interface. Deformation twin nucleation in Ag from the non-coherent twin interfaces was also explained by a Burgers vector minimization argument.

We summarize recent work on helium (He) interaction with various heterophase boundaries under high temperature irradiation. We categorize the ion-affected material beneath the He-implanted surface into three regions of depth, based on the He/vacancy ratio. The differing defect structures in these three regions lead to the distinct temperature sensitivity of He-induced microstructure evolution. The effect of He bubbles or voids on material mechanical performance is explored. Overall design guidelines for developing materials where He-induced damage can be mitigated in materials are discussed.

Experimentally quantifying the mechanical effects of radiation damage in reactor materials is necessary for the development and qualification of new materials for improved performance and safety. This can be achieved in a high-throughput fashion through a combination of ion beam irradiation and small scale mechanical testing in contrast to the high cost and laborious nature of bulk testing of reactor irradiated samples. The current work focuses on using spherical nanoindentation stress-strain curves on unirradiated and proton irradiated (10 dpa at 360 °C) 304 stainless steel to quantify the mechanical effects of radiation damage. Spherical nanoindentation stress-strain measurements show a radiation-induced increase in indentation yield strength from 1.36 GPa to 2.72 GPa and a radiation-induced increase in indentation work hardening rate of 10 GPa–30 GPa. These measurements are critically compared against Berkovich nanohardness, micropillar compression, and micro-tension measurements on the same material and similar grain orientations. The ratio of irradiated to unirradiated yield strength increases by a similar factor of 2 when measured via spherical nanoindentation or Berkovich nanohardness testing. A comparison of spherical indentation stress-strain curves to uniaxial (micropillar and micro-tension) stress-strain curves was achieved using a simple scaling relationship which shows good agreement for the unirradiated condition and poor agreement in post-yield behavior for the irradiated condition. The disagreement between spherical nanoindentation and uniaxial stress-strain curves is likely due to the plastic instability that occurs during uniaxial tests but is absent during spherical nanoindentation tests.

Basal slip and { 01 1 ¯ 2 } twinning are two major plastic deformation mechanisms in hexagonal closed-packed magnesium. Here we quantify the critical stresses associated with basal slip and twinning in single-crystal and bi-crystal magnesium samples by performing in situ compression of micropillars with different diameters in a scanning electron microscope. The micropillars are designed to favor either slip or twinning under uniaxial compression. Compression tests imply a negligible size effect related to basal slip and twinning as pillar diameter is greater than 10 μm. The critical resolved shear stresses are deduced to be 29 MPa for twinning and 6 MPa for basal slip from a series of micropillar compression tests. Employing full-field elasto-visco-plastic simulations, we further interpret the experimental observations in terms of the local stress distribution associated with multiple twinning, twin nucleation, and twin growth. Our simulation results suggest that the twinning features being studied should not be close to the top surface of the micropillar because of local stress perturbations induced by the hard indenter.

Kink band formation is a common deformation mode for anisotropic materials and has been observed in polymer matrix fiber composites, single crystals, geological formations, and recently in metallic nanolaminates. While numerous studies have been devoted to kink band formation, the majority do not consider the often rapid and unstable process of kink band propagation. Here we take advantage of stable kink band formation in Cu-Nb nanolaminates to quantitatively map the local strain fields surrounding a propagating kink band during uniaxial compression. Kink bands are observed to initiate at specimen edges, propagate across the sample during a rising global stress, and induce extended strain fields in the non-kinked material surrounding the propagating kink band. It is proposed that these stress/strain fields significantly contribute to the total energy dissipated during kinking and, analogous to crack tip stress/strain fields, influence the direction of kink propagation and therefore the kink band inclination angle.

Low elastic modulus and hardness, as well as anomalous indentation behavior, have been observed during indentation of xenotime rare-earth orthophosphate ceramics (REPO4s) with compositions near the monazite/xenotime phase boundary. Pressure-induced phase transformation has been identified as a potential cause for both observations. This study comprehensively characterizes the mechanical properties and indentation behavior of four elemental REPO4 materials (EuPO4, GdPO4, TbPO4, and DyPO4) that span the monazite/xenotime phase boundary using ex situ nanoindentation for a range of loading rates and indentation depths. In situ nanoindentation within a SEM was used to correlate discrete load-depth behavior to the development of surface features. Anomalous, elbow-type behavior was not restricted to xenotimes, but occurred in all four materials; thus we concluded that the presence of an elbow in the indentation data was not a unique identifier of phase transformation in rare-earth orthophosphates. Furthermore, it was shown that the elastic modulus of each of these compositions approached the value predicted by simulations and hardness was consistently above 5 GPa, provided that the samples were processed to nearly full density.

Interface engineering is an important strategy for developing radiation tolerant materials. In prior work, bulk nanolayered composites fabricated by accumulative roll bonding (ARB) showed outstanding radiation resistance. However, the effects of layer thickness and radiation conditions on damage distributions and their effect on hardness have not been explored. Here, we use transmission electron microscopy (TEM) and nanoindentation to investigate the effects of radiation on the distribution of radiation-induced cavities and post-radiation hardness in ARB nanolayered Cu-Nb composites. We show that whether the cavities cross the interface depends on layer thickness and temperature, and that, remarkably, radiation could generate softening, not always hardening. We posit that the softening mainly results from the recovery of dislocations stored in the crystal after the bulk forming ARB processing due to He radiation and this phenomenon offsets radiation-induced hardening as layers become finer and temperatures rise.

The role of heterogeneous interfaces in improving mechanical properties of polycrystalline aggregates and laminated composites has been well recognized with interface structure being of fundamental importance in designing composites containing multiple interfaces. In this paper, taking the Mg (hexagonal close-packed (hcp))/Nb (body-centered cubic (bcc)) interface as an example, we develop Mg-Nb interatomic potentials for predicting atomic configurations of Mg/Nb interfaces. We systematically characterize interface dislocations of Mg/Nb interfaces with Nishiyama-Wassermann (NW) and Kurdjumov-Sachs (KS) orientation relationships and propose a generalized procedure of characterizing interface structure by combining atomistic simulation and interface dislocation theory, which is applicable for not only hcp/bcc interfaces, but also other systems with complicated interface dislocation configurations. In Mg/Nb, interface dislocation networks of two types of interfaces are significantly different although they originate from partial dislocations of similar character: the NW interface is composed of three sets of partial dislocations, while the KS interface is composed of four sets of interface dislocations - three sets of partial dislocations and one set of full dislocations that forms from the reaction of two close partial dislocations.