Evolution of dislocation substructures in metals via high-strain-rate nanoindentation.

Deformation at high strain rates often results in high stresses on many engineering materials, potentially leading to catastrophic failure without proper design. High-strain-rate mechanical testing is thus needed to improve the design of future structural materials for a wide range of applications. Although several high-strain-rate mechanical testing techniques have been developed to provide a fundamental understanding of material responses and microstructural evolution under high-strain-rate deformation conditions, these tests are often very time consuming and costly. In this work, we utilize a high-strain-rate nanoindentation testing technique and system in combination with transmission electron microscopy to reveal the deformation mechanisms and dislocation substructures that evolve in pure metals from low (10-2 s-1) to very high indentation strain rates (104 s-1), using face-centered cubic aluminum and body-centered cubic molybdenum as model materials. The results help to establish the conditions under which micro- and macro-scale tests can be compared with validity and also provide a promising pathway that could lead to accelerated high-strain-rate testing at substantially reduced costs.

A reference-area-free strain mapping method using precession electron diffraction data.

In this work, we developed a method using precession electron diffraction data to map the residual elastic strain at the nano-scale. The diffraction pattern of each pixel was first collected and denoised. Template matching was then applied using the center spot as the mask to identify the positions of the diffraction disks. Statistics of distances between the selected diffracted disks enable the user to make an informed decision on the reference and to generate strain maps. Strain mapping on an unstrained single crystal sapphire shows the standard deviation of strain measurement is 0.5%. With this method, we were able to successfully measure and map the residual elastic strain in VO2 on sapphire and martensite in a Ni50.3Ti29.7Hf20 shape memory alloy. This approach does not require the user to select a "strain-free area" as a reference and can work on datasets even with the crystals oriented away from zone axes. This method is expected to provide a robust and more accessible alternative means of studying the residual strain of various material systems that complements the existing algorithms for strain mapping.

Strong yet ductile nanolamellar high-entropy alloys by additive manufacturing.

Additive manufacturing produces net-shaped components layer by layer for engineering applications1-7. The additive manufacture of metal alloys by laser powder bed fusion (L-PBF) involves large temperature gradients and rapid cooling2,6, which enables microstructural refinement at the nanoscale to achieve high strength. However, high-strength nanostructured alloys produced by laser additive manufacturing often have limited ductility3. Here we use L-PBF to print dual-phase nanolamellar high-entropy alloys (HEAs) of AlCoCrFeNi2.1 that exhibit a combination of a high yield strength of about 1.3 gigapascals and a large uniform elongation of about 14 per cent, which surpasses those of other state-of-the-art additively manufactured metal alloys. The high yield strength stems from the strong strengthening effects of the dual-phase structures that consist of alternating face-centred cubic and body-centred cubic nanolamellae; the body-centred cubic nanolamellae exhibit higher strengths and higher hardening rates than the face-centred cubic nanolamellae. The large tensile ductility arises owing to the high work-hardening capability of the as-printed hierarchical microstructures in the form of dual-phase nanolamellae embedded in microscale eutectic colonies, which have nearly random orientations to promote isotropic mechanical properties. The mechanistic insights into the deformation behaviour of additively manufactured HEAs have broad implications for the development of hierarchical, dual- and multi-phase, nanostructured alloys with exceptional mechanical properties.

Twin boundary migration mechanisms in quasi-statically compressed and plate-impacted Mg single crystals.

Twinning is a prominent deformation mode that accommodates plasticity in many materials. This study elucidates the role of deformation rate on the atomic-scale mechanisms that govern twin boundary migration. Examination of Mg single crystals deformed under quasi-static compression was compared with crystals deformed via plate impact. Evidence of two mechanisms was uncovered. Atomic-level observations using high-resolution transmission electron microscopy revealed that twin boundaries in the -axis quasi-statically compressed single crystals are relatively smooth. At these modest stresses and rates, the twin boundaries were found to migrate predominantly via shear (i.e., disconnection nucleation and propagation). By contrast, in the plate-impacted crystals, which are subjected to higher stresses and rates, twin boundary migration was facilitated by local atomic shuffling and rearrangement, resulting in rumpled twin boundaries. This rate dependency also leads to marked variations in twin variant, size, and number density in Mg. Analogous effects are anticipated in other hexagonal closed-packed crystals.

Exploring the origins of the indentation size effect at submicron scales.

The origin of the indentation size effect has been extensively researched over the last three decades, following the establishment of nanoindentation as a broadly used small-scale mechanical testing technique that enables hardness measurements at submicrometer scales. However, a mechanistic understanding of the indentation size effect based on direct experimental observations at the dislocation level remains limited due to difficulties in observing and quantifying the dislocation structures that form underneath indents using conventional microscopy techniques. Here, we employ precession electron beam diffraction microscopy to "look beneath the surface," revealing the dislocation characteristics (e.g., distribution and total length) as a function of indentation depth for a single crystal of nickel. At smaller depths, individual dislocation lines can be resolved, and the dislocation distribution is quite diffuse. The indentation size effect deviates from the Nix-Gao model and is controlled by dislocation source starvation, as the dislocations are very mobile and glide away from the indented zone, leaving behind a relatively low dislocation density in the plastically deformed volume. At larger depths, dislocations become highly entangled and self-arrange to form subgrain boundaries. In this depth range, the Nix-Gao model provides a rational description because the entanglements and subgrain boundaries effectively confine dislocation movement to a small hemispherical volume beneath the contact impression, leading to dislocation interaction hardening. The work highlights the critical role of dislocation structural development in the small-scale mechanistic transition in indentation size effect and its importance in understanding the plastic deformation of materials at the submicron scale.

Understanding of Lithium Insertion into 3D Porous Carbon Scaffolds with Hybridized Lithiophobic and Lithiophilic Surfaces by In-Operando Study.

In-operando study coupled with voltage/current profiles are presented in order to unveil lithium insertion processes into 3D porous carbon nanotube (CNT) structures whose surfaces were altered to have lithiophobic, lithiophilic, and hybridized lithiophobic/philic characteristics using graphitic surfaces with/without carboxyl/hydroxyl groups. We found the lithiophobic graphitic surfaces hindered lithium insertion into the scaffold despite the high conductivity of CNT. The lithiophilic surface caused another problem of lithium deposition on the outer surface of the electrode, clogging pores and engendering dendrites. Conversely, in the hybridized CNT, lithiophilic trenches partially created on the pristine CNT allowed for uniform lithium deposition into the pores by simultaneously improved lithium attraction and charge transfer, reaching a high areal capacity of 16 mAh cm-2 even with a current density of 8 mA cm-2 without noticeable dendrite formation and volume expansion. Our hybridization approach provides valuable insight to realize a high-energy-density anode by uniformly impregnating lithium into porous media.

Tuning the deformation mechanisms of boron carbide via silicon doping.

Boron carbide suffers from a loss of strength and toughness when subjected to high shear stresses due to amorphization. Here, we report that a small amount of Si doping (~1 atomic %) leads to a substantial decrease in stress-induced amorphization due to a noticeable change of the deformation mechanisms in boron carbide. In the undoped boron carbide, the Berkovich indentation-induced quasi-plasticity is dominated by amorphization and microcracking along the amorphous shear bands. This mechanism resulted in long, distinct, and single-variant shear faults. In contrast, substantial fragmentation with limited amorphization was activated in the Si-doped boron carbide, manifested by the short, diffuse, and multivariant shear faults. Microcracking via fragmentation competed with and subsequently mitigated amorphization. This work highlights the important roles that solute atoms play on the structural stability of boron carbide and opens up new avenues to tune deformation mechanisms of ceramics via doping.

Nanotwinned metal MEMS films with unprecedented strength and stability.

Silicon-based microelectromechanical systems (MEMS) sensors have become ubiquitous in consumer-based products, but realization of an interconnected network of MEMS devices that allows components to be remotely monitored and controlled, a concept often described as the "Internet of Things," will require a suite of MEMS materials and properties that are not currently available. We report on the synthesis of metallic nickel-molybdenum-tungsten films with direct current sputter deposition, which results in fully dense crystallographically textured films that are filled with nanotwins. These films exhibit linear elastic mechanical behavior and tensile strengths exceeding 3 GPa, which is unprecedented for materials that are compatible with wafer-level device fabrication processes. The ultrahigh strength is attributed to a combination of solid solution strengthening and the presence of dense nanotwins. These films also have excellent thermal and mechanical stability, high density, and electrical properties that are attractive for next-generation metal MEMS applications.

Erratum: New Ground-State Crystal Structure of Elemental Boron [Phys. Rev. Lett. 117, 085501 (2016)].

This corrects the article DOI: 10.1103/PhysRevLett.117.085501.

Superstrength through Nanotwinning.

The theoretical strength of a material is the minimum stress to deform or fracture the perfect single crystal material that has no defects. This theoretical strength is considered as an upper bound on the attainable strength for a real crystal. In contradiction to this expectation, we use quantum mechanics (QM) simulations to show that for the boron carbide (B4C) hard ceramic, this theoretical shear strength can be exceeded by 11% by imposing nanoscale twins. We also predict from QM that the indentation strength of nanotwinned B4C is 12% higher than that of the perfect crystal. Further, we validate this effect experimentally, showing that nanotwinned samples are harder by 2.3% than the twin-free counterpart of B4C. The origin of this strengthening mechanism is suppression of twin boundary (TB) slip within the nanotwins due to the directional nature of covalent bonds at the TB.

Breaking the icosahedra in boron carbide.

Findings of laser-assisted atom probe tomography experiments on boron carbide elucidate an approach for characterizing the atomic structure and interatomic bonding of molecules associated with extraordinary structural stability. The discovery of crystallographic planes in these boron carbide datasets substantiates that crystallinity is maintained to the point of field evaporation, and characterization of individual ionization events gives unexpected evidence of the destruction of individual icosahedra. Statistical analyses of the ions created during the field evaporation process have been used to deduce relative atomic bond strengths and show that the icosahedra in boron carbide are not as stable as anticipated. Combined with quantum mechanics simulations, this result provides insight into the structural instability and amorphization of boron carbide. The temporal, spatial, and compositional information provided by atom probe tomography makes it a unique platform for elucidating the relative stability and interactions of primary building blocks in hierarchically crystalline materials.

New Ground-State Crystal Structure of Elemental Boron.

Elemental boron exhibits many polymorphs in nature based mostly on an icosahedral shell motif, involving stabilization of 13 strong multicenter intraicosahedral bonds. It is commonly accepted that the most thermodynamic stable structure of elemental boron at atmospheric pressure is the ß rhombohedral boron (ß-B). Surprisingly, using high-resolution transmission electron microscopy, we found that pure boron powder contains grains of two different types, the previously identified ß-B containing a number of randomly spaced twins and what appears to be a fully transformed twinlike structure. This fully transformed structure, denoted here as τ-B, is based on the Cmcm orthorhombic space group. Quantum mechanics predicts that the newly identified τ-B structure is 13.8 meV/B more stable than ß-B. The τ-B structure allows 6% more charge transfer from B_{57} units to nearby B_{12} units, making the net charge 6% closer to the ideal expected from Wade's rules. Thus, we predict the τ-B structure to be the ground state structure for elemental boron at atmospheric pressure.

Atomic-Level Understanding of "Asymmetric Twins" in Boron Carbide.

Recent observations of planar defects in boron carbide have been shown to deviate from perfect mirror symmetry and are referred to as "asymmetric twins." Here, we demonstrate that these asymmetric twins are really phase boundaries that form in stoichiometric B(4)C (i.e., B(12)C(3)) but not in B(13)C(2). TEM observations and ab initio simulations have been coupled to show that these planar defects result from an interplay of stoichiometry, atomic positioning, icosahedral twinning, and structural hierarchy. The composition of icosahedra in B(4)C is B(11)C and translation of the carbon atom from a polar to equatorial site leads to a shift in bonding and a slight distortion of the lattice. No such distortion is observed in boron-rich B(13)C(2) because the icosahedra do not contain carbon. Implications for tailoring boron carbide with stoichiometry and extrapolations to other hierarchical crystalline materials are discussed.

Resolving the morphology of niobium carbonitride nano-precipitates in steel using atom probe tomography.

Atom probe is a powerful technique for studying the composition of nano-precipitates, but their morphology within the reconstructed data is distorted due to the so-called local magnification effect. A new technique has been developed to mitigate this limitation by characterizing the distribution of the surrounding matrix atoms, rather than those contained within the nano-precipitates themselves. A comprehensive chemical analysis enables further information on size and chemistry to be obtained. The method enables new insight into the morphology and chemistry of niobium carbonitride nano-precipitates within ferrite for a series of Nb-microalloyed ultra-thin cast strip steels. The results are supported by complementary high-resolution transmission electron microscopy.

Nanocrystalline ß-Ti alloy with high hardness, low Young's modulus and excellent in vitro biocompatibility for biomedical applications.

High strength, low Young's modulus and good biocompatibility are desirable but difficult to simultaneously achieve in metallic implant materials for load bearing applications, and these impose significant challenges in material design. Here we report that a nano-grained ß-Ti alloy prepared by high-pressure torsion exhibits remarkable mechanical and biological properties. The hardness and modulus of the nano-grained Ti alloy were respectively 23% higher and 34% lower than those of its coarse-grained counterpart. Fibroblast cell attachment and proliferation were enhanced, demonstrating good in vitro biocompatibility of the nano-grained Ti alloy, consistent with demonstrated increased nano-roughness on the nano-grained Ti alloy. Results suggest that the nano-grained ß-Ti alloy may have significant application as an implant material in dental and orthopedic applications.

Spatial decomposition of molecular ions within 3D atom probe reconstructions.

Two methods for separating the constituent atoms of molecular ions within atom probe tomography reconstructions are presented. The Gaussian Separation Method efficiently deconvolutes molecular ions containing two constituent atoms and is tested on simulated data before being applied to an experimental HSLA steel dataset containing NbN. The Delaunay Separation Method extends separation to larger complex ions and is also tested on simulated data before being applied to an experimental GaAs dataset containing many large (>3 atoms) complex ions. First nearest neighbour (1NN) distributions and images of the reconstruction before and after the separations are used to show the effect of the algorithms and their validity and practicality are also discussed.

In vitro study of the effect of cyclic strains on the dermal fibroblast (GM3384) morphology--mapping of cell responses to strain field.

Cells can respond to mechanical forces and actively interact with mechanical stimulations in vitro. Understanding the effect of mechanical loading on cell morphology signifies a critical biomechanics issue in tissue engineering. In this study, human dermal fibroblasts (GM3384) underwent cyclic strain. This was done by culturing a monolayer of the cells onto a transparent membrane and applying a cyclic stress using a computer controlled bioreactor. The cells were mechanically stimulated at around 7% strain with 1 cycle per minute for 2 days. Finite element analysis (FEA) was then employed to characterize the strain field across the substrate membrane in the bioreactor. The results showed that strain distribution were non-uniform in the substrate membrane. The mapping of cell morphology with the strain field revealed that the cells exposed to the equibiaxial strain exhibited the classical spindle morphology while the cells subjected to uniaxial strain changed to a polygonal morphology. It is concluded that the nature of the strain has significant impact on the final cell morphology.

Overcoming challenges in the study of nitrided microalloyed steels using atom probe.

Nitrided steels are widely used in the engineering field due to their superior hardness and other attractive properties. Atom probe tomography (APT) was employed to study two Nb-microalloyed CASTRIP steels with different N contents. A major challenge of using APT to study this group of materials is the presence of tails after Fe peaks in the mass spectra, which overestimates the composition for alloying elements such as Nb and Cu in the steels. One important factor that contributes to the tails is believed to be delayed field evaporation from Fe²âº. This artefact of the mass spectrum was observed to be the most severe when voltage pulsing was used. The application of laser pulses with energy ranging from 0.2 to 1.2 nJ successfully reduced the tails and lead to better compositional measurement accuracy. Spatial resolution in the z-direction (along the tip direction) was observed to be less affected by changing laser energy but deteriorates in x-y direction with increasing laser energy. This investigation suggests that pulsed-laser atom probe with ∼0.4 nJ laser energy can be used to study this group of materials with improved mass resolution while still maintaining high spatial resolution.