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In-situ transmission electron microscopy (TEM) provides an avenue to explore time-dependent nanoscale material changes induced by a wide range of environmental conditions that govern material performance and degradation. The In-situ Ion Irradiation TEM (I3TEM) at Sandia National Laboratories is a JEOL 2100 microscope that has been highly modified with an array of hardware and software that makes it particularly well suited to explore fundamental mechanisms that arise from coupled extreme conditions. Examples pertaining to multibeam ion irradiation, rapid thermal cycling, and nanomechanical testing on the I3TEM are highlighted, along with prospective advancements in the field of in-situ microscopy.
Residual strain in electrodeposited Li films may affect safety and performance in Li metal battery anodes, so it is important to understand how to detect residual strain in electrodeposited Li and the conditions under which it arises. To explore this Li films, electrodeposited onto Cu metal substrates, were prepared under an applied pressure of either 10 or 1000 kPa and subsequently tested for the presence or absence of residual strain via sin2(ψ) analysis. X-ray diffraction (XRD) analysis of Li films required preparation and examination within an inert environment; hence, a Be-dome sample holder was employed during XRD characterization. Results show that the Li film grown under 1000 kPa displayed a detectable presence of in-plane compressive strain (−0.066%), whereas the Li film grown under 10 kPa displayed no detectable in-plane strain. The underlying Cu substrate revealed an in-plane residual strain near zero. Texture analysis via pole figure determination was also performed for both Li and Cu and revealed a mild fiber texture for Li metal and a strong bi-axial texture of the Cu substrate. Experimental details concerning sample preparation, alignment, and analysis of the particularly air-sensitive Li films have also been detailed. This work shows that Li metal exhibits residual strain when electrodeposited under compressive stress and that XRD can be used to quantify that strain.
Historically, the advent of robotics has important roots in metallurgy. The first industrial robot, Unimate, was used by General Motors to handle hot metal—transporting die castings and welding them to an automotive body. Now, nearly 60 years later, metallurgical use of robotics is still largely confined to automation of dangerous, complex, and repetitive tasks. Beyond metallurgy, the field of autonomy is undergoing a renaissance, impacting applications from pharmaceuticals to transportation. In this article, we review the emerging elements of high-throughput experimental automation, which, when combined with artificial intelligence or machine-learning systems, will enable autonomous discovery of novel alloys and process routes.
In this study, we report a micropillar stress relaxation technique employing a stable displacement-controlled, in-situ scanning electron microscope indenter, and unusually large micropillars to precisely measure stress relaxation in electroplated nanocrystalline Ni thin films. The observed stress relaxation is significant under constant displacement: even well below the 0.2% offset yield strength, the stresses relax by ∼4% within a minute; in the work hardening regime, stress relaxes by ∼9% in 1 min. A logarithmic fit of the relaxation curves is consistent with an Arrhenius thermal activation of plasticity and suggests an activation volume in the vicinity of ∼10 b3. The apparent and effective activation volumes diverge at lower strains, particularly in the “elastic” regime. These measurements are compared to similar measurements performed on free-standing thin film tensile coupons. Both methods yield similar results, thereby validating the applicability of pillar compression to capture time-dependent plasticity. To our knowledge, these are the first micropillar stress relaxation experiments on metals ever reported.
Recent studies have shown the potential for nanocrystalline metals to possess excellent fatigue resistance compared to their coarse-grained counterparts. Although the mechanical properties of nanocrystalline metals are believed to be particularly susceptible to material defects, a systematic study of the effects of geometric discontinuities on their fatigue performance has not yet been performed. In the present work, nanocrystalline Ni–40 wt%Fe containing both intrinsic and extrinsic defects were tested in tension–tension fatigue. The defects were found to dramatically reduce the fatigue resistance, which was attributed to the relatively high notch sensitivity in the nanocrystalline material. Microstructural analysis within the crack-initiation zones underneath the defects revealed cyclically-induced abnormal grain growth (AGG) as a predominant deformation and crack initiation mechanism during high-cycle fatigue. The onset of AGG and the ensuing fracture is likely accelerated by the stress concentrations, resulting in the reduced fatigue resistance compared to the relatively defect-free counterparts.
Using an in situ load frame within a scanning electron microscope, a microstructural section on the surface of an annealed tantalum (Ta) polycrystalline specimen was mapped at successive tensile strain intervals, up to ~20% strain, using electron backscatter diffraction. A grain identification and correlation technique was developed for characterizing the evolving microstructure during loading. Presenting the correlated results builds on the reference orientation deviation (ROD) map concept where individual orientation measurements within a grain are compared with a reference orientation associated with that grain. In this case, individual orientation measurements in a deformed grain are measured relative to a reference orientation derived from the undeformed (initial) configuration rather than the current deformed configuration as has been done for previous ROD schemes. Using this technique helps reveal the evolution of crystallographic orientation gradients and development of deformation-induced substructure within grains. Although overall crystallographic texture evolved slowly during deformation, orientation spread within grains developed quickly. In some locations, misorientation relative to the original orientation of a grain exceeded 20° by 15% strain. The largest orientation changes often appeared near grain boundaries suggesting that these regions were preferred locations for the initial development of subgrains.
Nanocrystalline (NC) metals are known for having excellent strength but perceived to have poor ductility. Miniature tensile tests on NC Ni–Fe measured ultimate strengths of 2 GPa and elongations, by digital image correlation, of up to 10%. Detailed examination of the fracture surface revealed dimpled rupture and cross-section reduction up to 75%, suggesting an intrinsic ability for small grained Ni–Fe to accommodate plasticity. A survey of published studies on NC metals reveals that this behavior is quite common; despite low macroscopic elongation, NC metals often achieve extensive deformation suggesting good intrinsic ductility. Unfortunately, the common sheet-like configuration of NC tensile specimens muddies a simple evaluation of ductility based on elongation, since thin and wide geometries promote localized necking that expedites catastrophic failure. This paper presents a compact review of ductility concepts and literature to interpret the experimental ductility measurements of an electrodeposited nickel alloy.
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