Publications

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Recent work suggests that thermally stable nanocrystallinity in metals is achievable in several binary alloys by modifying grain boundary energies via solute segregation. The remarkable thermal stability of these alloys has been demonstrated in recent reports, with many alloys exhibiting negligible grain growth during prolonged exposure to near-melting temperatures. Pt–Au, a proposed stable alloy consisting of two noble metals, is shown to exhibit extraordinary resistance to wear. Ultralow wear rates, less than a monolayer of material removed per sliding pass, are measured for Pt–Au thin films at a maximum Hertz contact stress of up to 1.1 GPa. This is the first instance of an all-metallic material exhibiting a specific wear rate on the order of 10−9 mm3 N−1 m−1, comparable to diamond-like carbon (DLC) and sapphire. Remarkably, the wear rate of sapphire and silicon nitride probes used in wear experiments are either higher or comparable to that of the Pt–Au alloy, despite the substantially higher hardness of the ceramic probe materials. High-resolution microscopy shows negligible surface microstructural evolution in the wear tracks after 100k sliding passes. Mitigation of fatigue-driven delamination enables a transition to wear by atomic attrition, a regime previously limited to highly wear-resistant materials such as DLC.

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Prior studies on the high-cycle fatigue behavior of nanocrystalline metals have shown that fatigue fracture is associated with abnormal grain growth (AGG). However, those previous studies have been unable to determine if AGG precedes fatigue crack initiation, or vice-versa. The present study shows that AGG indeed occurs prior to crack formation in nanocrystalline Ni-Fe by using a recently developed synchrotron X-ray diffraction modality that has been adapted for in-situ analysis. The technique allows fatigue tests to be interrupted at the initial signs of the AGG process, and subsequent microscopy reveals the precursor damage state preceding crack initiation.

We demonstrate inverse Hall-Petch behavior (softening) in pure copper sliding contacts at cryogenic temperatures. By kinetically limiting grain growth, it is possible to generate a quasi-stable ultra-nanocrystalline surface layer with reduced strength. In situ electrical contact resistance measurements were used to determine grain size evolution at the interface, in agreement with reports of softening in highly nanotwinned copper. We also show evidence of a direct correlation between surface grain size and friction coefficient, validating a model linking friction in pure metals and the transition from dislocation mediated plasticity to grain boundary sliding.

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Conventional structural metals suffer from fatigue-crack initiation through dislocation activity which forms persistent slip bands leading to notch-like extrusions and intrusions. Ultrafine-grained and nanocrystalline metals can potentially exhibit superior fatigue-crack initiation resistance by suppressing these cumulative dislocation activities. Prior studies on these metals have confirmed improved high-cycle fatigue performance. In the case of nano-grained metals, analyses of subsurface crack initiation sites have indicated that the crack nucleation is associated with abnormally large grains. However, these post-mortem analyses have led to only speculation about when abnormal grain growth occurs (e.g., during fatigue, after crack initiation, or during crack growth). In this study, a recently developed synchrotron X-ray diffraction technique was used to detect the onset and progression of abnormal grain growth during stress-controlled fatigue loading. This study provides the first direct evidence that the grain coarsening is cyclically induced and occurs well before final fatigue failure—our results indicate that the first half of the fatigue life was spent prior to the detectable onset of abnormal grain growth, while the second half was spent coarsening the nanocrystalline structure and cyclically deforming the abnormally large grains until crack initiation. Post-mortem fractography, coupled with cycle-dependent diffraction data, provides the first details regarding the kinetics of this abnormal grain growth process during high-cycle fatigue testing. Precession electron diffraction images collected in a transmission electron microscope after the in situ fatigue experiment also confirm the X-ray evidence that the abnormally large grains contain substantial misorientation gradients and sub-grain boundaries.

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The friction behavior of ultra-nanocrystalline Ni-W coatings was investigated. A critical stress threshold was identified below which friction remained low, and above which a time-dependent evolution toward higher friction behavior occurred. Founded on established plasticity models we propose a correlation between surface grain size and applied stress that can be used to predict the critical stress separating the two friction regimes. This interpretation of plasticity models suggests that macro-scale low and high friction regimes are respectively associated with the nano-scale mechanisms of grain boundary and dislocation-mediated plasticity.

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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.

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Bimodal grain structures are common in many alloys, arising from a number of different causes including incomplete recrystallization and abnormal grain growth. These bimodal grain structures have important technological implications, such as the well-known Goss texture which is now a cornerstone for electrical steels. Yet our ability to detect bimodal grain distributions is largely confined to brute force cross-sectional metallography. The present study presents a new method for rapid detection of unusually large grains embedded in a sea of much finer grains. Traditional X-ray diffraction-based grain size measurement techniques such as Scherrer, Williamson–Hall, or Warren–Averbach rely on peak breadth and shape to extract information regarding the average crystallite size. However, these line broadening techniques are not well suited to identify a very small fraction of abnormally large grains. The present method utilizes statistically anomalous intensity spikes in the Bragg peak to identify regions where abnormally large grains are contributing to diffraction. This needle-in-a-haystack technique is demonstrated on a nanocrystalline Ni–Fe alloy which has undergone fatigue-induced abnormal grain growth. In this demonstration, the technique readily identifies a few large grains that occupy <0.00001 % of the interrogation volume. While the technique is demonstrated in the current study on nanocrystalline metal, it would likely apply to any bimodal polycrystal including ultrafine grained and fine microcrystalline materials with sufficiently distinct bimodal grain statistics.

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