Defect structures as a function of ion irradiation and annealing in LiNbO3
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Engineering topics
Publications and source records attributed to Clark, Blythe G..
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The present invention relates to metal coatings and methods thereof. In certain embodiments, the invention relates to ultra-low wear noble metal alloys, such as for use in electrical contact coatings.
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. In this paper, we show that PtAu, a proposed stable alloy consisting of two noble metals, exhibits extraordinary resistance to wear. Ultra-low wear rates, less than a monolayer of material removed per sliding pass, were measured for PtAu 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 mm 3 /N-m, comparable to diamond-like carbon and sapphire. Remarkably, the wear rate of sapphire and silicon nitride probes used in wear experiments were either higher or comparable to that of the PtAu alloy, despite the substantially higher hardness of the ceramic probe materials. High-resolution microscopy showed negligible surface microstructural evolution in the wear tracks after 100k sliding passes. Finally, mitigation of fatigue-driven delamination enabled a transition to wear by atomic attrition, a regime previously limited to highly wear resistant materials such as diamond-like carbon.
Abstract 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 mm 3 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.
Ductile rupture in metals is generally a multi-step process of void nucleation, growth, and coalescence. Particle decohesion and particle fracture are generally invoked as the primary microstructural mechanisms for room-temperature void nucleation. However, because high-purity materials also fail by void nucleation and coalescence, other microstructural features must also act as sites for void nucleation. Early studies of void initiation in high-purity materials, which included post-mortem fracture surface characterization using scanning electron microscopy (SEM) and high-voltage electron microscopy (HVEM) and in-situ HVEM observations of fracture, established the presence of dislocation cell walls as void initiation sites in high-purity materials. Direct experimental evidence for this contention was obtained during in-situ HVEM tensile tests of Be single crystals. Voids between 0.2 and 1 μm long appeared suddenly along dislocation cell walls during tensile straining. However, subsequent attempts to replicate these results in other materials, particularly α -Fe single crystals, were unsuccessful because of the small size of the dislocation cells, and these remain the only published in-situ HVEM observations of void nucleation at dislocation cell walls in the absence of a growing macrocrack. Despite this challenge, other approaches to studying void nucleation in high-purity metals also indicate that dislocation cell walls are nucleation sites for voids.
Here, the widely recognized property improvements of nanocrystalline (NC) materials have generated significant interest, yet have been difficult to realize in engineering applications due to the propensity for grain growth in these interface-dense systems. While traditional pathways to thermal stabilization can slow the mobility of grain boundaries, recent theories suggest that solute segregation in NC alloy can reduce the grain boundary energy such that thermodynamic stabilization is achieved. Following the predictions of Murdock et al., here we compare for the first time the thermal stability of a predicted NC stable alloy (Fe-10at.% Mg) with a predicted non-NC stable alloy (Fe-10at.% Cu) using the same processing and characterization methodologies. Results indicate improved thermal stability of the Fe-Mg alloy in comparison to the Fe-Cu, and observed microstructures are consistent with those predicted by Monte Carlo simulations.
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. Furthermore, 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.
The goal of this SAND report is to provide guidance for other groups hosting workshops and peerto-peer learning events at Sandia. Thus this SAND report provides detail about our team structure, how we brainstormed workshop topics and developed the workshop structure. A Workshop “Nuts and Bolts” section provides our timeline and check-list for workshop activities. The survey section provides examples of the questions we asked and how we adapted the workshop in response to the feedback.
We report on the suppression of room temperature oxidation of DC sputtered niobium films and the effects upon the superconductive transition temperature, T{sub c}. Niobium was sputter-deposited on silicon dioxide coated 150 mm wafers and permitted to oxidize at room temperature and pressure for up to two years. Resistivity and stress measurements indicate that tensile films greater than 400 MPa resist bulk oxidation with measurements using transmission electron microscope, electron dispersive X-ray spectroscopy, x-ray photoelectric spectroscopy, and secondary ion mass spectrometry confirming this result. Although a surface oxide, Nb{sub 2}O{sub 5}, consumed the top 6–10 nm, we measure less than 1 at. % oxygen and nitrogen in the bulk of the films after the oxidation period. T{sub c} measurements using a SQUID magnetometer indicate that the tensile films maintained a T{sub c} approaching the dirty superconductive limit of 8.4 K after two years of oxidation while maintaining room temperature sheet resistance. This work demonstrates that control over niobium film stress during deposition can prevent bulk oxidation by limiting the vertical grain boundaries ability to oxidize, prolonging the superconductive properties of sputtered niobium when exposed to atmosphere.
Using in situ scanning transmission electron microscopy heating experiments, we observed the formation of a 3-dimensional (3D) epitaxial Cu-core and Ag-shell equilibrium structure of a Cu-Ag nanoalloy. The structure was formed during the thermal interaction of Cu(∼12 nm) and Ag NPs(∼6 nm) at elevated temperatures (150–300 °C) by the Ag NPs initially wetting the Cu NP along its (111) surfaces at one or multiple locations forming epitaxial Ag/Cu (111) interfaces, followed by Ag atoms diffusing along the Cu surface. This phenomenon was confirmed through Monte Carlo simulations to be a nanoscale effect related to the large surface-to-volume ratio of the NPs.
We present the results of a three-year LDRD project focused on understanding microstructural evolution and related property changes in Zr-based nuclear cladding materials towards the development of high fidelity predictive simulations for long term dry storage. Experiments and modeling efforts have focused on the effects of hydride formation and accumulation of irradiation defects. Key results include: determination of the influence of composition and defect structures on hydride formation; measurement of the electrochemical property differences between hydride and parent material for understanding and predicting corrosion resistance; in situ environmental transmission electron microscope observation of hydride formation; development of a predictive simulation for mechanical property changes as a function of irradiation dose; novel test method development for microtensile testing of ionirradiated material to simulate the effect of neutron irradiation on mechanical properties; and successful demonstration of an Idaho National Labs-based sample preparation and shipping method for subsequent Sandia-based analysis of post-reactor cladding.