Publications

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Under high-cycle fatigue conditions, a fatigue crack in nanocrystalline Pt was observed to undergo healing. The healing appears to occur by cold welding, facilitated by grain boundary migration, and also by local closure stresses. The healing may help explain several observations: role of air (or vacuum) on fatigue life, impeded subsurface fatigue cracking, apparent flaw healing in sub-critical cycling of ceramics, the existence of a fatigue threshold, and the role of vacuum on the fatigue threshold.

An in situ ion irradiation scanning electron microscope (I³SEM) has been developed, installed, and integrated into the Ion Beam Laboratory at Sandia National Laboratories. The I³SEM facility combines a field emission, variable pressure, scanning electron microscope, a 6 MV tandem accelerator, high flux low energy ion source, an 808 nm-wavelength laser, and multiple stages to control the thermal and mechanical state of the sample observed. The facility advances real-time understanding of materials evolution under combined environments at the mesoscale. As highlighted in multiple examples, this unique combination of tools is optimized for studying mesoscale material response in overlapping extreme environments, allowing for simultaneous ion irradiation, implantation, laser bombardment, conductive heating, cooling, and mechanical deformation.

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To model and quantify the variability in plasticity and failure of additively manufactured metals due to imperfections in their microstructure, we have developed uncertainty quantification methodology based on pseudo marginal likelihood and embedded variability techniques. We account for both the porosity resolvable in computed tomography scans of the initial material and the sub-threshold distribution of voids through a physically motivated model. Calibration of the model indicates that the sub-threshold population of defects dominates the yield and failure response. Finally, the technique also allows us to quantify the distribution of material parameters connected to microstructural variability created by the manufacturing process, and, thereby, make assessments of material quality and process control.

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This work explores the development of a heterogeneous nanostructured material through leveraging abnormal recrystallization, which is a prominent phenomenon in coarse-grained Ni-based superalloys. Through synthesis of a sputtered Inconel 725 film with a heterogeneous distribution of stored energy and subsequent aging treatments at 730°C, a unique combination of grain sizes and morphologies was observed throughout the thickness of the material. Three distinct domains are formed in the aged microstructure, where abnormally large grains are observed in-between a nanocrystalline and a nanotwinned region. In order to investigate the transitions towards a heterogeneous structure, crystallographic orientation and elemental mapping at interval aging times up to 8 h revealed the microstructural evolution and precipitation behavior. From the experimental observations and the detailed analysis of this study, the current methodology can be utilized to further expand the design space of current heterogeneous nanostructured materials.

The high-cycle fatigue life of nanocrystalline and ultrafine-grained Ni-Fe was examined for five distinct grain sizes ranging from approximately 50–600 nm. The fatigue properties were strongly dependent on grain size, with the endurance limit changing by a factor of 4 over this narrow range of grain size. The dataset suggests a breakdown in fatigue improvement for the smallest grain sizes <100 nm, likely associated with a transition to grain coarsening as a dominant rate-limiting mechanism. The dataset also is used to explore fatigue prediction from monotonic tensile properties, suggesting that a characteristic flow strength is more meaningful than the widely-utilized ultimate tensile strength.

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The mechanical properties of additively manufactured metals tend to show high variability, due largely to the stochastic nature of defect formation during the printing process. This study seeks to understand how automated high throughput testing can be utilized to understand the variable nature of additively manufactured metals at different print conditions, and to allow for statistically meaningful analysis. This is demonstrated by analyzing how different processing parameters, including laser power, scan velocity, and scan pattern, influence the tensile behavior of additively manufactured stainless steel 316L utilizing a newly developed automated test methodology. Microstructural characterization through computed tomography and electron backscatter diffraction is used to understand some of the observed trends in mechanical behavior. Specifically, grain size and morphology are shown to depend on processing parameters and influence the observed mechanical behavior. In the current study, laser-powder bed fusion, also known as selective laser melting or direct metal laser sintering, is shown to produce 316L over a wide processing range without substantial detrimental effect on the tensile properties. Ultimate tensile strengths above 600 MPa, which are greater than that for typical wrought annealed 316L with similar grain sizes, and elongations to failure greater than 40% were observed. It is demonstrated that this process has little sensitivity to minor intentional or unintentional variations in laser velocity and power.

Knowing when, why, and how materials evolve, degrade, or fail in radiation environments is pivotal to a wide range of fields from semiconductor processing to advanced nuclear reactor design. A variety of methods, including optical and electron microscopy, mechanical testing, and thermal techniques, have been used in the past to successfully monitor the microstructural and property evolution of materials exposed to extreme radiation environments. Acoustic techniques have also been used in the past for this purpose, although most methodologies have not achieved widespread adoption. However, with an increasing desire to understand microstructure and property evolution in situ, acoustic methods provide a promising pathway to uncover information not accessible to more traditional characterization techniques. This work highlights how two different classes of acoustic techniques may be used to monitor material evolution during in situ ion beam irradiation. The passive listening technique of acoustic emission is demonstrated on two model systems, quartz and palladium, and shown to be a useful tool in identifying the onset of damage events such as microcracking. An active acoustic technique in the form of transient grating spectroscopy is used to indirectly monitor the formation of small defect clusters in copper irradiated with self-ions at high temperature through the evolution of surface acoustic wave speeds. Here, these studies together demonstrate the large potential for using acoustic techniques as in situ diagnostics. Such tools could be used to optimize ion beam processing techniques or identify modes and kinetics of materials degradation in extreme radiation environments.

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