Daniel S. Gianola

Experimental Observations of Stress-Driven Grain Boundary Migration

Moving Boundaries Classical models of fine-grained metals view grain boundaries as static objects, but this view has been challenged by recent experimental observations. Drawing on techniques used by the fracture mechanics community, Rupert et al. (p. 1686) present experiments on freestanding aluminum films that show specific geometries cause either stress or strain concentrations on deformation. Confirming recent simulations, shear stresses were found to be a key driver of grain boundary motion. Shear stresses drive grain boundaries to move in a manner consistent with predictions of coupled grain boundary migration. In crystalline materials, plastic deformation occurs by the motion of dislocations, and the regions between individual crystallites, called grain boundaries, act as obstacles to dislocation motion. Grain boundaries are widely envisaged to be mechanically static structures, but this report outlines an experimental investigation of stress-driven grain boundary migration manifested as grain growth in nanocrystalline aluminum thin films. Specimens fabricated with specially designed stress and strain concentrators are used to uncover the relative importance of these parameters on grain growth. In contrast to traditional descriptions of grain boundaries as stationary obstacles to dislocation-based plasticity, the results of this study indicate that shear stresses drive grain boundaries to move in a manner consistent with recent molecular dynamics simulations and theoretical predictions of coupled grain boundary migration.

Ultrahigh Strength Single Crystalline Nanowhiskers Grown by Physical Vapor Deposition

The strength of metal crystals is reduced below the theoretical value by the presence of dislocations or by flaws that allow easy nucleation of dislocations. A straightforward method to minimize the number of defects and flaws and to presumably increase its strength is to increase the crystal quality or to reduce the crystal size. Here, we describe the successful fabrication of high aspect ratio nanowhiskers from a variety of face-centered cubic metals using a high temperature molecular beam epitaxy method. The presence of atomically smooth, faceted surfaces and absence of dislocations is confirmed using transmission electron microscopy investigations. Tensile tests performed in situ in a focused-ion beam scanning electron microscope on Cu nanowhiskers reveal strengths close to the theoretical upper limit and confirm that the properties of nanomaterials can be engineered by controlling defect and flaw densities.

A Robust Smart Window: Reversibly Switching from High Transparency to Angle‐Independent Structural Color Display

A smart window is fabricated from a composite consisting of elastomeric poly(dimethylsiloxane) embedded with a thin layer of quasi-amorphous silica nanoparticles. The smart window can be switched from the initial highly transparent state to opaqueness and displays angle-independent structural color via mechanical stretching. The switchable optical property can be fully recovered after 1000 stretching/releasing cycles.

Tunable Tensile Ductility in Metallic Glasses

Widespread adoption of metallic glasses (MGs) in applications motivated by high strength and elasticity combined with plastic-like processing has been stymied by their lack of tensile ductility. One emerging strategy to couple the attractive properties of MGs with resistance to failure by shear localization is to employ sub-micron sample or feature length scales, although conflicting results shroud an atomistic understanding of the responsible mechanisms in uncertainty. Here, we report in situ deformation experiments of directly moulded Pt57.5Cu14.7Ni5.3P22.5 MG nanowires, which show tunable tensile ductility. Initially brittle as-moulded nanowires can be coerced to a distinct glassy state upon irradiation with Ga+ ions, leading to tensile ductility and quasi-homogeneous plastic flow. This behaviour is reversible and the glass returns to a brittle state upon subsequent annealing. Our results suggest a novel mechanism for homogenous plastic flow in nano-scaled MGs and strategies for circumventing the poor damage tolerance that has long plagued MGs.

In situ nanomechanical testing in focused ion beam and scanning electron microscopes.

The recent interest in size-dependent deformation of micro- and nanoscale materials has paralleled both technological miniaturization and advancements in imaging and small-scale mechanical testing methods. Here we describe a quantitative in situ nanomechanical testing approach adapted to a dual-beam focused ion beam and scanning electron microscope. A transducer based on a three-plate capacitor system is used for high-fidelity force and displacement measurements. Specimen manipulation, transfer, and alignment are performed using a manipulator, independently controlled positioners, and the focused ion beam. Gripping of specimens is achieved using electron-beam assisted Pt-organic deposition. Local strain measurements are obtained using digital image correlation of electron images taken during testing. Examples showing results for tensile testing of single-crystalline metallic nanowires and compression of nanoporous Au pillars will be presented in the context of size effects on mechanical behavior and highlight some of the challenges of conducting nanomechanical testing in vacuum environments.

Measuring surface dislocation nucleation in defect-scarce nanostructures

Linear defects in crystalline materials, known as dislocations, are central to the understanding of plastic deformation and mechanical strength, as well as control of performance in a variety of electronic and photonic materials. Despite nearly a century of research on dislocation structure and interactions, measurements of the energetics and kinetics of dislocation nucleation have not been possible, as synthesizing and testing pristine crystals absent of defects has been prohibitively challenging. Here, we report experiments that directly measure the surface dislocation nucleation strengths in high-quality 〈110〉 Pd nanowhiskers subjected to uniaxial tension. We find that, whereas nucleation strengths are weakly size- and strain-rate-dependent, a strong temperature dependence is uncovered, corroborating predictions that nucleation is assisted by thermal fluctuations. We measure atomic-scale activation volumes, which explain both the ultrahigh athermal strength as well as the temperature-dependent scatter, evident in our experiments and well captured by a thermal activation model.

Extremely low drift of resistance and threshold voltage in amorphous phase change nanowire devices

Time-dependent drift of resistance and threshold voltage in phase change memory (PCM) devices is of concern as it leads to data loss. Electrical drift in amorphous chalcogenides has been argued to be either due to electronic or stress relaxation mechanisms. Here we show that drift in amorphized Ge2Sb2Te5 nanowires with exposed surfaces is extremely low in comparison to thin-film devices. However, drift in stressed nanowires embedded under dielectric films is comparable to thin-films. Our results shows that drift in PCM is due to stress relaxation and will help in understanding and controlling drift in PCM devices.

In situ deformation of thin films on substrates.

Metallic thin‐film plasticity has been widely studied by using the difference between the coefficients of thermal expansion of the film and the underlying substrate to induce stress. This approach is commonly known as the wafer curvature technique, based on the Stoney equation, which has shown that thinner films have higher yield stresses. The linear increase of the film strength as a function of the reciprocal film thickness, down to a couple hundred nanometers, has been rationalized in terms of threading and interfacial dislocations. Polycrystalline films also show this kind of dependence when the grain size is larger than or comparable to the film thickness. In situ TEM performed on plan‐view or cross‐section specimens faithfully reproduces the stress state and the small strain levels seen by the metallic film during wafer curvature experiments and simultaneously follows the change in its microstructure. Although plan‐view experiments are restricted to thinner films, cross‐sectional samples where the film is reduced to a strip (or nanowire) on its substrate are a more versatile configuration. In situ thermal cycling experiments revealed that the dislocation/interface interaction could be either attractive or repulsive depending on the interfacial structure. Incoherent interfaces clearly act as dislocation sinks, resulting in a dislocation density drop during thermal cycles. In dislocation‐depleted films (initially thin or annealed), grain boundaries can compensate for the absence of dislocations by either shearing the film similarly to threading dislocations or through fast diffusion processes. Conversely, dislocations are confined inside the film by image forces in the cases of epitaxial interfaces on hard substrates. To increase the amount of strain seen by a film, and to decouple the effects of stress and temperature, compliant substrates can also be used as support for the metallic film. The composite can be stretched at a given temperature using heating/cooling straining holders. Other in situ TEM methods that served to reveal scaling effects are also reviewed. Finally, an alternate method, based on a novel bending holder that can stretch metallic films on rigid substrates, is presented. Microsc. Res. Tech., 2009.

Strain- and Defect-Mediated Thermal Conductivity in Silicon Nanowires

The unique thermal transport of insulating nanostructures is attributed to the convergence of material length scales with the mean free paths of quantized lattice vibrations known as phonons, enabling promising next-generation thermal transistors, thermal barriers, and thermoelectrics. Apart from size, strain and defects are also known to drastically affect heat transport when introduced in an otherwise undisturbed crystalline lattice. Here we report the first experimental measurements of the effect of both spatially uniform strain and point defects on thermal conductivity of an individual suspended nanowire using in situ Raman piezothermography. Our results show that whereas phononic transport in undoped Si nanowires with diameters in the range of 170-180 nm is largely unaffected by uniform elastic tensile strain, another means of disturbing a pristine lattice, namely, point defects introduced via ion bombardment, can reduce the thermal conductivity by over 70%. In addition to discerning surface- and core-governed pathways for controlling thermal transport in phonon-dominated insulators and semiconductors, we expect our novel approach to have broad applicability to a wide class of functional one- and two-dimensional nanomaterials.

The role of confinement on stress-driven grain boundary motion in nanocrystalline aluminum thin films

3D molecular dynamics simulations are performed to investigate the role of microstructural confinement on room temperature stress-driven grain boundary (GB) motion for a general population of GBs in nanocrystalline Al thin films. Detailed analysis and comparison with experimental results reveal how coupled GB migration and GB sliding are manifested in realistic nanoscale networks of GBs. The proximity of free surfaces to GBs plays a significant role in their mobility and results in unique surface topography evolution. We highlight the effects of microstructural features, such as triple junctions, as constraints to otherwise uninhibited GB motion. We also study the pinning effects of impurities segregated to GBs that hinder their motion. Finally, the implications of GB motion as a deformation mechanism governing the mechanical behavior of nanocrystalline materials are discussed.