Autonomous healing of fatigue cracks via cold welding.

Fatigue in metals involves gradual failure through incremental propagation of cracks under repetitive mechanical load. In structural applications, fatigue accounts for up to 90% of in-service failure1,2. Prevention of fatigue relies on implementation of large safety factors and inefficient overdesign3. In traditional metallurgical design for fatigue resistance, microstructures are developed to either arrest or slow the progression of cracks. Crack growth is assumed to be irreversible. By contrast, in other material classes, there is a compelling alternative based on latent healing mechanisms and damage reversal4-9. Here, we report that fatigue cracks in pure metals can undergo intrinsic self-healing. We directly observe the early progression of nanoscale fatigue cracks, and as expected, the cracks advance, deflect and arrest at local microstructural barriers. However, unexpectedly, cracks were also observed to heal by a process that can be described as crack flank cold welding induced by a combination of local stress state and grain boundary migration. The premise that fatigue cracks can autonomously heal in metals through local interaction with microstructural features challenges the most fundamental theories on how engineers design and evaluate fatigue life in structural materials. We discuss the implications for fatigue in a variety of service environments.

Sample Preparation and Experimental Design for In Situ Multi-Beam Transmission Electron Microscopy Irradiation Experiments.

There is a need to understand materials exposed to overlapping extreme environments such as high temperature, radiation, or mechanical stress. When these stressors are combined there may be synergistic effects that enable unique microstructural evolution mechanisms to activate. Understanding of these mechanisms is necessary for the input and refinement of predictive models and critical for engineering of next generation materials. The basic physics and underlying mechanisms require advanced tools to be investigated. The in situ ion irradiation transmission electron microscope (I³TEM) is designed to explore these principles. To quantitatively probe the complex dynamic interactions in materials, careful preparation of samples and consideration of experimental design is required. Particular handling or preparation of samples can easily introduce damage or features that obfuscate the measurements. There is no one correct way to prepare a sample; however, many mistakes can be made. The most common errors and things to consider are highlighted within. The I³TEM has many adjustable variables and a large potential experimental space, therefore it is best to design experiments with a specific scientific question or questions in mind. Experiments have been performed on large number of sample geometries, material classes, and with many irradiation conditions. The following are a subset of examples that demonstrate unique in situ capabilities utilizing the I3TEM. Au nanoparticles prepared by drop casting have been used to investigate the effects of single ion strikes. Au thin films have been used in studies on the effects of multibeam irradiation on microstructure evolution. Zr films have been exposed to irradiation and mechanical tension to examine creep. Ag nanopillars were subjected to simultaneous high temperature, mechanical compression, and ion irradiation to study irradiation induced creep as well. These results impact fields including: structural materials, nuclear energy, energy storage, catalysis, and microelectronics in space environments.

Irradiation-induced grain boundary facet motion: In situ observations and atomic-scale mechanisms.

Metals subjected to irradiation environments undergo microstructural evolution and concomitant degradation, yet the nanoscale mechanisms for such evolution remain elusive. Here, we combine in situ heavy ion irradiation, atomic resolution microscopy, and atomistic simulation to elucidate how radiation damage and interfacial defects interplay to control grain boundary (GB) motion. While classical notions of boundary evolution under irradiation rest on simple ideas of curvature-driven motion, the reality is far more complex. Focusing on an ion-irradiated Pt Σ3 GB, we show how this boundary evolves by the motion of 120° facet junctions separating nanoscale {112} facets. Our analysis considers the short- and mid-range ion interactions, which roughen the facets and induce local motion, and longer-range interactions associated with interfacial disconnections, which accommodate the intergranular misorientation. We suggest how climb of these disconnections could drive coordinated facet junction motion. These findings emphasize that both local and longer-range, collective interactions are important to understanding irradiation-induced interfacial evolution.

Photo-exfoliation of MoS2quantum dots from nanosheets: anin situtransmission electron microscopy study.

Fabrication of transition metal dichalcogenide quantum dots (QDs) is complex and requires submerging powders in binary solvents and constant tuning of wavelength and pulsed frequency of light to achieve a desired reaction. Instead of liquid state photoexfoliation, we utilize infrared laser irradiation of free-standing MoS2flakes in transmission electron microscope (TEM) to achieve solid-state multi-level photoexfoliation of QDs. By investigating the steps involved in photochemical reaction between the surface of MoS2and the laser beam, we gain insight into each step of the photoexfoliation mechanism and observe high yield production of QDs, led by an inhomogeneous crystalline size distribution. Additionally, by using a laser with a lower energy than the indirect optical transition of bulk MoS2, we conclude that the underlying phenomena behind the photoexfoliation is from multi-photon absorption achieved at high optical outputs from the laser source. These findings provide an environmentally friendly synthesis method to fabricate QDs for potential applications in biomedicine, optoelectronics, and fluorescence sensing.

Evidence for a High Temperature Whisker Growth Mechanism Active in Tungsten during In Situ Nanopillar Compression.

A series of nanopillar compression tests were performed on tungsten as a function of temperature using in situ transmission electron microscopy with localized laser heating. Surface oxidation was observed to form on the pillars and grow in thickness with increasing temperature. Deformation between 850 °C and 1120 °C is facilitated by long-range diffusional transport from the tungsten pillar onto adjacent regions of the Y2O3-stabilized ZrO2 indenter. The constraint imposed by the surface oxidation is hypothesized to underly this mechanism for localized plasticity, which is generally the so-called whisker growth mechanism. The results are discussed in context of the tungsten fuzz growth mechanism in He plasma-facing environments. The two processes exhibit similar morphological features and the conditions under which fuzz evolves appear to satisfy the conditions necessary to induce whisker growth.

The role of grain boundary character in solute segregation and thermal stability of nanocrystalline Pt-Au.

Nanocrystalline (NC) metals suffer from an intrinsic thermal instability; their crystalline grains undergo rapid coarsening during processing treatments or under service conditions. Grain boundary (GB) solute segregation has been proposed to mitigate grain growth and thermally stabilize the grain structures of NC metals. However, the role of GB character in solute segregation and thermal stability of NC metals remains poorly understood. Herein, we employ high resolution microscopy techniques, atomistic simulations, and theoretical analysis to investigate and characterize the impact of GB character on segregation behavior and thermal stability in a model NC Pt-Au alloy. High resolution electron microscopy along with X-ray energy dispersive spectroscopy and automated crystallographic orientation mapping is used to obtain spatially correlated Pt crystal orientation, GB misorientation, and Au solute concentration data. Atomistic simulations of polycrystalline Pt-Au systems are used to reveal the plethora of GB segregation profiles as a function of GB misorientation and the corresponding impact on grain growth processes. With the aid of theoretical models of interface segregation, the experimental data for GB concentration profiles are used to extract GB segregation energies, which are then used to elucidate the impact of GB character on solute drag effects. Our results highlight the paramount role of GB character in solute segregation behavior. In broad terms, our approach provides future avenues to employ GB segregation as a microstructure design strategy to develop NC metallic alloys with tailored microstructures.

Hardening in Au-Ag nanoboxes from stacking fault-dislocation interactions.

Porous, nano-architected metals with dimensions down to ~10 nm are predicted to have extraordinarily high strength and stiffness per weight, but have been challenging to fabricate and test experimentally. Here, we use colloidal synthesis to make ~140 nm length and ~15 nm wall thickness hollow Au-Ag nanoboxes with smooth and rough surfaces. In situ scanning electron microscope and transmission electron microscope testing of the smooth and rough nanoboxes show them to yield at 130 ± 45 MPa and 96 ± 31 MPa respectively, with significant strain hardening. A higher strain hardening rate is seen in rough nanoboxes than smooth nanoboxes. Finite element modeling is used to show that the structure of the nanoboxes is not responsible for the hardening behavior suggesting that material mechanisms are the source of observed hardening. Molecular dynamics simulations indicate that hardening is a result of interactions between dislocations and the associated increase in dislocation density.

In Situ Transmission Electron Microscopy for Ultrahigh Temperature Mechanical Testing of ZrO2.

This work demonstrates a novel approach to ultrahigh-temperature mechanical testing using a combination of in situ nanomechanical testing and localized laser heating. The methodology is applied to characterizing and testing initially nanograined 10 mol % Sc2O3-stabilized ZrO2 up to its melting temperature. The results suggest that the low-temperature strength of nanograined, d < 50 nm, oxides is not influenced by creep. Tensile fracture of ZrO2 bicrystals produce a weak-temperature dependence suggesting that grain boundary energy dominates brittle fracture of grain boundaries even at high homologous temperatures; for example, T = 2050 °C or T ≈ 77% Tmelt. The maximum temperature for mechanical testing in this work is primarily limited by the instability of the sample, due to evaporation or melting, enabling a host of new opportunities for testing materials in the ultrahigh-temperature regime.

New nanoscale toughening mechanisms mitigate embrittlement in binary nanocrystalline alloys.

Nanocrystalline metals offer significant improvements in structural performance over conventional alloys. However, their performance is limited by grain boundary instability and limited ductility. Solute segregation has been proposed as a stabilization mechanism, however the solute atoms can embrittle grain boundaries and further degrade the toughness. In the present study, we confirm the embrittling effect of solute segregation in Pt-Au alloys. However, more importantly, we show that inhomogeneous chemical segregation to the grain boundary can lead to a new toughening mechanism termed compositional crack arrest. Energy dissipation is facilitated by the formation of nanocrack networks formed when cracks arrested at regions of the grain boundaries that were starved in the embrittling element. This mechanism, in concert with triple junction crack arrest, provides pathways to optimize both thermal stability and energy dissipation. A combination of in situ tensile deformation experiments and molecular dynamics simulations elucidate both the embrittling and toughening processes that can occur as a function of solute content.