Nanostructures with a high density of interfaces, such as in nanoporous materials and nanowires, resist radiation damage by promoting the annihilation and migration of defects. This study details the size effect and origins of the radiation damage mechanisms in nanowires and nanoporous structures in model face-centered (gold) and body-centered (niobium) cubic nanostructures using accelerated multi-cascade atomistic simulations and in-situ ion irradiation experiments. Our results reveal three different size-dependent mechanisms of damage accumulation in irradiated nanowires and nanoporous structures: sputtering for very small nanowires and ligaments, the formation and accumulation of point defects and dislocation loops in larger nanowires, and a face-centered-cubic to hexagonal-close-packed phase transformation for a narrow range of wire diameters in the case of gold nanowires. Smaller nanowires and ligaments have a net effect of lowering the radiation damage as compared to larger wires that can be traced back to the fact that smaller nanowires transition from a rapid accumulation of defects to a saturation and annihilation mechanism at a lower dose than larger nanowires. These irradiation damage mechanisms are accompanied with radiation-induced surface roughening resulting from defect-surface interactions. Comparisons between nanowires and nanoporous structures show that the various mechanisms seen in nanowires provide adequate bounds for the defect accumulation mechanisms in nanoporous structures with the difference attributed to the role of nodes connecting ligaments in nanoporous structures. Taken together, our results shed light on the compounded, size-dependent mechanisms leading to the radiation resistance of nanowires and nanoporous structures.
Dillon, Shen D.; Coffman, Keith C.; Grosso, Robson L.; Jawaharram, Gowtham S.; Feng, Lin F.; Ma, Yonghui M.; Navarro dos Santos Mucillo, Elina N.; Hattar, Khalid M.; Barr, Christopher M.; Castro, Ricardo C.; Ouyang, Jia-hu O.; Garcia, R.E.; Abdeljawad, Fadi A.
Ajantiwalay, Tanvi; Nagel, Lauren; Maloy, Stuart; Hattar, Khalid M.; Mecholsky, John J.; Aitkaliyeva, Assel
Ferritic/martensitic steels, such as HT-9, are known for their complex microstructural features and mechanical properties. In this paper, in-situ micro-tensile tests and traditional fractography methods were utilized to study the fracture behavior of proton-irradiated HT-9 steels. First, to evaluate the viability of micro-tensile tests for nuclear material qualification process, meso‑tensile tests on as-received HT-9 steels were performed. Fracture mechanisms of unirradiated HT-9 steels at both length scales were compared and underlying mechanisms discussed. The direct comparison of micro- and meso‑scale data shows a distinctive size effect demonstrated by the increase in yield stress (YS). Upon completion of initial assessment, specimens were irradiated with 4 MeV+ protons to three fluences, all of which were lower than 0.01 displacements per atom (dpa). As expected, the YS increases with irradiation. However, at 7 × 10−3 dpa, the reversal of the trend was observed, and the YS exhibited sharp decline. We demonstrate that at lower length scales, grain structure has a more profound impact on the mechanical properties of irradiated materials, which provides information needed to fill in the gap in current understanding of the HT-9 fracture at different length scales.
Nanocrystalline Al thin films have been strained in situ in a transmission electron microscope using two separate nanomechanical techniques involving a push-to-pull device and a microelectromechanical system (MEMS) device. Deformation-induced grain growth was observed to occur via stress-assisted grain boundary migration with extensive grain growth occurring in the necked region, indicating that the increase in local stress drives the boundary migration. Under applied tensile stresses close to the ultimate tensile strength of 450 MPa for a nanocrystalline Al specimen, measured boundary migration speeds are 0.2 – 0.7 nm s−1 for grains outside necked region and increases to 2.5 nm s−1 for grains within the necked region where the local estimated tensile stresses are elevated to around 630 MPa. By tracking grain boundary motion over time, molecular dynamics simulations showed qualitative agreement in terms of pronounced grain boundary migration with the experimental observations. The combined in situ observation and molecular dynamics simulation results underscore the important role of stress-driven grain growth in plastically deforming nanocrystalline metals, leading to intergranular fracture through predominant grain boundary sliding in regions with large localized deformation.
In this article, we have evaluated the Read-Retry (RR) functionality of the 3-D NAND chip of multilevel-cell (MLC) configuration after total ionization dose (TID) exposure. The RR function is typically offered in the high-density state-of-the-art NAND memory chips to recover data once the default memory read method fails to correct data with error correction codes (ECCs). In this work, we have applied the RR method on the irradiated 3-D NAND chip that was exposed with a Co-60 gamma-ray source for TID up to 50 krad (Si). Based on our experimental evaluation results, we have proposed an algorithm to efficiently implement the RR method to extend the radiation tolerance of the NAND memory chip. Our experimental evaluation shows that the RR method coupled with ECC can ensure data integrity of MLC 3-D NAND for TID up to 50 krad (Si).
Hong, Daniel H.; Hattar, Khalid M.; Li, Nan L.; Paranjape, Harshad P.; Schaffer, Jeremy S.; Hinojos, Alejandro H.; Mills, Michael J.; Yu, Taiwu Y.; Wang, Yunzhi W.; Anderson, Peter A.
Abstract: Multimodal in-situ experiments are the wave of the future, as this approach will permit multispectral data collection and analysis during real-time nanoscale observation. In contrast, the evolution of technique development in the electron microscopy field has generally trended toward specialization and subsequent bifurcation into more and more niche instruments, creating a challenge for reintegration and backward compatibility for in-situ experiments on state-of-the-art microscopes. We do not believe this to be a requirement in the field; therefore, we propose an adaptive instrument that is designed to allow nearly simultaneous collection of data from aberration-corrected transmission electron microscopy (TEM), probe-corrected scanning transmission electron microscopy, ultrafast TEM, and dynamic TEM with a flexible in-situ testing chamber, where the entire instrument can be modified as future technologies are developed. The value would be to obtain a holistic understanding of the underlying physics and chemistry of the process-structure–property relationships in materials exposed to controlled extreme environments. Such a tool would permit the ability to explore, in-situ, the active reaction mechanisms in a controlled manner emulating those of real-world applications with nanometer and nanosecond resolution. If such a powerful tool is developed, it has the potential to revolutionize our materials understanding of nanoscale mechanisms and transients. Graphical Abstract: [Figure not available: see fulltext.].
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. This journal is
In this study, we report on the thermal conductivity of amorphous carbon generated in diamond via nitrogen ion implantation (N 3 + at 16.5 MeV). Transmission electron microscopy techniques demonstrate amorphous band formation about the longitudinal projected range, localized approximately 7 μm beneath the sample surface. While high-frequency time-domain thermoreflectance measurements provide insight into the thermal properties of the near-surface preceding the longitudinal projected range depth, a complimentary technique, steady-state thermoreflectance, is used to probe the thermal conductivity at depths which could not otherwise be resolved. Through measurements with a series of focusing objective lenses for the laser spot size, we find the thermal conductivity of the amorphous region to be approximately 1.4 W m-1 K-1, which is comparable to that measured for amorphous carbon films fabricated through other techniques.
In-situ transmission electron microscopy (TEM) provides an avenue to explore time-dependent nanoscale material changes induced by a wide range of environmental conditions that govern material performance and degradation. The In-situ Ion Irradiation TEM (I3TEM) at Sandia National Laboratories is a JEOL 2100 microscope that has been highly modified with an array of hardware and software that makes it particularly well suited to explore fundamental mechanisms that arise from coupled extreme conditions. Here, examples pertaining to multibeam ion irradiation, rapid thermal cycling, and nanomechanical testing on the I3TEM are highlighted, along with prospective advancements in the field of in-situ microscopy.
Islam, Zahabul; Barr, Christopher M.; Hattar, Khalid M.; Haque, Aman
In this study, we explore the interaction of electron wind force (EWF) with defects originating from ion irradiation in-situ inside a transmission electron microscope. Nanocrystalline gold specimens were self-ion irradiated to a dose of 5 × 1015 ions/cm2 (45 displacement per atom) to generate a high density of displacement damage. We also developed a molecular dynamics simulation model to understand the associated atomic scale mechanisms. Both experiments and simulations show that the EWF can impart significant defect mobility even at low temperatures, resulting in the migration and elimination of defects in a few minutes. We propose that the EWF interacts with defects to create highly glissile Shockley partial dislocations, which makes the fast and low temperature defect annihilation possible.
Guo, Qianying; Gu, Yucong; Barr, Christopher M.; Koenig, Thomas; Hattar, Khalid M.; Li, Lin; Thompson, Gregory B.
The incorporation of nanostructured and amorphous metals into modern applications is reliant on the understanding of deformation and failure modes in constrained conditions. To study this, a 105 nm crystalline Cu/160 nm amorphous Cu45Zr55 (at.%) multilayer structure was fabricated with the two crystalline layers sputter deposited between the top-middle-bottom amorphous layers and prepared to electron transparency. The multilayer was then in situ indented either under a single load to a depth of ~ 100 nm (max load of ~ 100 μN) or held at 20 μN and then repeatedly indented with an additional 5 μN up to 20,000 cycles in a transmission electron microscope to compare the deformation responses in the nanolaminate. For the single indentation test, the multilayer showed serrated load-displacement behavior upon initial indentation inductive of shear banding. At an indentation depth of ~ 32 nm, the multilayer exhibited perfect plastic behavior and no strain hardening. Both indented and fatigue-indented films revealed diffraction contrast changes with deformation. Subsequent Automated Crystal Orientation Mapping (ACOM) measurements confirmed and quantified global texture changes in the crystalline layers with specifically identified grains revealing rotation. Using a finite element model, the in-plane displacement vectors under the indent mapped conditions where ACOM determined grain rotation was observed, indicating the stress flow induced grain rotation. The single indented Cu layers also exhibited evidence of deformation induced grain growth, which was not evident in the fatigue-indented Cu based multilayer. Finally, the single indented multilayer retained a significant plastic crater in the upper most amorphous layer that directly contacted the indenter; a negligible crater impression in the same region was observed in the fatigued tested multilayer. These differences are explained by the different loading methods, applied load, and deformation mechanisms experienced in the multilayers.