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Results for “dislocation microscopy”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Orientation-Dependent Nanomechanical Behavior of Pentaerythritol Tetranitrate as Probed by Multiple Nanoindentation Tip Geometries

Nanoindentation can be leveraged to aid in the high fidelity modeling of dislocation mediated plasticity in pentaerythritol tetranitrate (PETN), an anisotropic energetic molecular crystal. Moreover, nanoindentation tip parameters such as tip geometry, size, and degree of acuity can be utilized to target anisotropic behavior. In this work, nanoindentation was conducted across a range of orientations on the (110) face of PETN to characterize resultant yield behavior, mechanical property measurements, and resultant slip behavior and fracture initiation. Three different indentation tips were utilized: a 3-sided pyramidal Berkovich tip, a 4-sided high aspect ratio Knoop tip, and a 90° conical tip. Ultimately, indenter tip radius was documented to impact yield behavior, whereas tip geometry affected larger scale processes such as slip, and tip acuity was the dominating factor that led to fracture. The axisymmetric conical tip, serving as a baseline, showed the least amount of variation in mechanical property measurements but also the largest distribution of maximum shear stress at which initial yielding occurred. Its high degree of acuity, however, was more prone to induce fracture at higher loads. The Knoop tip was shown to be suitable for average measurements, but also for elucidation of certain anisotropic features. A distinctly higher perceived hardness at 45° was measured with the Knoop tip, indicating less dislocation motion in that direction also observed in this work via scanning probe microscopy. Lastly, the commonly used Berkovich tip was a good compromise whereby it provided a representative volume element describing the average behavior of the material. These results can be utilized to target desired anisotropic behavior in a wider range of molecular crystals, as well as to inform theoretical considerations for dislocation mediated plasticity in PETN.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Disorder-induced suppression of charge density wave order: STM study of Pd-intercalated ErTe 3

Pd-intercalated ErTe3 is studied as a model system to explore the effect of increasing disorder on an incommensurate two-component charge density wave (CDW). The ordering vectors of the CDW components lie along the two in-plane principal axes of the nearly tetragonal crystal structure. Using scanning tunneling microscopy (STM), we show that introducing Pd intercalants (i.e., disorder) induces CDW dislocations, which appear to be associated with each CDW component separately. Increasing Pd concentration has a stronger effect on the secondary CDW order, manifested in a higher density of dislocations, and thus increases the anisotropy (nematic character) of the CDW. Suggestive evidence of Bragg glass phases at weak disorder is also discussed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Activating dislocation mediated plasticity in boron carbide through Al-doping

Dislocation slip, deformation twinning, phase transformations, and fast fracture are energy dissipation mechanisms that accommodate mechanical loading in materials. The energetically unfavorable formation of dislocation attributes to the ease of cracking and the low damage tolerance observed in superhard ceramics, notably boron carbide. Here, this work demonstrates that room temperature dislocation slip can be enabled in boron carbide by altering its chemistry through Al doping. The activation of dislocation slip is mechanistically explained by quantum mechanics simulations and electron microscopy, which indicate that strain energy is released through basal icosahedral slip facilitated by icosahedral rotation and chain bond breaking and reconfiguring. The new insight gained through this work suggests that atomic doping could be an effective strategy to tune deformation mechanisms in boron carbide, which provides a significant potential for limiting amorphization and catastrophic failure, and opens a new strategy to enhance damage tolerance in brittle ceramics.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Creep properties of advanced austenitic steel 709 determined through short experiments under in-situ neutron diffraction followed by TEM characterization

Here in this study, the creep mechanisms at play in Alloy 709 (Fe-20Cr-25Ni) are investigated by performing short-term creep-type tests under in-situ neutron diffraction experiments. Short tests are performed in the temperature range of 500 to 900 °C under constant load with a load ranging from 50 to 150 MPa. The creep exponent and activation energy are determined using the Bird-Mukherjee-Dorn relation and compared to that obtained from conventional longer creep tests from the literature. Scanning transmission electron microscopy (S/TEM) of the post-creep microstructure indicates that interaction of dislocations with precipitates are a dominant mechanism at play. Furthermore, local elemental mapping indicated chemical segregation at grain boundaries and formation of complex precipitates.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Enhancing fatigue life by ductile-transformable multicomponent B2 precipitates in a high-entropy alloy

Catastrophic accidents caused by fatigue failures often occur in engineering structures. Thus, a fundamental understanding of cyclic-deformation and fatigue-failure mechanisms is critical for the development of fatigue-resistant structural materials. Here we report a high-entropy alloy with enhanced fatigue life by ductile-transformable multicomponent B2 precipitates. Its cyclic-deformation mechanisms are revealed by real-time in-situ neutron diffraction, transmission-electron microscopy, crystal-plasticity modeling, and Monte-Carlo simulations. Multiple cyclic-deformation mechanisms, including dislocation slips, precipitation strengthening, deformation twinning, and reversible martensitic phase transformation, are observed in the studied high-entropy alloy. Its improved fatigue performance at low strain amplitudes, i.e., the high fatigue-crack-initiation resistance, is attributed to the high elasticity, plastic deformability, and martensitic transformation of the B2-strengthening phase. This study shows that fatigue-resistant alloys can be developed by incorporating strengthening ductile-transformable multicomponent intermetallic phases.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Five-second STEM dislocation tomography for 300 nm thick specimen assisted by deep-learning-based noise filtering

Scanning transmission electron microscopy (STEM) is suitable for visualizing the inside of a relatively thick specimen than the conventional transmission electron microscopy, whose resolution is limited by the chromatic aberration of image forming lenses, and thus, the STEM mode has been employed frequently for computed electron tomography based three-dimensional (3D) structural characterization and combined with analytical methods such as annular dark field imaging or spectroscopies. However, the image quality of STEM is severely suffered by noise or artifacts especially when rapid imaging, in the order of millisecond per frame or faster, is pursued. Here we demonstrate a deep-learning-assisted rapid STEM tomography, which visualizes 3D dislocation arrangement only within five-second acquisition of all the tilt-series images even in a 300 nm thick steel specimen. The developed method offers a new platform for various in situ or operando 3D microanalyses in which dealing with relatively thick specimens or covering media like liquid cells are required.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

Multimodal microscopy of extended defects in β-Ga 2 O 3 (010) EFG crystals

Beta-phase gallium oxide (β-Ga 2 O 3 ) has attracted attention in recent years as a potentially low cost, large area substrate and active layer material for high power, high temperature power electronics and sensing devices. However, growth of β-Ga 2 O 3 crystals is complicated by easily activated (100) and (001) cleavage planes, the presence of low angle grain boundaries (LAGBs) and twins, and the potential formation of polycrystalline grains. In this study, β-Ga 2 O 3 crystals were grown by the edge-defined film-fed growth technique with an (010) principal face. Two crystals with apparently randomly formed high angle grain boundaries (HAGBs) were selected and analyzed by electron backscatter diffraction, electron channeling contrast imaging, and cathodoluminescence to investigate the nature of the LAGBs and the source of the HAGB formation. It was discovered that planar LAGBs lying parallel to the (010) plane exist in the region immediately preceding the start of an HAGB. Increased misorientation across the LAGB was observed, approaching the initiation of a new grain. We present multimodal microscopy characterization, correlating misorientation and variation in optoelectronic properties with LAGBs and the associated dislocations.

14 SOLAR ENERGY↗
DOE OSTI2022

Thermal diffusivity recovery and defect annealing kinetics of self-ion implanted tungsten probed by insitu transient grating spectroscopy

Tungsten is a promising candidate material for plasma-facing armour components in future fusion reactors. A key concern is irradiation-induced degradation of its normally excellent thermal transport properties. In this comprehensive study, thermal diffusivity degradation in ion-implanted tungsten and its evolution from room temperature (RT) to 1073 K is considered. Five samples were exposed to 20 MeV self-ions at RT to achieve damage levels ranging from 3.2 x 10 -4 to 3.2 displacements per atom (dpa). Transient grating spectroscopy with in-situ heating was then used to study thermal diffusivity evolution as a function of temperature. Using a kinetic theory model, an equivalent point defect density is estimated from the measured thermal diffusivity. The results showed a prominent recovery of thermal diffusivity between 450 K and 650 K, which coincides with the onset of mono-vacancy mobility. After 1073 K annealing samples with initial damage of 3.2 x 10 -3 dpa or less recover close to the pristine value of thermal diffusivity. For doses of 3.2 x 10 -2 dpa or higher, on the other hand, a residual reduction in thermal diffusivity remains even after 1073 K annealing. Transmission electron microscopy reveals that this is associated with extended, irradiation-induced dislocation structures that are retained after annealing. A sensitivity analysis shows that thermal diffusivity provides an efficient tool for the assessing total defect content in tungsten up to 1000 K.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Deformation mechanisms in an additively manufactured dual-phase eutectic high-entropy alloy

Nanostructured metals and alloys often exhibit high strengths but at the expense of reduced ductility. Through harnessing the far-from-equilibrium processing conditions of laser powder-bed fusion (L-PBF) additive manufacturing, we develop a dual-phase nanolamellar structure comprised of FCC/L1 2 and BCC/B2 phases in a Ni 40 Co 20 Fe 10 Cr 10 Al 18 W 2 eutectic high-entropy alloy (EHEA), which exhibits a combination of ultrahigh yield strength (>1.4 GPa) and large tensile ductility (~17%). The deformation mechanisms of the additively manufactured EHEA are studied via in-situ synchrotron X-ray diffraction and high-resolution transmission electron microscopy. The high yield strength mainly results from effective blockage of dislocation motion by the high density of lamellar interfaces. The refined nanolamellar structures and low stacking fault energy (SFE) promote stacking fault (SF)-mediated deformation in FCC/L1 2 nanolamellae. The accumulation of abundant dislocations and SFs at lamellar interfaces can effectively elevate local stresses to promote dislocation multiplication and martensitic transformation in BCC/B2 nanolamellae. The cooperative deformation of the dual phases, assisted by the semi-coherent lamellar interfaces, gives rise to the large ductility of the as-printed EHEA. In addition, here we also demonstrate that post-printing heat treatment allows us to tune the non-equilibrium microstructures and deformation mechanisms. After annealing, the significantly reduced SFE and thicknesses of the FCC nanolamellae facilitate the formation of massive SFs. The dissolution of nano-precipitates in the BCC/B2 nanolamellae reduces spatial confinement and further promotes martensitic transformation to enhance work hardening. Our work provides fundamental insights into the rich variety of deformation mechanisms underlying the exceptional mechanical properties of the additively manufactured dual-phase nanolamellar EHEAs.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Long-term thermal aging behavior and strength reduction in a laser powder bed fusion 316H stainless steel

The long-term thermal stability of structural alloys is essential for ensuring the safe and reliable operation of nuclear reactors and other power plants. While extensive research has explored the effects of thermal aging on conventional stainless steels, the behavior of additively manufactured (AM) alloys remains less understood. This study examines the thermal aging response of laser powder bed fusion (LPBF) 316H stainless steel (SS) at temperatures ranging from 550 °C to 750 °C over durations of up to 10,000 h (approximately 1.14 years). Advanced characterization techniques, including electron microscopy and synchrotron X-ray diffraction, were used to investigate dislocation recovery and phase evolution. Based on these findings, a time-temperature-precipitation (TTP) diagram was developed for LPBF 316H SS, revealing a 10- to100-fold acceleration in precipitation kinetics compared to wrought 316H SS. A physics-informed model was calibrated using the short-term experimental data, enabling predictions of average precipitate sizes, volume fractions of M 23 C 6 and Laves phases, and changes in molybdenum solute concentration for aging up to 1 × 10⁶ h (114 years). These microstructural insights were further utilized to estimate yield strength and extrapolate strength reduction factors over the extended aging period. Despite the accelerated aging kinetics, LPBF 316H SS demonstrated superior yield strength retention compared to its wrought counterpart. In conclusion, this study establishes a framework for evaluating long-term performance using short-term experimental data and supports the accelerated qualification of AM materials for high-temperature structural applications.

Laser powder bed fusion↗
DOE OSTI2021

Effects of helium on irradiation response of reduced-activation ferritic-martensitic steels: Using nickel isotopes to simulate fusion neutron response

Understanding the effects of helium on microstructures and mechanical properties of reduced-activation ferritic-martensitic steels is important to use of these steels in fusion reactor structures. The 9Cr-2WVTa steels were doped with 58Ni and 60Ni isotopes at 2 weight percent to control the rate of transmutation helium generation. The samples were irradiated in the High Flux Isotope Reactor to ~24 displacements per atom at nominal temperatures of 300, 400, and 500°C, producing 228 and 7 atomic parts-per-million helium in the 58 Ni- and 60 Ni-doped samples, respectively. Transmission electron microscopy revealed a variety of precipitates and the radiation-induced dislocation loops and cavities (voids or helium bubbles). Tensile tests of the irradiated samples at the irradiation temperatures showed radiation-induced hardening at 300°C and radiation-induced softening at 400°C. Analysis indicates that the hardening primarily originated from the loops and cavities. The 58 Ni-doped samples had greater strengthening contributions from loops and cavities, leading to higher hardening with lower ductility than the 60 Ni-doped samples. The greater helium production of 58 Ni did not show pronounced reductions in ductility of the samples.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Role of mechanical stress localizations on the radiation hardness of AlGaN/GaN high electron mobility transistors

Multi-material, multi-layered systems such as AlGaN/GaN high electron mobility transistors (HEMTs) contain residual mechanical stresses that arise from sharp contrasts in device geometry and materials parameters. These stresses, which can be either tensile or compressive, are difficult to detect and eliminate because of their highly localized nature. We propose that their high-stored internal energy makes potential sites for defect nucleation sites under radiation, particularly if their locations coincide with the electrically sensitive regions of a transistor. In this study, we validate this hypothesis with molecular dynamic simulation and experiments exposing both pristine and annealed HEMTS to 2.8 MeV Au +3 irradiation. Our unique annealing process uses mechanical momentum of electrons, also known as the electron wind force (EWF) to mitigate the residual stress at room temperature. High-resolution transmission electron microscopy and cathodoluminescence spectra reveal the reduction of point defects and dislocations near the two-dimensional electron gas region of EWF-treated devices compared to pristine devices. The EWF-treated HEMTs showed relatively higher resilience with approximately 10% less degradation of drain saturation current and ON-resistance and 5% less degradation of peak transconductance. Both mobility and carrier concentration of the EWF-treated devices were less impacted compared to the pristine devices. Our results suggest that the lower density of nanoscale stress localization contributed to the improved radiation tolerance of the EWF-treated devices. Intriguingly, the EWF is found to modulate the defect distribution by moving the defects to electrically less sensitive regions in the form of dislocation networks, which act as sinks for the radiation induced defects and this assisted faster dynamic annealing.

AlGaN/GaN HEMTs↗
DOE OSTI2020

Quantifying dislocation density in Al-Cu coatings produced by cold spray deposition

This work quantifies the plastic deformation in terms of dislocation density for a series of cold sprayed Al-Cu coatings with copper contents from 2 mass% to 5 mass%. The success of the deposition and consolidation of the feedstock powders during the cold spray process rely on the occurrence of significant plastic deformation. Inert gas atomized Al-Cu alloy powders were sprayed onto substrates made of an Al-Cu-Mg-Mn alloy (AA2024) to produce dense coatings using a low pressure cold spray system with helium as the carrier gas. X-ray diffraction patterns were obtained from the Al-Cu feedstock powder material and the cold sprayed coatings using a monochromatic X-ray source, and the dislocation density was determined via an X-ray whole profile analysis. Increasing the Cu alloy content (from 2 mass% to 5 mass%) systematically increased the dislocation density in the Al-Cu coatings from (4.3 ± 0.5) × 10 14 m -2 to (7.5 ± 0.8) × 10 14 m -2 . The dislocation densities in the feedstock powders ranging from (0.4 ± 0.1) × 10 14 m -2 to (1.8 ± 0.2) × 10 14 m -2 were all lower than the dislocation densities in the corresponding coatings. The increasing deformation level in the Al-Cu coatings with Cu additions were confirmed by the classic and modified Williamson-Hall analyses of X-ray diffraction data, and peak breadth measurements from neutron diffraction data. Finally, a high density of dislocations was also observed in these coatings via electron backscatter diffraction and transmission electron microscopy.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Coalescence of GaP on V-Groove Si

In recent years, better understanding and control over the formation of crystalline defects during the direct epitaxy of III-V semiconductors on Si substrates via metal organic vapor phase epitaxy (MOVPE) has enabled large gains in III-V-on-Si solar cell efficiency, pointing to pathway to lower-cost, high-performance III-V solar cells. However, such results have only been achieved on costly chemo-mechanically-polished (CMP) Si wafers. The use of V-groove nanopatterned Si substrates has demonstrated similarly high-crystalline-quality III-V-on-Si epitaxy, but also can be combined with lower-cost polishing techniques. Although they offer a potential cost advantage, growth on V-groove substrates adds challenges not present for epitaxy on planar wafers (the III-V material must be coalesced into a thin film after an initial nucleation stage). MOVPE growth conditions that promote highly facet-selective lateral growth needed for coalescence are generally actively avoided for conventional thin fim growth, so growth conditions need to be re-developed for V-groove-based epitaxy. Additionally, coalescence add complexity to the dislocation dynamics related to lattice relaxation, so strategies used to keep threading dislocation density (TDD) low on planar substrates need to be re-tuned for V-grooves. We have studied the morphological evolution and dislocation dynamics of GaP grown on V-groove Si by MOVPE. Growth conditions of V/III=5,000 and Tg=800 degrees C were uniquely found to produce extremely smooth coalesced thin films, with an RMS roughness of 0.2 nm measured by AFM. Additionally, at this growth condition, we identified two regimes of growth determined by the width of the SiNx cap (a remnant of the nanopatterning process) at the top of the V-grooves. For narrow caps, the GaP coalesces into a thin film, and for wide caps, the GaP evolves into {1 1 1}-faceted diamonds that do not coalesce. We suggest the influence of Si from the sidewalls of the V-grooves on the surface reconstruction of the GaP as the mechanism for this effect, with reflection difference spectroscopy (RDS) and Si doping experiments supporting this theory. In addition to morphology, the dislocation dynamics of the system were studied with electron channeling contrast imaging (ECCI) and transmission electron microscopy (TEM). The TDD of the coalesced GaP films was found to be 5 x 10^7 cm^-2 after coalescence via ECCI, a level still too high for high-quality solar cells. However, misfit dislocations crossing multiple grooves greater than 20 micrometers long were observed in ECCI, suggesting that the V-grooves do not block dislocation glide. TEM prior to and after coalescence was used to distinguish between dislocation creation driven by growth conditions and coalescence. Finally, strategies to reduce the dislocation density to levels acceptable for solar cells will be discussed.

GaP↗
DOE OSTI2022

Influence of strain and dislocations on GaSb/GaAs quantum dots: From nested to staggered band alignment

We investigate the influence of strain and dislocations on band alignment in GaSb/GaAs quantum dot systems. Composition profiles from cross-sectional scanning tunneling microscopy images are interpolated onto a finite element mesh in order to calculate the distribution of local elastic strain, which is converted to a spatially varying band alignment using deformation potential theory. Our calculations predict that dislocation-induced strain relaxation and charging lead to significant local variations in band alignment. Furthermore, misfit strain induces a transition from a nested (type I) to a staggered (type II) band alignment. Although dislocation-induced strain relaxation prevents the type I to type II transition, electrostatic charging at dislocations induces the staggered band alignment once again.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2020

STEM Characterization of Dislocation Loops in Irradiated FCC Alloys

In this study, we demonstrate the methodology systematically developed for dislocation loop (perfect and faulted loops) imaging and analysis in irradiated face-centered-cubic (FCC) alloys using scanning transmission electron microscopy (STEM). On-zone [001] STEM imaging was identified as the preferred choice for its accuracy and effectiveness based on the comparison with other dislocation loop imaging techniques including: (i) on-zone STEM imaging using other major low-index zone axes, (ii) kinematic two-beam conditions bright field imaging near the [001] zone axis in conventional TEM (CTEM) mode, and (iii) Rel-Rod CTEM dark-field (DF) imaging near the [011] zone axis. The effect of STEM collection angle on the contrast formation of dislocation loops was also investigated. The developed method was confirmed by imaging all populations of perfect and faulted loops of types a/2$\langle$110$\rangle${110} and a/3$\langle$111$\rangle${111} found in an ion irradiated Ni40Fe40Cr20 alloy. The proposed STEM-based technique can easily identify said loops with a size greater than 10 nm without any assumptions such as those commonly made using the conventional Rel-Rod CTEM-DF technique. The recommended methodology in this study is developed as a quick and convenient tool that can be generally applied to irradiated FCC-based materials due to their common crystallography.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Correlative STEM-APT characterization of radiation-induced segregation and precipitation of in-service BWR 304 stainless steel

In this study, radiation induced segregation and precipitation phenomena in an in-service boiling water reactor 304 stainless steel component were investigated using directly correlated 3D-atom probe tomography and scanning transmission electron microscopy. Significant quantitative differences in measured segregation at grain boundaries were found between the atom probe and energy dispersive spectroscopy measurements of the exact same locations. In particular, a much stronger Si segregation (~10 atomic% via atom probe versus ~4 atomic% via electron microscopy) and different Cr profile shapes were detected that are critical to models of radiation induced segregation and stress corrosion cracking behavior. These quantitative differences highlight the need for comparative microscopy and critical evaluation of limitations in each analytical method. Elemental segregation to dislocations and conjoined-clusters were also highlighted by atom probe; confirming and expanding upon what has been observed in test reactor neutron and accelerator-based ion irradiations.

36 MATERIALS SCIENCE↗
DOE OSTI2022

High-temperature deformation mechanisms in a BCC+B2 refractory complex concentrated alloy

The current study reports the analysis of the deformation mechanisms at 600 °C in a two-phase, BCC+B2, refractory complex concentrated alloy (RCCA) Al 0.5 NbTa 0.8 Ti 1.5 V 0.2 Zr. At this temperature, the alloy microstructure is unstable and dynamic coarsening of B2 precipitates is evidenced during the mechanical testing. After true plastic strain of 0.030 at strain rate of 10 -4 s -1 , the deformation becomes highly localized in wavy bands reflecting the profusion of cross-slip. Scanning transmission electron microscopy (STEM) observations highlight the presence of paired a/2$\langle$111$\rangle$ dislocations that shear the B2 precipitates in a cooperative process. Additionally, some chemical segregation effect is observed along the narrow dislocation bands likely induced to decrease the antiphase boundary (APB) energy of the system.

ordering↗