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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 361 records · Page 20
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Native lattice strain induced structural earthquake in sodium layered oxide cathodes

Abstract High-voltage operation is essential for the energy and power densities of battery cathode materials, but its stabilization remains a universal challenge. To date, the degradation origin has been mostly attributed to cycling-initiated structural deformation while the effect of native crystallographic defects induced during the sophisticated synthesis process has been significantly overlooked. Here, using in situ synchrotron X-ray probes and advanced transmission electron microscopy to probe the solid-state synthesis and charge/discharge process of sodium layered oxide cathodes, we reveal that quenching-induced native lattice strain plays an overwhelming role in the catastrophic capacity degradation of sodium layered cathodes, which runs counter to conventional perception—phase transition and cathode interfacial reactions. We observe that the spontaneous relaxation of native lattice strain is responsible for the structural earthquake (e.g., dislocation, stacking faults and fragmentation) of sodium layered cathodes during cycling, which is unexpectedly not regulated by the voltage window but is strongly coupled with charge/discharge temperature and rate. Our findings resolve the controversial understanding on the degradation origin of cathode materials and highlight the importance of eliminating intrinsic crystallographic defects to guarantee superior cycling stability at high voltages.

25 ENERGY STORAGE↗
NASA NTRS1973

Correlation of creep rate with microstructural changes during high temperature creep

The techniques of electron microscopy were used to examine the microstructural changes which occur during primary creep for two important types of engineering alloys: (1) alloys strengthened by solid-solution additions, and (2) dispersion-strengthened alloys. The metals chosen for study are unalloyed titanium, Ti-6Al-4V, and the cobalt-base alloy, Haynes 188. Results to date on NGR 47-004-108 show that development of prior dislocation substructure in Haynes 188 by 10% prestrain and annealing for one hour at 1800 F increases the time to reach 0.5% creep strain at 1600 F by more than an order of magnitude for creep stresses from 3 to 20 ksi. For creep at 1800 F, similar results were obtaind for stresses above 7 ksi, but the prior substructure decreases creep resistance below 7 ksi. This effect appears to be related to instability of grain structure at 1800 F in prestrained material.

Young, C. T.↗
DOE OSTI2024

Microstructural evolution of compositionally complex solid-solution alloys under in-situ dual-beam irradiation

Here, this work attempts to link the microstructural evolution of single-phase compositionally complex alloy (CCA) compositions under dual-beam irradiation to their Mn-content via the stacking-fault energy (SFE) and vacancy migration energies. Two alloys, Cr 18 Fe 27 Mn 27 Ni 28 and Cr 15 Fe 35 Mn 15 Ni 35 , along with less compositionally complex pure Ni and Fe 56 Ni 44 binary were irradiated at 500 and 600 °C under dual-beam 1 MeV Kr 2+ and 16 keV He + heavy-ions up to 7 displacements per atom (dpa) with a He/dpa ratio of 0.75 %/dpa using in situ transmission electron microscopy (TEM). Due to the bubble-stabilizing effect of implanted He, bubbles were observed in all irradiations, and populations of faulted interstitial loops were characterized in Cr 18 Fe 27 Mn 27 Ni 28 and Cr 15 Fe 35 Mn 15 Ni 35 . A reduction in swelling was observed in the two CCAs compared to pure Ni and Fe 56 Ni 44 . Although swelling increased from 500 to 600 °C in Fe 56 Ni 44 , Cr 15 Fe 35 Mn 15 Ni 35 and Cr 18 Fe 27 Mn 27 Ni 28 both swelled slightly more at 500 °C. This was attributed to the difference in vacancy mobility, stronger pinning effect of vacancies on He, and the sink strength of faulted dislocation loops. Faulted interstitial loops nucleated with a higher number density and dislocation line density in Cr 15 Fe 35 Mn 15 Ni 35 at both temperatures, and at 600 °C in both materials. The differences in faulted loop population and temperature effect on swelling are correlated to the Mn-content and the measured SFE (20.2 ± 6.7 mJ/m 2 for Cr 18 Fe 27 Mn 27 Ni 28 and 9.2 ± 3.4 mJ/m 2 for Cr 15 Fe 35 Mn 15 Ni 35 ).

36 MATERIALS SCIENCE↗
DOE OSTI2024

Correlating microstructure and mechanical properties of harvested high dose Zorita light water reactor internals

Here, in this study, microstructural studies and micro-mechanical testing of an ex-plant material harvested from the decommissioned pressurized water reactor (PWR) is carried out. Irradiated 304 stainless steel (SS) components were harvested by the Electric Power Research Institute, U.S. Nuclear Regulatory Commission, and members of the José Cabrera Nuclear Power Station (Zorita) in Spain. The bi-crystalline micro-tensile specimens, atom probe tomography (APT) tips, and transmission electron microscopy (TEM) lamellae were fabricated from the baffle plate materials irradiated to 0.05, 15 and 50 dpa to elucidate microstructural, microchemical, and local mechanical properties changes as a function of dose. TEM and APT studies reveal radiation induced Ni, Cr, and Si rich precipitates in the 15 dpa sample that become smaller and partially redissolve into the matrix of the 50 dpa sample (decreasing size and number density). Dislocation loop and cavity number density and size were quantified as a function of dose as well as swelling. Intergranular Ni and Si enrichments with concomitant Fe and Cr depletion were observed in the 15 dpa sample and were more pronounced in the 50 dpa sample. Micro-tensile testing performed in the scanning electron microscope (SEM) at room temperature and 300 °C shows that the material's local yield strength and ultimate tensile strength decreases with increased dose and elevated test temperature and provides further insights via localized strain mapping. Current and previous mechanical data was compared with calculated values using the dispersed barrier hardening model with inputs of dislocation loops, precipitates, and cavities from microstructural characterization.

36 MATERIALS SCIENCE↗
NASA NTRS1981

Experiment K-314: Fetal and neonatal rat bone and joint development following in Utero spaceflight

Infant rat limb specimens from Soviet and U.S. ground-based studies were examined by radiography, macrophotography, histologic sectioning and staining and scanning electron microscopy. A comparison was conducted between vivarium and flight-type diets suggesting that nutritional obesity may adversely affect pregnancy. Data were obtained on maturation of ossification centers, orientation of collagen fibers in bone, tendon and ligaments, joint surface texture and spatial relationships of bones of the hind limb. Computer reconstructions of the knee and hip show promise as a means of investigating the etiology of congenital hip dislocation.

Sabelman, E. E.↗
NASA NTRS1975

Structure-property relationships in thermomechanically treated beryllia dispersed nickel alloys

BeO dispersed nickel alloys, produced by powder metallurgy techniques, were studied extensively in stress rupture at 815, 982, and 1093 C (1088, 1255, and 1366 K) and by transmission electron microscopy. The alloys were subjected to a variety of thermomechanical treatments (TMT) to determine the benefits of TMT on properties. It is shown that the use of intermediate annealing treatments after 10 pct reduction steps is highly beneficial on both low and high temperature properties. It is indicated that the high temperature strength is not primarily dependent on the grain aspect ratio or texture but depends strongly on the dislocation density and distribution of dislocations in a stable substructure which is pinned by the fine oxide dispersion.

Grewal, M. S.↗
DOE OSTI2020

Electron tomography imaging methods with diffraction contrast for materials research

Transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) enable the visualization of three-dimensional (3D) microstructures ranging from atomic to micrometer scales using 3D reconstruction techniques based on computed tomography algorithms. This 3D microscopy method is called electron tomography (ET) and has been utilized in the fields of materials science and engineering for more than two decades. Although atomic resolution is one of the current topics in ET research, the development and deployment of intermediate-resolution (non-atomic-resolution) ET imaging methods have garnered considerable attention from researchers. This research trend is probably not irrelevant due to the fact that the spatial resolution and functionality of 3D imaging methods of scanning electron microscopy (SEM) and X-ray microscopy have come to overlap with those of ET. In other words, there may be multiple ways to carry out 3D visualization using different microscopy methods for nanometer-scale objects in materials. From the above standpoint, this review paper aims to (i) describe the current status and issues of intermediate-resolution ET with regard to enhancing the effectiveness of TEM/STEM imaging and (ii) discuss promising applications of state-of-the-art intermediate-resolution ET for materials research with a particular focus on diffraction contrast ET for crystalline microstructures (superlattice domains and dislocations) including a demonstration of in situ dislocation tomography.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Ordering effects on deformation substructures and strain hardening behavior of a CrCoNi based medium entropy alloy

Here, a CrCoNi based medium entropy alloy with small additions of Ti, Al and Nb (denoted as (CrCoNi) 93 Al 4 Ti 2 Nb) in the as-quenched condition, exhibits tensile properties comparable to those of the equiatomic CrCoNi alloy at room temperature. Dark field transmission electron microscopy (TEM), atomic resolution high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) together with atom probe tomography (APT) show that spatially-localized long range ordering (LRO) L1 2 domains exist in this alloy. The evolution of deformation substructure with plastic deformation in this alloy was characterized using electron backscatter diffraction (EBSD), electron channeling contrast imaging (ECCI) and STEM based techniques including the recently developed weak beam dark field STEM imaging. Plastic deformation occurs by the slip of a/2<110>dislocations, which are narrowly dissociated into Shockley partial dislocations on {111} slip planes. Their dissociation distances in the (CrCoNi) 93 Al 4 Ti 2 Nb alloy are much smaller than the widths of the corresponding partials in the equiatomic CrCoNi alloy due to one or more of the minor alloying elements (Al, Ti, Nb). Dislocation slip in this alloy has a pronounced planar character. The leading dislocations in slip bands glide as pairs due to the existence of LRO domains. Multipoles were formed through the slip of dislocations with opposite signs on adjacent {111} slip planes. Those multipoles serve as building blocks for the formation of subgrain structures consisting of fine slip bands. The distances between slip bands were continuously refined during plastic deformation and dynamic refinement of slip bands plays a crucial role in strain hardening. The effects of LRO domains on planar dislocation slip, the deactivation of deformation twinning and strain hardening of this alloy are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Dynamics and structure of the B2→B19’ phase transformation in NiTi revealed through in situ 4D-STEM

The structural evolution of NiTi during the B2→B19’ martensitic phase transformation via thermal cycling is investigated using in situ four dimensional scanning transmission electron microscopy (4D-STEM). With 4D-STEM, we can directly visualize and quantify the nanoscale evolution of the martensitic structure on thermal cycling and also investigate the origin of diffuse scattering of NiTi in the pre-transitional state. Mapping of the martensite orientation and strain visualizes the progression of the transformation front and self-accommodation of the B19’ structure. Diffuse streaking and strain are measured in the pre-transitional austenite (B2) phase and demonstrate no localization or preferential directionality hinting that long-range homogeneous instability rather than nanoscale heterogeneities may be the origin of the pre-transitional anomalies in NiTi. Finally, it is revealed that NiTi does not reform the same martensite nanostructure on thermal cycling but does express similar features. This small variation is likely owing to transformation-induced dislocations.

36 MATERIALS SCIENCE↗
NASA NTRS1988

Studies of molecular-beam epitaxy growth of GaAs on porous Si substrates

GaAs has been grown on porous Si directly and on Si buffer layer-porous Si substrates by molecular-beam epitaxy. In the case of GaAs growth on porous Si, transmission electron microscopy (TEM) reveals that the dominant defects in GaAs layers grown on porous Si are microtwins and stacking faults, which originate from the GaAs/porous Si interface. GaAs is found to penetrate into the porous Si layers. By using a thin Si buffer layer (50 nm), GaAs penetration diminishes and the density of microtwins and stacking faults is largely reduced and localized at the GaAs/Si buffer interface. However, there is a high density of threading dislocations remaining. Both Si (100) aligned and four degree tilted substrates have been examined in this study. TEM results show no observable effect of the tilted substrates on the quality of the GaAs epitaxial layer.

Mii, Y. J.↗
DOE OSTI2025

Selenium Migration and Local Structures in Cu‐Doped CdSeTe Solar Cells after Aging

Selenium grading plays a critical role in state-of-the-art Cadmium Telluride photovoltaic cells by enhancing long-wavelength absorption and extending minority carrier lifetimes —key to enabling the current performance record of 23.08%. However, very little is understood about selenium motion. In this study, a comprehensive, multimodal, and multiscale approach is employed to investigate Se migration and local structural changes in copper (Cu)-doped CdSeTe solar cells subjected to accelerated stress. X-ray fluorescence (XRF) microscopy shows unexpected levels of Se diffusion after 500 h under heat (75°C) and light (0.8 suns, 80 mW/cm 2 ), suggesting the coexistence of fast and slow diffusion channels even at low temperatures, with unexpectedly low activation energies (<0.85 eV). X-ray Absorption Near Edge Structure (XANES) analysis indicates a preferential migration of Se atoms to anionic lattice sites and a reduction in Se-Cl co-passivation at Te-terminated dislocation cores. Furthermore, these findings point to a reconfiguration of Se local environments and highlight the potential role of extended structural defects in enabling Se transport at low temperatures. Additionally, XANES results suggest that the presence of metallic Cu across the absorber layer may contribute to back-contact degradation and reduced hole density in both fresh and aged devices.

14 SOLAR ENERGY↗
DOE OSTI2020

In-situ observation of nano-oxide and defect evolution in 14YWT alloys

Nanostructured ferritic alloys (NFAs) are considered as candidates for structural components in advanced nuclear reactors due to their excellent radiation resistance as a result of a high density of nano-oxides (NOs) in the microstructure. Therefore, gaining an understanding on the stability of NOs under irradiation is crucial. In this study, we have investigated the evolution of defects and NOs in 14YWT NFAs under in-situ Kr ion irradiation at room temperature (RT) and 450°C up to 10 dpa. It has been found that irradiations at 450°C do not create any changes in the NOs, similar to the bulk irradiations. On the other hand, elemental mapping indicates that NOs dissolve mostly after 10 dpa irradiations at RT. Thus, while defects are both annihilated and pinned by NOs at low doses (before the dissolution of NOs), glissile loops start to escape to the foil surface at high doses (after the dissolution of NOs), justifying the significantly low fraction of (111) loops compared to the literature values. Furthermore, high resolution transmission electron microscopy analysis has shown that the NOs are mostly coherent Y 2 Ti 2 O 7 particles with pyrochlore crystal structure after both RT and 450°C irradiations, similar to those observed before irradiation.

36 MATERIALS SCIENCE↗
DOE OSTI2021

In situ transmission electron microscopy with dual ion beam irradiation and implantation

To study the helium effects and their interactions with displacement damage in irradiated materials, an in situ dual-ion beam irradiation capability with transmission electron microscopy was recently established at the IVEM-Tandem Facility at Argonne National Laboratory. Pure nickel was irradiated in situ individually with 1 MeV Kr ions for displacement damage study, 16 keV He ions for helium implantation, and simultaneously with 1 MeV Kr ions and 16 keV He ions at the rate of 1 at.% He/dpa to study the interaction of helium and displacement damage at 500 degrees C. Helium bubbles were formed and segregated within dislocation loops during the He implantation experiment and no bubbles were observed outside the loops. The loop size increased with increasing helium concentration. In contrast, helium bubbles were formed uniformly in the matrix when nickel was irradiated simultaneously with 1 MeV Kr ions and 16 keV He ions. Overall, it is suggested that the uniformly-distributed defect clusters formed under 1 MeV Kr ion irradiation serve as trapping sites of helium atoms resulting in homogeneous nucleation of helium bubbles under the dualion beam irradiation in nickel.

36 MATERIALS SCIENCE↗
NASA NTRS1982

Pre- and post-annealing of mechanical damage in silicon wafers

Basic properties of mechanical damage in silicon consisting of cracks and abrasion were studied using transmission electron microscopy. The crystallographic structure of mechanical damage was determined before and after high temperature annealing. The main findings include that stresses in silicon around crack tips are not plastically relieved at room temperature and that abrasion at room temperature introduces shear loops into the silicon. It was also found that cracks of micron size can be annealed out, specifically, if cleavage occurs on 111 planes. The healing products of such cracks are 60 deg and 90 deg dislocations. Submicron cracks transform into stacking faults during annealing. Likewise high concentrations of shear loops due abrasion were found to anneal into stacking faults. A one to one correlation between surface areas containing small cracks and stacking faults was made. Measurements of damage removal on silicon surfaces through chemical-mechanical etching techniques are presented. It is shown that silicon dioxide repolishes damaged silicon surfaces most effectively.

Schwottke, G. H.↗
DOE OSTI2023

Creep strength boosted by a high-density of stable nanoprecipitates in high-chromium steels

There is a need worldwide to develop materials for advanced power plants with steam temperatures of 700°C and above that will achieve long-term creep-rupture strength and low CO 2 emissions. The creep resistance of actual 9-12Cr steels is not enough to fulfil the engineering requirements above 600°C. In this paper, the authors report their advances in the improvement of creep properties of this type of steels by the microstructural optimization through nano-precipitation using two methodologies. 1) Applying a high temperature austenitization cycle followed by an ausforming step (thermomechanical treatment, TMT) to G91 steel, to increase the martensite dislocation density and, thus, the number density of MX precipitates (M = V,Nb; X = C,N) but at the expense of deteriorating the ductility. 2) Compositional adjustments, guided by computational thermodynamics, combined with a conventional heat treatment (no TMT), to design novel steels with a good ductility while still possessing a high number density of MX precipitates, similar to the one obtained after the TMT in G91. The microstructures have been characterized by optical, scanning and transmission electron microscopy, EBSD and atom probe tomography. The creep behaviour at 700°C has been evaluated under a load of 200 N using small punch creep tests.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Report on Evolution of Inconel 718 Following HFIR Irradiation

The report presents the microstructure and mechanical properties of 3D printed Inconel 718 after irradiation in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL) to assess its potential use as a structural material. The structural components near the outlets of several proposed reactor cores will experience significant neutron fluxes and outlet coolant temperatures ranging from the hot standby temperature of 300 °C to nearly 550 °C at the center of the part. These components must support the core in appropriate loading conditions and require structural analysis at relevant temperatures. In FY21, three heat treatments were designed and conducted to simplify the microstructure and to determine how each precipitating phase contributed to the overall strength. In FY21, baseline mechanical properties were measured from uniaxial tensile tests on subsize SS-J2 specimens at room temperature and at elevated temperatures of 300, 450, and 600 °C to serve a comparison to the irradiated properties. Four capsules containing 3D printed Inconel 718 were inserted into HFIR in FY21 for a matrix of two temperatures and two doses. The lower of the two doses was available for characterization in FY22. Multiple heat treatments of Inconel 718 irradiated to nominal conditions of 2 displacements per atom (dpa) at either 300 or 600 °C were strained with uniaxial tensile tests at the Irradiated Material Examination and Testing (IMET) Facility to discern the mechanical properties. Transmission electron microscopy was performed to correlate the observed mechanical properties with nanoscale features. The initially homogenous AM718-HM increased in strength at both irradiation temperatures based on a high density of nanometer-scale radiation-induced cavities at lower temperature and nucleation and growth of γ" precipitates at higher temperatures. The precipitate-hardened AM718-HT2 showed very small differences in strength before and after irradiation: the contribution to strength from γ" precipitates was replaced with dislocation loops. Because the radioactivity of the nickel superalloys from neutron activation limited the scope of the analysis, a feasibility study examined the possibility of an ultra-miniature specimen geometry, colloquially SS-Tiny (SS-T), for mechanical property determination using the nonirradiated Inconel 718. This study found an overestimation of ductility from the SS-T geometry with yield strength and ultimate tensile strength slightly above the SS-J2 geometry: this could be contributed to a reduction in specimen thickness.

36 MATERIALS SCIENCE↗
DOE OSTI2023

In-situ investigation of strengthening and strain hardening mechanisms of Cu-added medium-Mn steels by synchrotron-based high-energy X-ray diffraction

A novel Cu-added medium-Mn steel with a chemical composition of Fe–0.27C–9.1Mn–1.86Al–3.3Cu (wt.%) was designed and subjected to intercritical annealing (IA) temperature range from 620 °C to 680 °C for 1 h. The ultimate tensile strength (UTS) increases and the yielding strength (YS) decreases with the IA temperature increasing. The YS of 824 MPa, UTS of 1222 MPa, total elongation (TE) of 55%, and product of strength and elongation (PSE) of 67.2 GPa·% are achieved after IA at 660 °C. Transmission electron microscopy confirmed that Cu-rich nanoparticles precipitate in the ferrite. The in-situ high-energy X-ray diffraction (HE-XRD) experiments show that at the beginning of plastic deformation, both austenite and ferrite bear the applied load. The load is mainly undertaken by martensite with effective transformation-induced plasticity (TRIP) effect triggered. The YS of ferrite is significantly higher than that of austenite. The individual contribution of solid solution strengthening, grain refinement strengthening, dislocation strengthening, and precipitation strengthening in ferrite and austenite is analyzed. The discrepancy between the YS of ferrite and austenite is mainly attributed to the precipitation strengthening due to the Cu-rich nanoparticles precipitation. The moderate mechanical stability and the collaboration of TRIP and twinning-induced plasticity (TWIP) effects of austenite contributed to the enhanced strain hardening capability and resulted in large ductility.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Evolution of microstructure and strength of a high entropy alloy undergoing the strain-induced martensitic transformation

In a recent work, we have reported outstanding strength and work hardening exhibited by a metastable high entropy alloy (HEA), Fe 42 Mn 28 Co 10 Cr 15 Si 5 (in at. %), undergoing the strain-induced martensitic transformation from metastable gamma austenite (γ) to stable epsilon martensite (ε). However, the alloy exhibited poor ductility, which was attributed to the presence of the brittle sigma (σ) phase in its microstructure. The present work reports the evolution of microstructure, strength, and ductility of a similar HEA, Fe 38.5 Mn 20 Co 20 Cr 15 Si 5 Cu 1.5 (in at. %), designed to suppress the formation of σ phase. A cast and then rolled plate of the alloy was processed into four conditions by annealing for 10 and 30 min at 1100 °C and by friction stir processing (FSP) at tool rotation rates of 150 and 400 revolutions per minute (RPM) to facilitate detailed examinations of variable initial grain structures. Neutron diffraction and electron microscopy were employed to characterize the microstructure and texture evolution. The initial materials had variable grain size but nearly 100% γ structure. Diffusionless strain induced γ→ε phase transformation took place under compression with higher rate initially and slower rate at the later stages of deformation, independent on the initial grain size. The transformation facilitated part of plastic strain accommodation and rapid strain hardening owing to a transformation-induced dynamic Hall-Petch-type barrier effect, increase in dislocation density, and texture. Here, the peak strength of nearly 2 GPa was achieved under compression using the structure created by double pass FSP (150 RPM followed by 150 RPM). Remarkably, the tensile elongation exhibited by the alloy was nearly 20% with fracture surfaces featuring a combination of ductile dimples and cleavage.

36 MATERIALS SCIENCE↗