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At least 415 records · Page 23
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Crystal Plasticity Simulation of Magnesium and Its Alloys: A Review of Recent Advances

Slip and extension twinning are the dominant deformation mechanisms in Magnesium (Mg) and its alloys. Crystal plasticity is a powerful tool to study these deformation mechanisms. Different schemes have incorporated crystal plasticity models to capture different properties, which vary from the simple homogenization Taylor model to the full-scale crystal plasticity finite element model. In the current study, a review of works available in the literature that addresses different properties of Mg and its alloys using crystal plasticity modes is presented. In addition to slip and twinning, detwinning is another deformation mechanism that is activated in Mg and its alloys. The different models that capture detwinning will also be addressed here. Finally, the recent experimental frameworks, such as in-situ neutron diffraction, 3D high energy synchrotron X-ray techniques, and digital image correlation under scanning electron microscopy (SEM-DIC), which are incorporated along crystal plasticity models to investigate the properties of Mg and its alloys, are addressed. Future research directions towards improving the deformation response of Mg and its alloys are identified, which can lead to increased deployment of the lightest structural metal in engineering applications.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Electron beam irradiation effects on bulk metals: a comparative study of polycrystalline versus single-crystalline structures

This study investigates the effects of electron beam (e-beam) irradiation on the mechanical and structural properties of eight bulk metallic samples, comprising both polycrystalline (PC) and single-crystalline (SC) forms of Ni, Cr, V, and Ti. These metals were evaluated as potential candidates for beam exit windows in high-power (MW-class) particle accelerators. The primary objective is to identify metals capable of withstanding the conditions of high-power/MW-class e-beam accelerators and serve effectively as exit windows. Selection criteria were based on each metal’s intrinsic properties, power dissipation capability, and irradiation-induced changes in mechanical behavior, including hardness, elastic modulus, and defect density. Comprehensive characterization was conducted using field-emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM–EDS), X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and nanoindentation, performed both before and after exposure to a ~¿66 kGy dose from a 10 MeV e-beam accelerator. Results revealed that e-beam irradiation induced hardening in PC Ni, whereas PC Ti, commonly used in beam exit windows, exhibited softening. The observed softening in PC Ti is attributed to grain coarsening, elongation, and the formation of twins and twin boundaries, in contrast to the smaller, compressed grains in the pristine (Pr) PC Ti samples, consistent with the Hall–Petch relationship. The stresses due to twinning are small and insignificant in influencing the overall hardening of the PC Ti irradiated sample when compared to the stresses due to the dislocation density. Conversely, SC Ti samples exhibited irradiation-induced hardening. The SC Ti irradiated samples developed additional irradiation-induced modifications in crystallographic texture of (100), (101), (110), (200), (112), (004), and (211) as evidenced from the XRD results, which could probably explain the hardening effect that is caused by irradiation.

36 MATERIALS SCIENCE↗
NASA NTRS1982

Fatigue and creep-fatigue deformation of several nickel-base superalloys at 650 C

Transmission electron microscopy has been used to study the bulk deformation characteristics of seven nickel-base superalloys tested in fatigue and creep-fatigue at 650 C. The alloys were Waspalloy, HIP Astroloy, H plus F Astroloy, H plus F Rene 95, IN 100, MERL 76, and NASA IIB-7. The amount of bulk deformation observed in all the alloys was low. In tests with inelastic strain amplitudes less than about 0.003, only some grains exhibited yielding and the majority of those had the 110 line near the tensile axis. Deformation occurred on octahedral systems for all of the alloys except MERL 76 which also showed abundant primary cube slip. Creep-fatigue cycling occasionally produced extended faults between partial dislocations, but otherwise deformation was much the same as for fatigue cycling.

Miner, R. V.↗
DOE OSTI2025

Generalizable Image Segmentation for Microstructure Characterization Through Integrated SEM and EBSD Analysis

We demonstrate generalizable semantic segmentation using minimal ground truth data. Correlated scanning electron microscopy (SEM) images and electron backscatter diffraction (EBSD) measurements of frictionstir processed 316L stainless steel plates were used to train deep learning models for grain boundary segmentation. Secondary electron (SE) imaging taken at an accelerating voltage of 10 keV correlated to EBSD-derived grain boundaries produced the best performing model. Notably, an ensemble of three models trained on a single SE image produced accurate segmentation over a series of BSE images of samples manufactured under different processing parameters, with a resultant mean absolute error in grain size of 0.34 µm. The striking generalizability of the models likely results from the similar escape depths of the SE training input and the EBSD training output and the reduced probability of dislocation artifacts appearing in the image. This finding highlights the importance of considering the physical principles behind imaging in the development of robust segmentation models for microstructure characterization.

Taufique, Mohammad Fuad Nur↗
DOE OSTI2021

Precipitation Hardening in Ferroelectric Ceramics

Domain wall motion in ferroics, similar to dislocation motion in metals, can be tuned by well-concepted microstructural elements. In demanding high-power applications of piezoelectric materials, the domain wall motion is considered as a lossy hysteretic mechanism that should be restricted. Current applications for so-called hard piezoelectrics are abundant and hinge on the use of an acceptor-doping scheme. However, this mechanism features severe limitations due to enhanced mobility of oxygen vacancies at moderate temperatures. By analogy with metal technology, the authors present here a new solution for electroceramics, where precipitates are utilized to pin domain walls and improve piezoelectric properties. Through a sequence of sintering, nucleation, and precipitate growth, intragranular precipitates leading to a fine domain structure are developed as shown by transmission electron microscopy, piezoresponse force microscopy, and phase-field simulation. This structure impedes the domain wall motion as elucidated by electromechanical characterization. As a result, the mechanical quality factor is increased by ≈50% and the hysteresis in electrostrain is suppressed considerably. This is even achieved with slightly increased piezoelectric coefficient and electromechanical coupling factor. This novel process can be smoothly implemented in industrial production processes and is accessible to simple laboratory experimentation for microstructure optimization and implementation in various ferroelectric systems.

36 MATERIALS SCIENCE↗
DOE OSTI2023

In-Situ Transmission Electron Microscopy Study of the Evolution of Extended Defects in Oxide Nuclear Fuels

In-situ transmission electron microscopy (TEM) with simulated extreme environments is an effective tool for understanding and tracking microstructural changes down to the atomic scale. The objective of this research is to study the effect of temperature on the evolution of extended defects in ThO2 and UO2. Here, we present in-situ TEM isochronal thermal annealing experiments using a micro-electro-mechanical-system (MEMS)-based heating holder. ThO2 and UO2 single crystal specimens were grown inside an inert silver ampoule using hydrothermal synthesis. Both samples were irradiated using 2 MeV protons at 600oC up to 0.1 dpa at Texas A&M University’s Accelerator Laboratory. Fig. 1a shows a weak-beam dark field TEM image of ThO2 after irradiation, indicating the presence of faulted 1/3 <111> type dislocation loops. This presentation will discuss the effect of annealing temperature (600oC, 800oC, 1000oC, 1100oC, etc.) on dislocation loop density, size and distribution, loop nature (interstitial/vacancies) and Burgers vector, as well as the formation of voids in both ThO2 and UO2. This work will also discuss the interaction between defects during annealing. The in-situ TEM annealing cycle is shown in Fig 1b. This research significantly improves the understanding of defect behavior in oxide nuclear fuels with temperature and will aid computational modeling efforts. This work was supported as part of the Center for Thermal Energy Transport under Irradiation (TETI) Energy Frontier Research Center, funded by the U.S. Department of Energy Office of Science.

36 MATERIALS SCIENCE↗
NASA NTRS1993

Temperature dependence of protein solubility-determination, application to crystallization, and growth kinetics studies

A scintillation method was developed for determinations of the temperature dependence of the solubility, and of nucleation induction times of proteins, in 50-100 mu(l) volumes of solution. Solubility data for lysozyme and horse serum albumin were obtained for various combinations of pH and precipitant concentrations. These data and the nucleation induction information were used for dynamic crystallization control, that is, for the controlled separation of nucleation and growth stages. Individual lysozyme and horse serum albumin crystals were grown in 15-20 mu(l) solution volumes contained in x-ray capillaries. The morphology and kinetics of the growth and dissolution of lysozyme in aqueous solutions with 2.5 percent NaCl and at pH = 4.5 was studied in situ with a depth resolution of 300 A (4 unit cells) by high resolution optical microscopy and digital image processing. The bulk super- or under saturation, sigma, of the solution inside a closed growth cell was controlled by temperature. The growth habit was bound by (110) and (101) faces that grew through layer spreading, although with different growth rate dependencies on supersaturation/temperature. At sigma less than 10 (obtained at higher temperatures) growth was purely kinetic ally controlled, with impurity effects (macrostep formation and kinetic hindrance) becoming significant for sigma less than 2. At sigma greater than 10 (lower temperatures), anisotropies in the interfacial kinetics were more pronounced, with interfacial kinetics and bulk transport becoming equally important to the growth morphology. Growth rates were growth history dependent. The formation of striations (layers of irregularly incorporated solution) was unambiguously correlated with growth temperature variations. Etching exposed dislocations and various high-index faces whose growth morphologies were studied during return to the steady state growth form. Growth steps were observed to originate from two-dimensional nuclei or from outcrops of growth striations, and from dislocations that preferentially formed in growth sector boundaries.

Rosenberger, Franz↗
DOE OSTI2022

Data-driven electron-diffraction approach reveals local short-range ordering in CrCoNi with ordering effects

Abstract The exceptional mechanical strength of medium/high-entropy alloys has been attributed to hardening in random solid solutions. Here, we evidence non-random chemical mixing in a CrCoNi alloy, resulting from short-range ordering. A data-mining approach of electron nanodiffraction enabled the study, which is assisted by neutron scattering, atom probe tomography, and diffraction simulation using first-principles theory models. Two samples, one homogenized and one heat-treated, are observed. In both samples, results reveal two types of short-range-order inside nanoclusters that minimize the Cr–Cr nearest neighbors (L1 2 ) or segregate Cr on alternating close-packed planes (L1 1 ). The L1 1 is predominant in the homogenized sample, while the L1 2 formation is promoted by heat-treatment, with the latter being accompanied by a dramatic change in dislocation-slip behavior. These findings uncover short-range order and the resulted chemical heterogeneities behind the mechanical strength in CrCoNi, providing general opportunities for atomistic-structure study in concentrated alloys for the design of strong and ductile materials.

36 MATERIALS SCIENCE↗
DOE OSTI2022

In-situ irradiation-induced studies of grain growth kinetics of nanocrystalline UO 2

The thermal conductivity of UO 2 fuel needs to be high enough to dissipate the heat generated from the fission reaction. Since grain size affects thermal conductivity and grain size can evolve with irradiation, it is critical to understand in-reactor UO 2 grain growth. Most studies of grain growth in UO 2 are based on thermally driven processes at elevated temperatures. However, studies have shown that grain growth can occur even at cryogenic temperatures by ballistic processes. Such irradiation-induced grain growth in UO 2 is yet to be studied. Advanced in-situ Kr ion irradiation and transmission electron microscopy were systematically performed on nanocrystalline UO 2 thin films at temperatures ranging from 50 K to 1073 K; grain growth was observed at all temperatures. A combination of manual and machine learning techniques was used to measure and plot grain size evolution against irradiation fluence at various irradiation temperatures. The machine learning method has significantly improved the analysis efficiency and reduced human labors. The grain diameter data were fitted using classical grain growth and thermal spike models to describe grain growth kinetics with and without irradiation effect. Grain growth during low temperature irradiation (≤ 475 K) can be well described by the thermal spike model. Above 475 K, there were additional thermally assisted processes that further accelerate the grain growth. At the highest irradiation temperature about 1075 K, both irradiation-induced dislocation loops and cavities/bubbles were observed to form in the UO 2 . In this report, the effects of irradiation-induced defects on grain growth kinetics are discussed.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Parameter development and characterization of laser powder directed energy deposition of Nb – Alloy C103 for thin wall geometries

This work focuses on the parameter development and microstructural characterization of Nb-based alloy C103 for thin wall structures produced via laser powder – directed energy deposition (LP – DED). Laser power and scanning speeds were varied as part of a design of experiments to identify adequate print parameters. Combinations were evaluated for relative density, porosity, and geometrical accuracy. A combination of a laser power of 1420 W and scanning speed of 14 mm/s resulted in a relative density >99%, exhibited a consistent weld bead profile and was used for further microstructural evaluation. A mix of optical and scanning electron microscopy (SEM) revealed small, slightly elongated grains along the edges and large epitaxial grains in the central region along the Build – Transverse view. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) analysis revealed Hf rich columnar cells in the center that transition into an evenly spaced cellular structure towards the edges of the built sample. Electron backscatter diffraction (EBSD) scans show a sharp [001] texture when looking at the cross section of the sample along the build direction. The Build – Scan view revealed a zig – zag pattern that follows the back – and – forth deposition strategy that was used. Finally, microhardness measurements were taken in the as – built (AB) and stress relieved (SR) conditions to baseline preliminary mechanical properties. The AB condition exhibited a large amount of scatter in the data and averages up to 11% larger than the SR condition. The reduction in scatter upon applying the SR cycle are indicative of a large concertation of dislocations present in the AB condition.

36 MATERIALS SCIENCE↗
NASA NTRS1972

Microscopic observations of X-ray and gamma-ray induced decomposition of ammonium perchlorate crystals

The X-ray and gamma-ray induced decomposition of ammonium perchlorate was studied by optical, transmission, and scanning electron microscopy. This material is a commonly used oxidizer in solid propellents which could be employed in deep-space probes, and where they will be subjected to a variety of radiations for as long as ten years. In some respects the radiation-induced damage closely resembles the effects produced by thermal decomposition, but in other respects the results differ markedly. Similar radiation and thermal effects include the following: (1) irregular or ill-defined circular etch pits are formed in both cases; (2) approximately the same size pits are produced; (3) the pit density is similar; (4) the c face is considerably more reactive than the m face; and (5) most importantly, many of the etch pits are aligned in crystallographic directions which are the same for thermal or radiolytic decomposition. Thus, dislocations play an important role in the radiolytic decomposition process.

Herley, P. J.↗
DOE OSTI2020

Electron Nanocrystallography of Complex Materials and Processes

The proposed work is to develop Scanning CBED (SCBED) for the study of multi element crystals, including multiple principal elements alloys or high entropy alloys and relaxor-ferroelectric crystals. SCBED works like scanning transmission electron microscopy (STEM) but records the whole CBED at each probe position. Since CBED is a highly sensitive electron diffraction technique, SCBED combines the full benefits of CBED and STEM. Specifically, the SCBED based approach enables a quantitative determination of local atomic and electronic structures. The proposed work is thus to take advantage of SCBED for the study of complex multi-element crystals. The results from SCBED are expected to complement the methods of electron energy loss spectroscopy (EELS) near edge fine structure for probing local bonds, and X-ray and neutron scattering using the total scattering approach for probing local structure. Under the DOE BES support, we have developed SCBED to determine the structure of high entropy alloys, and we have coupled the work with in-situ compression study of dislocation dynamics to uncover the fundamental mechanisms of crystal slip.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Comparing structure-property evolution for PM-HIP and forged alloy 625 irradiated with neutrons to 1 dpa

The nuclear power industry has growing interest in qualifying powder metallurgy with hot isostatic pressing (PM-HIP) to replace traditional alloy fabrication methods for reactor structural components. But there is little known about the response of PM-HIP alloys to reactor conditions. This study directly compares the response of PM-HIP to forged Ni-base Alloy 625 under neutron irradiation doses ~0.5–1 displacements per atom (dpa) at temperatures ranging ~321–385 °C. Post-irradiation examination involves microstructure characterization, ASTM E8 uniaxial tensile testing, and fractography. Up through 1 dpa, PM-HIP Alloy 625 appears more resistant to irradiation-induced cavity nucleation than its forged counterpart, and consequently experiences significantly less hardening. This observed difference in performance can be explained by the higher initial dislocation density of the forged material, which represents an interstitial-biased sink that leaves a vacancy supersaturation to nucleate cavities. These findings show promise for qualification of PM-HIP Alloy 625 for nuclear applications, although higher dose studies are needed to assess the steady-state irradiated microstructure.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2024

Fracture behavior of irradiation induced nanocrystalline UO 2 studied by in-situ mechanical testing in transmission electron microscopy

Uranium Dioxide (UO 2 ) is widely used as a fuel in current light water reactors (LWRs). Upon accumulation of radiation damage, LWR UO 2 fuel pellets start to develop a different microstructure at the pellet periphery when fuel burnup exceeds 45–50 GWd/tHM. The resulting porous, nanocrystalline microstructure is one of the most prominent microstructural changes occurring in such fuel. Its fracture mechanisms, which causes fuel fine fragmentation, could impact safety limits when the cladding breaches. Direct measurements of these properties are challenging, therefore a surrogate obtained via ion irradiation can be used. In this study, multiple microcantilevers were fabricated by focused ion beam from both fresh UO 2 and UO 2 irradiated with 84 MeV Xe 26+ ions to a peak dose of 1357 displacements per atom (dpa). Further, the irradiation produced a pseudo high burnup structure approximately 2 µm below the surface. In-situ nano-mechanical bending tests were conducted to investigate the fracture behavior and the effect of the surrogate UO 2 high burnup structure on local fracture properties. Fresh UO 2 fuel was observed to fracture in transgranular mode without nucleation or movement of dislocations. However, the Xe-irradiated nanocrystalline microcantilevers fractured along the grain boundaries, with no influence from the pre-existing micro-cracks in the microcantilever. Fracture toughness for this type of surrogate high burnup UO 2 structure is reported for the first time in literature. Both the fracture stress and toughness show degradation for UO 2 as a result of Xe-irradiation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

Strengthening model development and effects of low diffusing solutes to coarsening resistance in aluminum alloys

A modified Orowan strengthening model is proposed to account for finite rod-shaped precipitates with hemispherical caps in aluminum alloy systems. A combined computational and experimental approach is used to study the influences of anisotropic Orowan looping and solute-dislocation interaction on temperature-dependent yield strength. Here, the strengthening model is validated with a dataset containing 297 experimental precipitate geometries, chemistries, temperatures, and strength measurements, and achieves a strong predictive correlation of 0.8713 with experimentally measured yield strengths. Under conditions that are applicable to coarsening, constant particle volume fraction and aspect ratio, the model predicts that short rod precipitates provide far superior strengthening effects compared to plate precipitates. A cast Al-Si-Mg-Cu alloy with rod-shaped Q-phase (Al 3 Cu 2 Mg 9 Si 7 ) precipitates was developed with a novel chemistry exploring the use of low-diffusivity elements (Mn, Ni, V, Zr) to limit precipitate coarsening. The thermodynamic behavior of Mn, Ni, V, and Zr across the Q-phase interface is examined using transmission electron microscopy (TEM), first-principles density-functional theory (DFT) calculations. and atom-probe tomography (APT). DFT calculations utilizing TEM identified Q-phase/Al-matrix interfaces show that Mn, Ni, V, and Zr preferentially segregate to the Q-phase precipitate boundaries which suggests inhibition of precipitate coarsening and higher strengths after temperature exposure. Atom-probe tomography confirms solute atom partitioning/segregation at the Q-phase/Al-matrix interface, found in the modified commercial AS7GU alloy (A356 +0.5%Cu), which supports these observations.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Origins of radiation-induced optical attenuation in neutron-irradiated single-crystal sapphire at elevated temperatures

Sapphire (α-Al 2 O 3 ) is a candidate fiber-optic sensor material for extreme temperature environments, potentially including those of nuclear reactors. However, its optical transmission under high-dose neutron irradiation is not well understood compared with that of conventional fused silica. This study examined dimensional changes, optical transmission, and irradiation-induced defects in neutron-irradiated α-Al 2 O 3 at temperatures of 298 °C to 688 °C and doses of 3.2 to 12 dpa. Although previous studies attributed radiation-induced attenuation (RIA) at the highest irradiation temperatures to increased optical scattering from radiation-induced voids, our findings indicate that scattering from neither voids nor dislocation loops can explain the measured attenuation. Instead, absorption due to aluminum vacancy centers appears more likely based on a comparison of the spectral features of the measured optical attenuation with previous literature. Significant c-axis swelling (5.51 % ± 0.83 %) was observed in the 12 dpa, 592 °C irradiated sample, much higher than earlier measurements, suggesting temperature sensor drift of 543 °C to 1,140 °C. Void patterning was predominantly observed along the a-axis, differing from previous studies on polycrystalline samples, which showed c-axis patterning. Dislocation loops evolved into network dislocations with increasing temperature and dose; voids formed within these structures, showing no size or density changes, indicating an atypical growth mechanism.

Neutron irradiation↗
DOE OSTI2022

The influence of pearlite fraction on the shock properties of ferrite–pearlite steel microstructures: Insight into the effect of second-phase particles

Here, the goal of this work is to investigate the effect of varying phase fractions on the overall spall strength and damage behavior of a material. Specifically, two plain carbon, ferrite–pearlite steels (1045 and A283) were subjected to spall recovery experiments to investigate the effect of pearlite fraction on spall strength and total damage. The A283 (20% pearlite) alloy exhibited a higher Hugoniot elastic limit and spall strength compared with 1045 (60% pearlite). Discontinuous and continuous yielding behaviors were observed at quasi-static and dynamic rates for A283 and 1045, respectively. The yielding behavior was connected to pearlite fraction and the prevalence of dislocation-emitting, ferrite/cementite interfaces. Postmortem characterization revealed cementite lamellae cracking within pearlite of 1045, suggesting that pearlite reduces spall strength by providing low-energy damage nucleation sites. The rate of damage growth and coalescence was similar between the two alloys; however, 1045 exhibited more continuous cracks than A283, which exhibited a greater prevalence of discrete voids.

36 MATERIALS SCIENCE↗
NASA NTRSDate not supplied

Hypervelocity Dust Impact in Olivine: Fib/Tem Characterization and Comparison of Experimental and Natural Microcraters

The flux of objects impacting the surfaces of solar system airless bodies is dominated by micrometeoroids less than 1 mm diameter whose impact effects play a major role in the space weathering of airless body surfaces. To obtain better understanding of how small scale impact effects vary as a function of impact speed in an important lunar and asteroidal mineral, we produced artificial microcraters in San Carlos olivine using Fe metal dust particles 0.10 to 5 µm in diameter electrostatically accelerated to speeds between 0.35 to 25 km s-1. The crater morphologies, size distrrubiton and microstruc-tures were characterized by field-emission SEM (FE-SEM) and also by FIB cross sectioning of selected craters for field-emission scanning transmission electron microscopy (FE-STEM). These same techniques were also applied to study a natural 20 µm-diameter microcrater in a olivine grain on the surface of lunar rock 12075. Measured microcrater diameters in the experimental sample range between 0.20 to 5 µm with larger craters having more irregular outlines dominated by spallation fractures. FE-SEM and FE-STEM imaging docu-ment the formation of shock melt in the size population of experimental craters below approximately 1 µm in diameter, corresponding to particle impact speeds in the 10-25 km s-1 range. The natural olivine crater exhibits similar shock melt features along the perimeter of its cavity, but the shock melt also contains nanophase Fe metal particles, something not observed in the experimental samples. FE-STEM imaging of the experimental craters reveals complex shock-generated dislocation and nanofracture microstructures in zones extend-ing 1-2 µm into the olivine from the crater cavity. The natural microcrater shows a lower density of shock-generated disloca-tions that extends a factor of 2 deeper into the the olivine than in the experimental samples.

Roy Gray Christoffersen↗