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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 127 records · Page 7
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Investigating relationship between surface topography and emissivity of metallic additively manufactured parts

Due to the direct relationship between thermal history and mechanical behavior, in situ thermal monitoring is key in gauging quality of parts produced with additive manufacturing (AM). Accurate monitoring of temperatures in an AM process requires knowledge of environment and object parameters including object emissivity. The emissivity is dependent on several variables, including: wavelength, material composition, temperature, and surface topography. Researchers have been concerned with the thermal emissivity dependence on temperature since large ranges are seen in metal powder bed processes, but there is also an extensive range of surfaces produced by AM. This work focused on discovering what roughness characteristics control thermal emissivity through investigation of prototypic 316 stainless steel AM samples produced with a range of build conditions on a laser powder bed fusion machine. Through experimental measurements of emissivity using hemispherical directional reflectance (HDR), guided by simulations using a finite-difference time-domain (FDTD) Maxwell solver, it was found that combinations of existing roughness parameters describing both height and slope of the surface correlate well with emissivity changes. Furthermore, these parameters work well due to their apt description of surface features encouraging internal reflection, which is the phenomenon that increases emissivity when a surface falls under the geometric optical region conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Understanding the microstructural stability in a y’-strengthened Ni-Fe-Cr-Al-Ti alloy

Ni-Fe-Cr-Al-Ti alloys, with Ni levels near 50 wt.%, have the potential to develop a microstructure consisting of a face-centered cubic ? matrix with the homogeneous precipitation of fine ordered ?’ precipitates similar to traditional Ni-based superalloys with significantly greater Ni content. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), atom probe tomography (APT), and CALPHAD -based thermodynamic modeling were employed to understand the phase stabilities and microstructural evolution in an age-hardenable Ni-27Fe-18Cr-1Co-1.6Al-3.75Ti-1.2Mo-0.03C (wt%) alloy. The primary heat-treatment of solution annealing at 1121°C for 4h and age-hardening treatment at 760 °C for 16h resulted in a microstructure consisting of fine ?’ precipitates in an austenitic matrix along with grain boundary carbides, consistent with thermodynamic calculations. Long-term aging at 900 °C for 250h resulted in the coarsening of ?’ along with a change in the morphology of the precipitates from spherical to a more cuboidal shape. In addition, ? phase formation was observed concomitant with the partial dissolution of the ?’ phase. The ability of computational thermodynamic models to predict microstructural characteristics is discussed.

Gwalani, Bharat↗
DOE OSTI2024

Effect of microalloying additions on microstructural evolution and thermal stability in cast Al-Ni alloys

Enhancement of thermal stability in Al-Ni alloys through microalloying with slow-diffusing elements, specifically Zr, has been previously reported which is attributed to Zr segregation at the Al/Al 3 Ni interface. In this study, we explore the influence of microalloying Al-Ni alloys with Zr, Ti, V, and Fe on microstructural evolution, hardness, and electrical and thermal conductivity across a range of heat-treatment temperatures from 300 to 450 °C. The distribution of microalloying elements and precipitates after heat treatment is characterized using atom probe tomography (APT). Our investigation confirms Zr segregation to the Al/Al 3 Ni interface, while similar interfacial segregation is absent with the addition of Ti, V, and Fe. Additionally, our analysis of the Al 3 Ni microfiber morphology reveals that their coarsening and spheroidization rates are similar with and without interfacial segregation; thus, retaining the fiber reinforcement through interfacial segregation of slow diffusing elements may not be an effective strategy. Precipitation of L1 2 nanoparticles was found to be the dominant mechanism affecting enhanced hardness and electrical conductivity in Al-Ni-Zr alloys, attributed to precipitation strengthening and solute depletion, respectively. Similar precipitation was not observed for additions of Ti, V, and Fe following heat treatment. We provide a thermodynamic explanation for this limitation. Furthermore, the findings of this study suggest that an effective approach for designing Al-Ni alloys should involve prioritizing microalloying elements to maximize L1 2 precipitation and minimize solute content in the FCC-Al matrix post heat treatment, rather than focusing on Al/Al3Ni interfacial segregation.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Microstructural Engineering of Cu-Rich Nanoprecipitate formation in NiCoFeCrCu0.12 High-Entropy Alloy via Severe Plastic Deformation for Enhanced Irradiation Tolerance

This study demonstrates a defect-engineering approach for controlling Cu-rich precipitates in FeNiCrCoCu0.2 high-entropy alloys (Cu-HEAs), delivering a novel pathway for next-generation nuclear reactor materials with superior irradiation resistance. This work establishes that severe plastic deformation (SPD) processing via Shear Assisted Processing and Extrusion (ShAPE) and Friction Stir Layer Deposition (FSLD) creates dense dislocation networks and subgrain boundaries that fundamentally alter precipitation behavior under identical thermal treatments. Atom probe tomography (APT) indicates that SPD produces a metastable, atomically homogeneous solid solution that, upon moderate heat treatment (500°C/10 hour), develops remarkedly stronger Cu clustering than the as-cast counterpart. High-temperature exposure (800°C/100 h) produces near-pure Cu precipitates (~90 at% Cu) with significantly enhanced defect-sink efficacy in SPD-processed alloys: precipitate sizes of 50-60 nm and number densities of 2.7-3.8 × 10¹7 m?³, compared to 89 nm and 0.44 × 10¹7 m?³ in as-cast materials. Collectively, the findings establish defect-mediated precipitation control as a scalable, high-impact route to tailor sink density and distribution in HEAs, enabling microstructures optimized for irradiation tolerance and mechanical robustness in nuclear reactor environments.

Meher, Subhashish↗
DOE OSTI2021

Origins of high ductility exhibited by an extruded magnesium alloy Mg-1.8Zn-0.2Ca: Experiments and crystal plasticity modeling

Low ductility and strength are major bottlenecks against Mg alloys' wide applications. In this work, we systematically design the composition and fabrication process for a low-alloyed Mg-Zn-Ca alloy, showing that it can be extruded at low temperatures (~ 250 degrees C) and high speeds (~2 mm/s). After the extrusion, this alloy exhibits a substantially weakened basal texture, relatively small grain size, very high tensile elongation (~ 30%), and good strength. The origin of the considerably improved ductility was studied using a combination of three-dimensional atom probe tomography (3D-APT), transmission electron microscopy (TEM), electron backscattered diffraction (EBSD) in conjunction with surface slip trace analysis, in-situ synchrotron X-ray diffraction, and elasto-plastic self-consistent (EPSC) modeling. Co-segregation of Zn and Ca atoms at a grain boundary is observed and associated with texture weakening and grain boundary mediated plasticity, both improving the ductility. While basal slip and prismatic slip are identified as the dominant deformation systems in the alloy, the ratio between their slip resistances is substantially reduced relative to pure Mg and most other Mg alloys, significantly contributing to the improved ductility of the alloy. This Mg-Zn-Ca alloy exhibiting excellent mechanical properties and low fabrication cost is a promising candidate for industrial productions.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Revealing the complex chemistry of grain boundaries in K-doped BaFe 2 As 2 with atom probe tomography

Iron-based superconductors have attractive properties for high-field applications, but there is a lack of understanding of the effect of grain boundary chemistry on the in-field performance. The near atomic-scale resolution, ppm sensitivity and 3D analysis offered by atom probe tomography make it a powerful tool to investigate the nanoscale structure and chemistry of these defects in fine-grained K-doped BaFe 2 As 2 samples. A computational method to systematically extract and compare the Gibbsian interfacial excess of chemical species across grain boundaries has been explored in this work. The robustness of the method has been tested by evaluating the effects of selected variables on simulated APT datasets. The accuracy and precision of the calculated Gibbsian interfacial excess were found to be stable over a range of analysis conditions: varying grain boundary widths and detection efficiencies, spatial precisions below 1.5 nm, and bin widths between 1.2 and 1.6 nm. For the K-doped BaFe 2 As 2 samples studied, segregation of As, Ba, K and impurities of O, Na, and Sb were found at grain boundaries. The Gibbsian excess values were found to vary widely between different boundaries, showing the complexity of the grain boundary chemistry in this material. Possible links between the observed critical current density (Jc) of these samples and their nano- and micro-structure have also been investigated and discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2020

On the use of charged particles to characterize precipitation in irradiated reactor pressure vessel steels with a wide range of compositions

Nuclear reactor lifetimes may be limited by nano-scale Cu-Mn-Ni-Si precipitates (CRPs and MNSPs) that form under neutron irradiation (NI) of pressure vessel (RPV) steels, resulting in hardening and ductile to brittle transition temperature increases (embrittlement). Physical models of embrittlement must be based on characterization of precipitation as a function of the combination of metallurgical and irradiation variables. Here we focus on rapid and convenient charged particle irradiations (CPI) to both: a) compare to precipitates formed in NI; and, b) use CPI to efficiently explore precipitation in steels with a very wide range of compositions. Atom probe tomography (APT) comparisons show NI and CPI for similar bulk steel solute contents yield nearly the same precipitate compositions, albeit with some differences in their number density, size and volume fraction (f) dose (dpa) dependence. Yet, the overall precipitate evolutions are very similar. Advanced high Ni (>3 wt%) RPV steels, with superior unirradiated properties, were also investigated at high CPI dpa. For typical Mn contents, MNSPs have Ni 16 Mn 6 Si 7 or Ni 3 Mn 2 Si phase type compositions, with f values that are close to the equilibrium phase separated values. In contrast, in steels with very low Mn and high Ni, Ni 2-3 Si silicide phase type precipitate compositions are observed; and when Ni is low, the precipitate compositions are close to the MnSi phase field. Low Mn significantly reduces, but does not eliminate, precipitation in high Ni steels. A comparison of dispersed barrier model predictions with measured hardening data suggests that the Ni-Si dominated precipitates are weaker dislocation obstacles than the G phase type MNSPs.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2021

Atom Probe Tomography Characterization of High-Dose Ion Irradiated MA957

This paper presents a comprehensive characterization study of the microstructural responses to ion irradiation of the oxide dispersion strengthened (ODS) ferritic alloy MA957 using atom probe tomography (APT). The MA957 specimens were irradiated by 1.8 MeV Cr3+ ions to doses and temperatures relevant to advanced fast reactors (100 and 500 dpa at 400-500 °C). The average sizes of the YTiO particles decreased slightly after irradiation at all temperatures, with the most pronounced change at 400 °C. The particle number densities for 400 and 500 °C were slightly below number densities for the unirradiated condition, while the values were slightly higher at 420 and 450 °C. This behavior is consistent with the Nelson-Hudson-Mazey rate theory model that considers the competing effects between recombination and dissolution. An increase in the Y/Ti ratio of the YTiO particles was observed at the two lower temperatures. The formation of Cr-rich precipitates (a') was observed in specimens irradiated at temperatures up to 450 °C. Irradiation-induced segregation on grain boundaries was also investigated. Grain boundary element concentration profiles and ion maps demonstrate differences among the irradiation temperatures, with most datasets differing from the unirradiated condition. A key focus of this ion irradiation study is the high-dose response, and this quantitative assessment revealed relatively small but distinct effects of irradiation on microstructure evolution. Overall, these results showing minor second phase evolution suggest that MA957 should retain mechanical performance generally well up to 500 dpa for the irradiation temperatures studied.

Wang, Jing↗
DOE OSTI2021

Evolution of {delta}ferrite in a CF3 cast stainless steel upon neutron irradiation to 3, 5, 10, 20, and 40 dpa

The microstructural evolution of delta ferrite in a CF3 cast stainless steel irradiated to 3, 5, 10, 20, and 40 dpa with two dose rates was studied with atom probe tomography (APT) and transmission electron mi-croscopy. Spinodal decomposition and G-phase precipitates induced by neutron irradiation and thermal aging were quantified systematically. The neutron irradiation significantly enhances the spinodal decom-position in delta ferrite as both the spinodal wavelength (i.e. a characteristic repeat distance) and am-plitude (i.e. magnitude of elemental concentration fluctuation) increase after irradiation. The wavelength only varies slightly when the dose increases from 5 to 40 dpa, while the amplitude increases dramatically from 10 to 20 dpa and starts to saturate before 20 dpa. The dose rate and irradiation temperature also have a notable effect on the spinodal wavelength and amplitude. The study shows that higher dose rate promotes a larger wavelength at given irradiation doses. Regarding the G-phase precipitates, a slightly lower irradiation temperature would result in a smaller mean size of G-phase precipitates, while a lower irradiation dose rate would lead to a larger G-phase precipitates at a given temperature and dose. Over-all, the spinodal decomposition and G-phase precipitates in the delta ferrite continue to evolve with the increasing dose beyond 10 dpa. This study confirms that the formation of G-phase precipitates at the in-terdomain region between alpha and alpha-prime is facilitated by the Si and Mo atoms rejected from Fe rich alpha phase and the Ni and Mn atoms rejected from Cr rich alpha-prime phase. Neutron irradiation plays a dominant role in the ferrite instability, and the effect of prior thermal aging at 400 degrees C for 10,000 hours is negligible as the dose is 3 dpa and above.

duplex stainless steel↗
DOE OSTI2022

Friction stir welding and self-ion irradiation effects on microstructure and mechanical properties changes within oxide dispersion strengthened steel $\mathrm{MA956}$

We report the joining process for oxide dispersion strengthened (ODS) alloys remains a key challenge facing the nuclear community. The microstructure and mechanical properties were characterized in the base material and friction stir welded ODS MA956 irradiated with 5 MeV Fe 2+ ions from 400 to 500°C up to 25 dpa. Nanoindentation was performed to assess changes in hardness and yield stress, and the dispersed barrier hardening (DBH) model was applied to described results. A combination of scanning transmission electron microscopy (STEM) and atom probe tomography (APT) were used to assess evolution of the microstructure including dispersoids, network dislocations and dislocation loops, nanoclusters, and solid solution concentrations. Overall, softening was observed as a result of increased dose, which was exacerbated at 500°C. The formation and coarsening of new dispersoids was noted while nanoclusters tended to dissolve in the base material, and were not observed in the stir zone. Solute nanocluster evolution was identified as a primary driver of the changes in mechanical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Nanoscale clustering and fission product segregation in irradiated annular U-10Zr fuel

Zirconium (Zr) is added to uranium (U) to improve the performance of metallic fuel for fast reactor applications. This study employs transmission electron microscopy (TEM) and atom probe tomography (APT) to investigate nanoscale clustering of U and Zr, as well as segregation of fission products (FPs), in annular U-10Zr (in weight) metallic fuel irradiated at the Advanced Test Reactor (ATR). The results reveal variations in the shape, size, and chemical composition of clusters at different radial locations within the irradiated fuel cross-section. Zr-rich clusters exhibit higher concentration of FPs compared to U-rich clusters, potentially due to the co-precipitation of Zr and FPs in the fuel matrix during cooling at the end-of-life. In conclusion, this work complements the study of fuel constituents and fission product distribution across multiple length scales in irradiated U-10Zr metallic fuel.

Atom probe tomography↗
DOE OSTI2024

Atom probe tomography of segregation at grain boundaries and gas bubbles in neutron irradiated U-10 wt% Mo fuel

During neutron irradiation to fission densities > 5.2 × 10 21 fiss/cm 3 , Xe agglomerates forming gas bubbles of varying size within the U-Mo fuel matrix. Herein, segregation of fission products to Xe bubbles and grain boundaries (GB) were studied using atom probe tomography (APT). Segregation behavior was found to vary among GBs, small bubbles (<10 nm), and larger bubbles (>10 nm). Solid fission products were enriched at GBs and larger bubbles, but not at small bubbles. Finally, a denuded zone was identified adjacent to a > 10 nm Xe gas bubble and a GB.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Precipitation hardening of laser powder bed fusion Ti-6Al-4V

Here, the laser powder bed fusion (PBF-L) additive manufacturing (AM) community has dedicated significant efforts into process optimization and control for defect-free Ti-6Al-4V. As defects become less of an issue for PBF-L Ti-6Al-4V, the processing-structure-properties (PSP) relationships between AM microstructures can now be explored to optimize mechanical properties. Lower temperature aging treatments around 550 °C in wrought Ti-6A-4V have been historically understood to precipitation harden the α phase with an ordered, hexagonal close packed (HCP) α 2 phase. The α 2 phase existed as nanoscale Ti 3 Al precipitates coherent with the parent α phase. The goal of the present investigation was to implement a vacuum heat treatment of 545 °C for 100 hours on PBF-L Ti-6Al-4V. This vacuum heat treatment took place after an initial hot isostatic pressure (HIP) treatment that decomposed the as-built, martensitic microstructure. The vacuum aging successfully produced nanoscale precipitates of α 2 phase within α-laths, confirmed via atom probe tomography (APT). Microstructural-length scale and quasi-static mechanical properties were investigated by nanoindentation and uniaxial tensile tests of miniaturized test specimens. Given the sensitivity of Ti-6Al-4V mechanical properties to small changes in chemistry, all test specimens originated from the same build. The α 2 precipitation resulted in significantly harder α-laths (≈ 2 GPa) as measured via nanoindentation, as well as a relative yield and ultimate tensile strength increase of 60 MPa and 38 MPa, respectively. Analysis of Variance (ANOVA) of the datasets revealed no statistical differences in total elongation between the HIPed and HIPed + aged specimens, indicative of the aging treatment producing a net benefit of strength with no loss in ductility.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Microstructure and mechanical behavior of a TiC nanoprecipitate strengthened V Alloy

The V-4Cr-4Ti (V44) alloys have been proposed as the prime candidate structural material for self-cooled liquid Li blanket and other designs for fusion energy applications. However, the applications of the V44 alloy are limited to a narrow operation temperature window, due to reduction in creep strength at or above 700 °C and susceptibility to irradiation hardening and embrittlement when irradiated below 400 °C. Here, in this work, we explore the feasibility of designing a novel V alloy to form a high number density of TiC nanoprecipitates, in order to simultaneously improve creep strength and provide defect sinks to mitigate irradiation hardening. Computational thermodynamics was used to design a new alloy (V44C) to achieve our goal of high TiC nanoprecipitates density within the alloy V44 matrix. To ensure scalability, the new alloy was made through arc-melting and ingot-casting followed by hot forging, cold rolling and heat treatments of homogenization and precipitation aging. The microstructure was characterized by SEM, TEM, XRD and APT, confirming the existence of nanoprecipitates predicted in the thermodynamic calculations. In addition to microstructural evaluation tensile properties at room temperature and 700 °C, and Charpy impact energy at room temperature were measured. The microstructure and mechanical properties were then compared with those from a historic reference V44 alloy. The tensile strength improvement in V44C was rationalized based on particle and solid solution strengthening mechanism. The fracture behavior was discussed based on the fractography results and necking deformation behavior.

Alloys development↗
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 OSTI2020

Partitioning of tramp elements Cu and Si in a Ni-based superalloy and their effect on creep properties

An alloy's processing history, including melting, remelting or the choice of stock material, affects its purity and eventually involves tramp element pickup or retention. Herein, variants of a novel Ni-based superalloy were manufactured with different levels of purity. The so-called low purity alloys contained 0.138 wt. % Cu and 0.019 wt. % Si while the Cu and Si levels were below x-ray fluorescence (XRF) detection limits of 0.003 and 0.010 wt. %, respectively, in the high purity ingots. Atom-probe tomography (APT) was carried out and revealed Si partitioning at the following interfaces: grain boundaries, MC carbide/γ, M 3 B 2 boride/$γ$ and M 3 B 2 boride/$γ$'. Copper was found to primarily segregate to the $γ$' precipitates. An average of 2.4 × decrease in creep life and 4.3 × decrease in creep ductility was measured in the low purity alloys, which was attributed to the embrittlement caused by Si segregation to grain boundaries. Furthermore, the positive effect of B on the creep properties was mitigated by the presence of Si. Thermodynamic predictions for the matrix and γ' precipitate compositions represented the trends observed experimentally although the extent of preferential partitioning lacks accuracy. Monte Carlo simulations were performed to describe the partitioning of Cu and Si atoms to either $γ$ or $γ$' phases.

36 MATERIALS SCIENCE↗