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At least 1,207 records · Page 67
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Binder-jetted AISI M2 tool steel during hot isostatic pressing: Densification and carbide transformation

Binder jetting (BJ) enables fabrication of complex components from high-alloy steels such as AISI M2; however, residual porosity after sintering limits mechanical performance. This study investigates the coupled effects of binder chemistry, sintering conditions, cooling rate, and subsequent hot isostatic pressing (HIP) on densification, microstructure, and mechanical response in binder-jetted M2 tool steel. HIP increased relative density from ∼93 to 95% to >99% and improved compressive strength by ∼40-70%. Densification was governed by initial pore morphology, where closed porosity was effectively eliminated, while interconnected porosity limited full consolidation. Microstructural analysis (XRD, EBSD, SEM) shows that HIP promotes dissolution of metastable carbides and redistribution of alloying elements (W, Mo, V), transforming heterogeneous carbide networks into finer and more uniformly distributed M 2 C, MC, and M 6 C phases through diffusion-assisted homogenization. Among the investigated conditions, the FluidFuse binder combined with sintering at 1270 °C for 60 min and furnace cooling produced the most balanced response, achieving ∼99.7% density, ∼855 HV hardness, ∼4130 MPa compressive strength, and ∼24% strain. In contrast, higher sintering temperatures promoted carbide coarsening, reducing ductility despite high density. HIP reduces microstructural heterogeneity and drives the system toward a near-equilibrium state with reduced sensitivity to prior processing history. A comparative assessment with conventional and additive manufacturing routes (LPBF, DED, EBM, FFF) shows that the BJ-HIP approach achieves competitive densification and mechanical performance. These findings provide a mechanistic basis for controlling densification and microstructure in high-alloy steels processed via BJAM.

AISI M2 tool steel↗
DOE OSTI2022

Phase stability, mechanical properties, and ion irradiation effects in face-centered cubic CrFeMnNi compositionally complex solid-solution alloys at high temperatures

We report two CrFeMnNi face-centered cubic complex concentrated solid-solution alloys (CSA) have been evaluated for phase stability, mechanical properties, and radiation damage effects from heavy ions. Cr 18 Fe 27 Mn 27 Ni 28 and Cr 15 Fe 35 Mn 15 Ni 35 were predicted by thermodynamic calculations to phase separate and maintain a single phase at 700 °C, respectively. Aging experiments at this temperature confirmed varying degrees of precipitation of a body-centered cubic phase in both Cr 18 Fe 27 Mn 27 Ni 28 and Cr 15 Fe 35 Mn 15 Ni 35 . The alloys showed promising strength in tensile deformation at room temperature, with yield strengths of 155 MPa and 151 MPa for Cr 18 Fe 27 Mn 27 Ni 28 and Cr 15 Fe3 5 Mn 15 Ni 35 , respectively. At 500 °C, the yield strength of Cr 18 Fe 27 Mn 27 Ni 28 fell to 93 MPa, and to 100 MPa in Cr 15 Fe3 5 Mn 15 Ni 35 . Unlike Cr 18 Fe 27 Mn 27 Ni 28 , Cr 15 Fe 35 Mn 15 Ni 35 gained some ductility at 500 °C compared to room temperature. The two CSAs were irradiated to 75 dpa at 500 °C in the plateau region of the displacement curve using 3.7 MeV Ni 2+ ions, alongside model alloy 709 as a reference. Irradiation results produced similar densities and sizes of dislocations loops in the two CSAs compared to the reference. However, while large voids form in the plateau region of Cr 18 Fe 27 Mn 27 Ni 28 , small voids form just beyond the displacement peak of Cr 15 Fe 35 Mn 15 Ni 35 . Atom probe tomography and energy dispersive X-ray spectroscopy-equipped scanning transmission electron microscopes were used to characterize the alloys for changes in chemical distribution.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Cold spray manufacturing of oxide-dispersion strengthened (ODS) steels using gas-atomized and ball-milled 14YWT powders

The cold spray deposition process has been investigated for the manufacture of 14YWT oxide-dispersion strengthened (ODS) steel, a nanostructured ferritic alloy (NFA), using gas-atomized and ball-milled feedstock powders. Cold spraying of the gas-atomized powder resulted in a thick dense deposit, but annealing them above 900 °C induced grain growth and heterogeneous precipitation of nanoparticles, thus resulting in lower hardness (~ 170 HV) compared to 14YWT ODS steel manufactured by the conventional method. The ball-milled powder (Fe-14Cr-3W-0.4Ti-0.2Y-0.125O) was cryomilled in liquid N 2 to achieve small particle sizes followed by annealing in a H 2 /Ar environment at 1000 °C and 1100 °C to reduce the hardness from ~ 8 GPa to ~ 5 GPa. Both smaller particle sizes and lower hardness of annealed powders made them amenable to the cold spray deposition process, resulting in thick and dense deposits, while retaining the favorable fully solutionized microstructure of the ball-milled powders. The microstructure of the as-deposited ODS exhibited very fine grain sizes (50–250 nm) with a uniform dispersion of Y-Ti-O nanoprecipitates in the ferritic steel matrix. The hardness values of the cold spray deposits using the powders annealed at 1000 °C and 1100 °C was 770 HV and 496 HV, respectively. Post-heat treatment of the as-deposited material up to 1100 °C showed a high-density microstructure with uniformly dispersed nanoscale oxide particles. The hardness of the annealed deposits up to 1000 °C had a notably higher hardness than bulk 14YWT ODS steel manufactured by conventional methods. The study demonstrates that cold spray deposition of the microstructurally-tailored feedstock powders can be used to successfully manufacture ODS steel with microstructure and properties comparable to those produced by the conventional methods, while providing for an attractive option for the more rapid and cost-effective manufacturing of ODS steel cladding tubes.

14YWT↗
DOE OSTI2018

Characterization of the microstructures and the shape memory properties of the Fe-Mn-Si-Cr-Ni-C shape memory alloy after severe plastic deformation by differential speed rolling and subsequent annealing

Highlights: • The Fe-SMA was subjected to severe plastic deformation and then annealed. • Recovery strain increased with increasing grain size. • An optimum grain size existed for the largest recovery stress. • Grain reduction is useful for having a high recovery stress. - Abstract: The Fe-13.51Mn-4.82Si-8.32Cr-3.49Ni-0.15C shape memory alloy was subjected to severe plastic deformation by high-ratio differential speed rolling and subsequent annealing (between 873 and 1373 K) to find the factors that affect recovery stress and recovery strain. As the annealing temperature increased (i. e., as grain size increased), the recovery strain increased. This was attributed to decrease in the density of grain boundaries and the density of twins with increasing grain size. The recovery stress, however, showed a different behavior. It increased with annealing temperature up to 973 K, at which an ultrafine grain size near 1.6 μm was obtained, and then decreased with further increase in the temperature. The difference between the recovery strain and the plastic strain induced by recovery stress under constrained displacement during cooling was proposed to determine the amount of recovery stress. There was an optimum grain size for the largest difference between the recovery strain and the plastic strain. The current study shows that grain-size reduction is not good for having a high recovery strain but it is beneficial for having a high recovery stress in the Fe-Mn-Si shape memory alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Electron backscatter diffraction helps direct calculation of magnetocrystalline anisotropy energy in API 5L steels

Highlights: • Experimental evidence of the capability of EBSD to accurately estimate MAE of API 5L steels. • MAE can be calculated directly from raw EBSD data for reduced sample sizes. • Number of grains sufficient to estimate MAE from EBSD is in the order of several hundreds. • The use of equivalent orientations increases drastically the accuracy of MAE estimations. • EBSD helps explain origin of the observed correlation between MAE and Barkhausen noise. - Abstract: This paper shows evidence of the capability of electron backscatter diffraction (EBSD) to accurately estimate the magnetocrystalline anisotropy energy (MAE) of API 5L steels. The crystallographic texture of five circular steel samples was characterized by X-ray global texture and EBSD microtexture measurements. The average MAE of each one of these samples was estimated from the set of individual grain orientations obtained from orientation maps measured by EBSD. The angular dependence of EBSD-derived MAE was compared with predictions made from X-ray texture and Barkhausen noise (BHN) measurements. The average MAE determined from the EBSD data is in good agreement with the predictions made from X-ray and BHN measurements for all the studied samples. This agreement can be explained by the fact that the number of grains used to predict the average MAE from the EBSD results was statistically sufficient to reproduce the MAE predicted by the other two methods. The EBSD measurement strategy for the accurate MAE estimation was established in terms of parameters such as the number of individual grain orientations to be measured, the sample's texture acuity and grain size, the use of equivalent orientations given by the statistical orthorhombic symmetry of the studied samples, and different measurement planes.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Elements distribution and deformation features of a 4.5% Re nickel-based single crystal superalloy during creep at high temperature

Highlights: • Atom probe is used to investigate the element concentration changes in γ and γ' phase during creep. • Mo, W and Re diffuse from γ' to γ phase and enrich in γ/γ' interface during high temperature creep. • Super-dislocations in γ' phase may cross-slip from {111} to {100} plane due to the elements diffusions. • Dislocations shearing into γ' phase may decompose into K-W locks plus APB due to the refractory elements enrichment. - Abstract: By means of creep property measurement, microstructure observation and atom probe tomography, the elements distribution and deformation features of a 4.5% Re nickel-based single crystal superalloy during creep are investigated. Results show that after fully heat treated, the elements Al and Ta are mainly distributed in γ′ phase of alloy. After the alloy is crept up to fracture at 1100 °C/137 MPa, the change of the elements distributing in γ and γ′ phases occurs, wherein, the concentration decrement of the elements Al and Cr in γ′ and γ phases is attributed to their oxidation which may consume the ones. Moreover, some of the atoms Re, W and Mo dissolving in γ′ phase are repelled into γ matrix to reduce its internal energy. And the peak concentration of the atoms Re and W appears in the γ phase near the transition region, the atoms Re, W in the peak region cause the lattice distortion to increase the resistance of dislocations motion, which may improve the creep resistance of alloy. In the later stage of creep, dislocations shearing into the rafted γ′ phase may cross-slip from {111} to {100} plane to form the configuration of K-W locks, which may restrain the slipping of dislocations to improve the creep resistance of alloy. Wherein, the atom Re with lower diffusion coefficient may delay the dislocations in K-W locks for slipping and cross-slipping, which is thought to be the main reason of the K-W locks keeping in 4.5%Re alloy during creep at 1100 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Analysis of position-dependent cavity parameters in irradiated metals to obtain insight on fundamental defect migration phenomena

Motion of point defects is a fundamental process that governs microstructure and properties of materials. Here, we examine the near-surface and grain boundary cavity swelling depth profiles in neutron- and ion-irradiated simple metals (Cu, Ni, and Fe-Cr) and investigate diffusional broadening of implanted Ni ions in Fe-Cr alloys. Vacancy migration energies and radiation-enhanced diffusion were experimentally estimated. Cavity denuded zone widths near planar sinks are shown to be dependent on temperature, damage rate, balance of point defects and sinks, and vacancy migration energies. An enhanced cavity swelling zone adjacent to the void-denuded zone was observed in specimens with low to moderate sink strength and interpreted as evidence of 1D gliding interstitial clusters. Radiation-enhanced diffusional broadening of implanted Ni ions (at 400–550 °C) in Fe and Fe-Cr was up to 250 nm toward the surface, which leads to a much broader near-peak-damage region where cavity swelling is suppressed. Diffusional broadening of implanted ions is calculated to be similarly pronounced for self-ion irradiations, particularly near the peak and higher swelling temperature regimes. Adequately high ion energies (~8–15 MeV) are recommended for ion-irradiation studies to provide a sufficiently broad midrange safe analysis region with minimized surface and injected ion effects.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Structural, magnetic and impedance spectroscopy analysis of (0.7)CoFe2O4+(0.3)BaTiO3 magnetoelectric composite

Highlights: • Successfully synthesized (0.7)CoFe{sub 2}O{sub 4}+(0.3)BaTiO{sub 3} composite by ball-milling method. • Structural properties confirmed the presence of both constituent phases. • Dielectric properties showed high value of permittivity and diminished dielectric loss at higher frequency. • Electric response of the constituent phases explained the observed relaxation processes. • Small polaron hopping mechanism governed the conduction mechanism. - Abstract: Magnetoelectric composite of particular composition (0.7)CoFe{sub 2}O{sub 4}+(0.3)BaTiO{sub 3} was synthesized by ball-milling method. X-ray diffraction pattern confirmed the presence of cubic spinel phase for CoFe{sub 2}O{sub 4} and the coexistence of tetragonal phase along with a small fraction of hexagonal phase for BaTiO{sub 3} in the prepared composite. The dielectric permittivity increased with increasing temperature (298–373 K); however, it showed relatively high magnitude of permittivity (∼1100) and diminished dielectric loss (∼0.045) at higher frequency. Complex impedance and modulus plots exhibited responses of different electro-active regions which are explained on the basis of coexistence of resistive and comparatively conductive phases in the prepared composite. Small polaronic hopping model was employed to explain the n-type carrier’s mobility as a possible conduction mechanism; whereas the activation energies calculated from the conduction and relaxation processes were found to be comparable. These results indicate that electric/dielectric properties and relaxation phenomenon are associated to the same origin.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

A high-strength precipitation hardened cobalt-free high-entropy alloy

Recent studies on precipitation-hardened high-entropy alloys (HEAs) demonstrate their high strength and thermal stability, making them promising materials for high-temperature structural applications such as nuclear reactors. However, many existing HEAs contain cobalt (Co), which is unsuitable for nuclear applications because of the long-term activation issue of Co. Co is also expensive and considered a critical material for other applications. Therefore, it is desired to exclude Co from the composition. A Co-free (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 88 Ti 4 Al 8 HEA was developed and studied in this work. In contrast to previous Co-free HEAs, this alloy is close to equiatomic in its composition and promises a more pronounced high-entropy effect. Scanning electron microscopy, transmission electron microscopy, atom probe tomography, and synchrotron-based, high-energy X-ray diffraction were used to characterize this alloy and revealed a complex four-phase structure, with an FCC matrix, γ’ precipitates, and a network of B2 and χ phase particles. This structure granted 2151 MPa compressive strength and good thermal stability, but with limited ductility and slow precipitation kinetics. A strengthening analysis of the alloy shows that the B2 and χ provided the most significant strengthening contribution, adding 312 MPa and 788 MPa respectively. Furthermore the strengthening effect from the nanoscale γ' is also considerable, adding 608 MPa in total. This study lays the foundation for the continued development of high-strength Co-free HEAs with improved and satisfactory ductility.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Compositionally graded aluminum-silicon alloy fabricated via friction extrusion

Herein, a novel solid-phase gradient alloying technique was developed for a high throughput composition-microstructure-mechanical property assessment. Friction extrusion of a two-piece billet setup facilitated the formation of a seamless compositionally graded aluminum (Al)-silicon (Si) extrudate rod, with Si concentration in Al matrix gradually increasing from ~1 at% at one end to ~7 at% at the other end of the rod. We observed a strong dependence of the Al grain size, morphology, and texture on the Si concentration. The Si particles pinned the recrystallized grain boundaries resulting in refined (< 10 µm) and textured grains in the high Si content region, while the Al grains in the low Si region are equiaxed, randomly textured, and with a larger average size (~50 µm). The hardness of Al-Si gradient extrudate increases by ~50% percent with a 6 at% increase in Si content due to Hall Petch and particle strengthening effects. Our approach demonstrates the use of a solid phase processing technique to successfully produce a defect-free continuously compositionally graded bulk components thus overcoming the limitations of porosity and material heterogeneities commonly observed in other techniques such as by additive laser deposition.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Design of novel refractory equiatomic multi-principal elemental alloys based on Mo-Nb-Ti system for Gen IV reactor applications

Excellent irradiation damage resistance demonstrated by multi-principal elemental alloys (MPEAs) has sparked significant interest among researchers, prompting exploration into their vast compositional space, to validate their suitability for nuclear applications. A combined approach of thermodynamic and empirical parameters calculations alongside CALPHAD (CALculation of PHAse Diagrams) for phase formation predictions enable high-throughput material selection for sophisticated applications like nuclear, overcoming laborious and time-consuming experiments. Key thermodynamic and empirical parameters for eight novel equiatomic MPEAs, based on seven low thermal neutron cross section refractory elements, for predicting phase formation were calculated, and equilibrium and non-equilibrium simulations in CALPHAD were employed to comprehensively model the systems. Pseudo binary phase diagram simulations showed that Zr, V or equiatomic CrV additions to the base MoNbTi alloy (MoNbTi-Zr, MoNbTi-V and MoNbTi-CrV alloys) favor the formation of isomorphous body-centered cubic (BCC) phase at high temperatures, while Cr, Al, equiatomic ZrV, or equiatomic CrAl additions (MoNbTi-Cr, MoNbTi-Al, MoNbTi-ZrV or MoNbTi-CrAl alloys) limit the solubility of them. Equilibrium CALPHAD simulations at 750 oC were consistent with XRD results on MoNbTi, MoNbTiZr and MoNbTiCr alloys, and partially for others. Notably, elemental segregation observed in the backscattered electron (BSE) scanning electron microscopy (SEM) images of the alloys was accurately simulated through non-equilibrium Scheil solidification calculations in CALPHAD, further verified by experiments. The precipitation of TiCr2 Laves phase in Cr containing MoNbTiCr and MoNbTiCrAl was accurately predicted while discrepancies were noted in MoNbTiCrV. The equilibrium simulations also provided insights into phase compositions at specific temperatures offering a pathway for tailoring the desired microstructure and properties of these systems. Empirical parameters calculations successfully predicted random solid solution in the base MoNbTi alloy, and with an exception in MoNbTiV and MoNbTiAl, predicted intermetallic precipitation in the rest, especially, Laves phase precipitation in Cr containing alloys.

36 - MATERIALS SCIENCE↗
DOE OSTI2022

Sputter deposition of high electrical resistivity Au-Ta alloy coatings on rotating substrates

Sputter deposition of gold-tantalum alloy coatings is a key process for manufacturing hohlraums for magnetically-assisted inertial confinement fusion implosions. In this report we describe direct current magnetron sputter deposition of ~ 10 - μ~ 10 - μm-thick films of Au-80 at.% Ta onto rotating sphero-cylindrical hohlraum and planar Si witness substrates. Emphasis is given to how film microstructure and properties are affected by main deposition parameters, including argon working gas pressure, substrate bias, and the source composition (a single alloyed target compared to co-sputtering from two elemental targets). Experimental findings are correlated with distributions of landing energies and incident angles of depositing species calculated by Monte Carlo simulations of ballistic collisions and gas phase atomic transport. Deposition conditions characterized by low energetics of depositing species favor the formation of a β-Ta-like phase. Implications of these results to hohlraum fabrication are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Room-Temperature Ferroelectric LiNb 6 Ba 5 Ti 4 O 30 Spinel Phase in a Nanocomposite Thin Film Form for Nonlinear Photonics

Tetragonal tungsten bronze (TTB) materials are one of the most promising classes of materials for ferroelectric and nonlinear optical devices, owing to their very unique noncentrosymmetric crystal structure. In this work, a new TTB phase of LiNb 6 Ba 5 Ti 4 O 30 (LNBTO) has been discovered and studied. A small amount of a secondary phase, LiTiO 2 (LTO), has been incorporated as nanopillars that are vertically embedded in the LNBTO matrix. The new multifunctional nanocomposite thin film presents exotic highly anisotropic microstructure and properties, e.g., strong ferroelectricity, high optical transparency, anisotropic dielectric function, and strong optical nonlinearity evidenced by the second harmonic generation results. An optical waveguide structure based on the stacks of α-Si on SiO 2 /LNBTO–LTO has been fabricated, exhibiting low optical dispersion with an optimized evanescent field staying in the LNBTO–LTO active layer. Lastly, this work highlights the combination of new TTB material designs and vertically aligned nanocomposite structures for further enhanced anisotropic and nonlinear properties.

36 MATERIALS SCIENCE↗