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DOE OSTI2024

Effect of post-deposition heat treatment on microstructure and mechanical properties of NASA HR-1 cold spray coatings

The primary goal of this work was to examine the impact of heat treatment on the evolution of microstructure and mechanical properties of NASA HR-1 cold spray coatings. Coatings were produced employing a high pressure cold spray system using N2 and He process gases and the effect of process gas and deposition temperature on the microstructure and mechanical properties of the coatings was examined. Microstructural characterization was performed using optical microscopy, scanning electron microscopy, micro X-ray computed tomography, and electron backscatter diffraction. NASA HR-1 coatings produced with He process gas exhibited improved plastic deformation and resulted in the lowest porosity compared to those deposited with N2 process gas. All coatings showed brittle failure with limited ductility in the as-deposited condition. Heat treatment of the NASA HR-1 cold spray coatings was performed at 550°C and 950°C for 1 h to improve the mechanical strength of the coatings. Heat treatment improved the particle bonding and enhanced the mechanical properties of the cold spray coatings. Heat treatment performed at 550°C resulted in higher mechanical strength of coatings, whereas the heat treatment performed at 950°C resulted in recrystallized microstructure and improved ductility of the coatings. However, heat treatment at 950°C resulted in forming the Eta (η) phase and Ni-Ti intermetallics in all the NASA HR-1 cold spray coatings. Here, the overall results suggest that using He as process gas contributed to reduced porosity and enhanced mechanical properties of the cold spray coatings.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2023

Beyond the Stokes approximation: shallow visco-elastic ice-sheet models

Abstract The hypothesis that ice-sheet evolution is only controlled by the long-term non-Newtonian viscous behavior of ice has been challenged by observations indicating that effects like brittle failure, stick-slip sliding, tides and wave action may affect ice-sheet evolution on sub-daily timescales. Over these timescales, the quasi-static-creep approximation is no longer appropriate and elastic effects become important. Simulating elastic effects in ice-sheet models over relevant timescales, however, remains challenging. Here, we show that by including a visco-elastic rheology and reintroducing the oft neglected acceleration term back into the ice-sheet stress balance, we can create a visco-elastic system where the velocity is locally determined and information propagates at the elastic wave speed. Crucially, the elastic wave speed can be treated like an adjustable parameter and set to any value to reproduce a range of phenomena, provided the wave speed is large compared to the viscous velocity. We illustrate the system using three examples. The first two examples demonstrate that the system converges to the steady-state viscous and elastic limits. The third example examines ice-shelf rifting and iceberg calving. This final example hints at the utility of the visco-elastic formulation in treating both long-term evolution and short-term environmental effects.

58 GEOSCIENCES↗

DOE OSTI2026

Iron-Catalyzed Cross-[2 + 2] Cycloaddition of Butadiene and α,ω-Dienes for Ductile and Chemically Recyclable Poly(oligocyclobutanes)

Poly(divinyloligocyclobutanes) (pDVOCBs) are a distinct class of butadiene-derived, chemically recyclable polyolefins prepared from iron-catalyzed [2 + 2] cycloaddition followed by ruthenium-catalyzed ADMET polymerization. These polymers are highly crystalline, with high melting temperatures and unique rotator phases. The high degree of crystallinity in these materials not only leads to high stiffness over a broad temperature range but also results in brittle failure for polymers of modest molecular weights. Iron-catalyzed cross-[2 + 2] cycloaddition of butadiene and α,ω-dienes was accomplished, where the number of methylene units between the four-membered rings was systematically varied. Subsequent ADMET polymerization of the resulting telechelic oligomers provided a new class of chemically recyclable polyolefins that exhibit distinct thermomechanical properties. Specifically, methylene units induce changes in crystallinity that, in combination with the increased molecular weight, favored the formation of stable necks upon tensile deformation, with ∼10× enhanced ductility and improved toughness compared to pDVOCB. Through combined experimental and computational studies, the effects of methylene spacers on the crystal-to-rotator transition of the cyclobutane polymers were established. Ultimately, these methylene-modified cyclobutane polymers expand the range of properties and potential applications of this class of recyclable polyolefins.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Unsupervised Clustering of Microseismic Events and Focal Mechanism Analysis at the CO 2 Injection Site in Decatur, Illinois

Characterization of induced microseismicity at a carbon dioxide (CO 2 ) storage site is critical for preserving reservoir integrity and mitigating seismic hazards. We apply a multilevel machine learning (ML) approach that combines the nonnegative matrix factorization and hidden Markov model to extract spectral representations of microseismic events and cluster them to identify seismic patterns at the Illinois Basin-Decatur Project. Unlike traditional waveform correlation methods, this approach leverages spectral characteristics of first arrivals to improve event classification and detect previously undetected planes of weakness. By integrating ML-based clustering with focal mechanism analysis, we resolve small-scale fault structures that are below the detection limits of conventional seismic imaging. Our findings reveal temporal bursts of microseismicity associated with brittle failure, providing insights into the spatio-temporal evolution of fault reactivation during CO 2 injection. This approach enhances seismic monitoring capabilities at CO 2 injection sites by improving fault characterization beyond the resolution of standard geophysical surveys.

Willis, Rachel Marie [Sandia National Laboratories↗

DOE OSTI2025

Seismic Tremors From Sea‐Landfast Ice Interactions Near Utqiaġvik, Alaska

The mechanical state of Arctic landfast sea ice remains poorly constrained due to limited observations. This study investigates interactions between drifting sea ice and the coastal landfast ice near Utqiaġvik, Alaska by integrating data from broadband seismometer, Distributed Acoustic Sensing, and marine radar. We find that decreases in sea ice velocity, marking transitions from drift to compressive contact, coincide with increased seismic energy. Tremor characteristics vary seasonally with ice conditions. In January, dense ice packs produced sustained harmonic tremors with gliding and U-shaped spectral features, consistent with repetitive stick-slip motion at the ice–ice or ice–ground interface under velocity-weakening friction. In April, smaller fragmented floes generated short-lived, chaotic tremors linked to brittle failure and spatially dispersed impacts. These findings demonstrate that seismic tremors encode the mechanical properties of interacting ice, offering a new tool to distinguish ice regimes and monitor evolving Arctic coastal dynamics under climate change.

58 GEOSCIENCES↗

DOE OSTI2026

Why Firn Quakes

Snow dampens sounds, but anecdotal reports concisely describe audible propagating collapse events—firnquakes—in Antarctic and Arctic snowfields. We propose combining granular and continuum mechanics to form a testable theory for conditioning, triggering, and propagation of firnquakes consistent with scarce data. A central condition for collapse events is unconsolidated firn at depth. As firn grains compact, stresses are transmitted along force chains which carry the overburden and transition into a continuous medium by pressure sintering. This granular legacy creates solid-like supports of denser layers that keep the material below unconsolidated. Dynamic amplification triggers local brittle failure of the supports, which induces a cascade of collapse propagation. Using bulk density from ice cores as proxy for stiffness, we find the flexural wave speed by collapsing supports matches the recorded firnquake velocities on the order of 100 m/s. Our theory is to be tested in firn sheets and other compacting granular materials.

Voigtländer, A. [Lawrence Berkeley National Labora↗

DOE OSTI2022

Metamorphism-facilitated faulting in deforming orthopyroxene: Implications for global intermediate-depth seismicity

Significance The exothermic metamorphic reaction in orthopyroxene (Opx), a major component of oceanic lithospheric mantle, is shown to trigger brittle failure in laboratory deformation experiments under conditions where garnet exsolution takes place. The reaction product is an extremely fine-grained material, forming narrow reaction zones that are mechanically weak, thereby facilitating macroscopic faulting. Oceanic subduction zones are characterized by two separate bands of seismicity, known as the double seismic zone. The upper band of seismicity, located in the oceanic crust, is well explained by dehydration-induced mechanical instability. Our newly discovered metamorphism-induced mechanical instability provides an alternative physical mechanism for earthquakes in the lower band of seismicity (located in the oceanic lithospheric mantle), with no requirement of hydration/dehydration processes.

58 GEOSCIENCES↗

DOE OSTI2021

Characterizing environment-dependent fracture mechanisms of ceramic matrix composites via digital image correlation

Not provided.

Materials Science↗

DOE OSTI2021

Addressing amorphization and transgranular fracture of B 4 C through Si doping and TiB 2 microparticle reinforcing

Over the last two decades, many studies have contributed to improving our understanding of the brittle failure mechanisms of boron carbide and provided a road map for inhibiting the underlying mechanisms and improving the mechanical response of boron carbide. This paper provides a review of the design and processing approaches utilized to address the amorphization and transgranular fracture of boron carbide, which are mainly based on what we have found through 9 years of work in the field of boron carbides as armor ceramics.

36 MATERIALS SCIENCE↗

DOE OSTI2026

The 10 September 2025 M w 4.1 Earthquake in Northeastern Utah, United States: An Archetypal Continental Mantle Event

The 10 September 2025 M w 4.1 earthquake in northeastern Utah, United States, had a focal depth 68 km beneath sea level, which is ∼20–25 km greater than estimates of local crustal thickness, making it a rare example of a continental mantle earthquake (CME). The focal depth is well resolved from arrival-time inversion (nearest station ∼13 km away) and moment tensor inversion of regional waveforms. Similar to other CMEs in the Intermountain West, there were no obvious aftershocks or foreshocks, and the waveforms were enriched in high-frequency energy. Spectral modeling gives a stress drop of ∼80 MPa and a radiation efficiency of ∼0.08, albeit with large uncertainties. The high stress drop and low radiation efficiency are consistent with a dissipative source process such as thermal runaway. Also similar to previous Intermountain West CMEs, the event occurred along the boundary of the Archean Wyoming craton, where pressure–temperature conditions favor ductile deformation. We hypothesize that edge-driven or regional-scale mantle convection produces increased strain rates near the craton boundary that make either conventional brittle failure or thermal runaway feasible at relatively high pressure–temperature conditions. High conductivity inferred around the edge of the craton may suggest that fluids also contribute to CME occurrence.

Koper, Keith D. [Univ. of Utah, Salt Lake City, UT↗

DOE OSTI2022

Fine Pitch Bonding for High Density Interconnects

CTE (coefficient of thermal expansion) mismatch between two wafers has potential for brittle failure when large areas are bonded on top of one another (wafer to wafer or wafer to die bonds). To address this type of failure, we proposed patterning a polymer around metallic interconnects. For this project, utilized benzo cyclobutene (BCB) to form the bond and accommodate stress. For the metal interconnects, we used indium. To determine the benefits of utilizing BCB, mechanical shear testing of die bonding with just BCB were compared to die bonded just with oxide. These tests demonstrated that BCB, when cured for only 30 minutes and bonded at 200°C, the BCB was able to withstand shear forces similar to oxide. Furthermore, when the BCB did fail, it experienced a more ductile failure, allowing the silicon to crack, rather than shatter. To demonstrate the feasibility of using BCB between indium interconnects, wafers were pattered with layers of BCB with vias for indium or ENEPIG (electroless nickel, electroless palladium, immersion gold). Subsequently, these wafers were pattered with a variety of indium or ENEPIG interconnect pitches, diameters, and heights. These dies were bonded under a variety of conditions, and those that held a bond, were cross-sectioned and imaged. Images revealed that certain bonding conditions allow for interconnects and BCB to achieve a void-less bond and thus demonstrate that utilizing polymers in place of oxide is a feasible way to reduce CTE stress.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Laser Powder Directed Energy Deposition of Steels for Nuclear Applications

This comprehensive investigation examines the structure–property relationships in two nuclear alloy systems—Alloy 709 (A709) austenitic stainless steel and Grade 92 (G-92) ferritic/martensitic (F/M) steel—manufactured via directed energy deposition (DED) for sodium-cooled fast reactor applications. This study establishes the fundamental mechanisms for controlling microstructures for optimizing the mechanical performance of additively manufactured nuclear materials through systematic heat treatment optimization and multiscale characterization. As-deposited A709 steel develops a complex multiscale strengthening architecture consisting of a fine cellular solidification structure with diameter of 2-3 µm within10–50 µm grains, elevated dislocation densities from rapid thermal cycling, and grain boundary precipitates that activate concurrent Hall–Petch, dislocation, and precipitation hardening mechanisms to achieve exceptional properties [yield strength (YS): 603 MPa, ultimate tensile strength (UTS): 844 MPa, Vickers hardness: 220 HV] that achieve a 44% superior strength compared to that of the wrought material. Heat treatments produce different results. Solution annealing (SA) dissolves the cellular structure and reduces the hardness to 190 HV. Precipitation treatment (PT) keeps the cellular structure but adds carbides, allowing the hardness to reach 205 HV. The best approach combines both treatments (SA+PT) and creates uniform precipitate distributions with M 23 C 6 carbides at the grain boundaries and MX carbonitrides in the matrix, achieving a hardness of 195 HV. However, directional differences persist, with a 12%–15% strength variation between orientations due to the inherited layered microstructural architecture that survives aggressive heat treatment. While tensile testing at 550°C demonstrates 40%–50% thermal softening with dynamic strain aging, DED A709 steel still maintains a 71% higher YS than that of the wrought material. Ion irradiation studies (100–400 dpa) of DED A709 steel reveal progressive radiation damage with increasing void density and radiation-induced segregation causing nickel enrichment and chromium depletion, which will ultimately compromise mechanical properties. As-deposited G-92 exhibits exceptional strength (UTS: 1650–1700 MPa, 430 HV) through a complex microstructure containing both ferrite and martensite phases, a high geometrically necessary dislocation (GND) density (17.04×10 14 /m 2 ), and fine carbides. Heat treatments create distinct changes. Normalizing produces fresh martensite with the highest hardness (460 HV) and an increased GND density (20.23×10 14 /m 2 ). Tempering develops dual precipitation systems and reduces the hardness to 290 HV. The optimal approach uses sequential normalizing plus tempering, achieving balanced properties with the lowest hardness (250 HV) and a reduced GND density (11.01×10 14 /m 2 ). A processing-dependent anisotropy is observed: horizontal specimens achieve superior ductile behavior, while vertical specimens exhibit brittle failure. A tempering heat treatment successfully mitigates this anisotropic behavior by transforming the hard martensitic as-deposited structure into tempered martensite enabling both horizontal and vertical specimens to exhibit similar stress–strain characteristics with visible necking behavior. Remarkably, testing at 550°C reveals a reversal in the anisotropy, where as-deposited specimens achieve near isotropy with superior thermal stability (a 15%–20% strength reduction), while tempered specimens develop an orientation dependence with a 25%–30% strength reduction. Both alloy systems demonstrate that DED processing creates specimens with a superior strength through refined microstructural features, though with distinct strengthening mechanisms—austenitic through cellular structures and precipitates versus F/M through phase transformations and precipitates. Heat treatment optimization requires alloy-specific approaches, with A709 benefiting from controlled precipitation while G-92 requires careful phase transformation control. The results show that DED manufacturing can produce nuclear materials with exceptional performance, but directional effects and temperature-dependent behavior must be carefully considered for reactor component design and qualification.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2025

Development and Evaluation of Embrittlement Resistant Alloys for Advanced LWR Cladding

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2025

Development and Evaluation of Embrittlement Resistant Alloys for Advanced LWR Cladding

The primary challenge preventing the deployment of reactor designs that leverage wrought FeCrAl as an advanced light-water reactor (LWR) cladding is irradiation hardening and embrittlement. Wrought FeCrAl alloys experience a loss of post-irradiation ductility and fracture toughness under low-temperature neutron irradiation (< 350°C) resulting from the combined effects of dislocation loop formation and the irradiation-enhanced precipitation of Cr-rich alpha-prime precipitates throughout the microstructure. Over the past decade, significant improvements in our understanding regarding the effect of Cr and Al content have been enabled through neutron irradiations, but even optimized wrought alloys such as C26M remain vulnerable to brittle failure during storage, transportation, and handling following irradiation. This report summarizes multiple irradiation campaigns initiated over the past 7 years and provides recent insights into the effect of (1) minor alloying composition, (2) alloy processing strategy, (3) crystal structure, and (4) the use of advanced oxide dispersion strengthened (ODS) alloys. The first irradiation campaign irradiated body-centered cubic FeCrAl alloy C26M with and without elements such as Mo and Y. It also included face-centered cubic alumina-forming austenitic (AFA) alloys that have a steeper neutronic penalty but that have far superior high-temperature strength than wrought FeCrAl. Finally, this campaign compared conventional wrought C26M with the same material produced using modern powder metallurgical hotisostatic pressing (PM-HIP). The second irradiation campaign, initiated in 2018, irradiated wrought and FeCrAl-ODS materials up to 50 dpa to assess their irradiation resistance to high-doses. The results of this work indicate that wrought C26M suffers significant degradation following neutron irradiation at LWR-relevant temperatures regardless of Mo and Y content. The PM-HIP variant appears to be more resilient to irradiation-induced ductility loss in comparison with wrought variants but still loses almost all ductility by 8 dpa. Notably, the AFAs retained at least 5% total elongation after irradiation at the same dose and temperature condition, although additional deterioration may be expected at higher fluence levels. FeCrAl-ODS materials show the greatest promise as a transformative longer-term accident-tolerant fuel (LT-ATF) cladding material. The extruded 106ZY10C alloy retained 10% total elongation after 16 dpa irradiation and retained 8% total elongation after 50 dpa. Additional challenges with FeCrAl-ODS alloys also remain, including optimization of end cap joining methodologies, enhancement of fracture toughness, scaling production to prove economic viability, and optimizing post-pilger heat treatments to maximize ductility and irradiation resistance. This series of irradiations demonstrates the efficacy of the LWR testbed available within the United States for the rapid irradiation and down-selection of LT-ATF candidates. As the country rapidly accelerates its timeline for the deployment of advanced reactor concepts, the effective utilization of the High Flux Isotope Reactor for separate-effects style irradiations should continue to be prioritized to answer the final questions pertaining to LT-ATF candidates necessary for the deployment of advanced boiling water reactors and small modular reactors.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1973

Low temperature mechanical properties, fractographic and metallographic evaluation of several alloy steels

The mechanical properties are presented of alloy steels, 4130, 4140, 4340, 6150, and 8740. Test specimens were manufactured from approximately 1.00 inch (2.54 cm) diameter bar stock which had been heat treated to two different hardness levels. The following mechanical tests were performed at temperatures of 80 F (+26.7 C), 0 F (-17.8 C), -100 F (-73 C), and -200 F (-129 C): (1) tensile test (Ultimate, yield, modulus, elongation, and reduction of area), (2) notched tensile test, (3) charpy V-notched impact test (impact energy), and (4) double shear strength test (ultimate and yield). The test data indicate excellent tensile strength, notched/unnotched tensile ratios, ductility, impact, and shear properties at all test temperatures, except at -200 F (-129 C) where the impact strength of the higher strength group of alloy steels, 4130 (Rc-37) and 4140 (Rc-44) decreased to approximately 9 ft. lbs. (12 joules) and 6 ft. lbs. (8 joules), respectively. Chemical, metallographic, and fractographic analyses were also performed to evaluate microstructure, microhardness and the effect of decrease in temperature on the ductile to brittle failure transition.

Montano, J. W.↗

NASA NTRS1986

The size distributions of fragments ejected at a given velocity from impact craters

The mass distribution of fragments that are ejected at a given velocity for impact craters is modeled to allow extrapolation of laboratory, field, and numerical results to large scale planetary events. The model is semi-empirical in nature and is derived from: (1) numerical calculations of cratering and the resultant mass versus ejection velocity, (2) observed ejecta blanket particle size distributions, (3) an empirical relationship between maximum ejecta fragment size and crater diameter, (4) measurements and theory of maximum ejecta size versus ejecta velocity, and (5) an assumption on the functional form for the distribution of fragments ejected at a given velocity. This model implies that or planetary impacts into competent rock, the distribution of fragments ejected at a given velocity is broad, e.g., 68% of the mass of the ejecta at a given velocity contains fragments having a mass less than 0.1 times a mass of the largest fragment moving at that velocity. The broad distribution suggests that in impact processes, additional comminution of ejecta occurs after the upward initial shock has passed in the process of the ejecta velocity vector rotating from an initially downward orientation. This additional comminution produces the broader size distribution in impact ejecta as compared to that obtained in simple brittle failure experiments.

Okeefe, J. D.↗

NASA NTRS1986

A dynamical model of lithosphere extension and sedimentary basin formation

The effect of convection-induced stresses at the base of the continental lithosphere on surface and extensional deviatoric stresses is investigated. The biaxial strain in the continental lithosphere is controlled by power law creep in the upper and lower crust, brittle failure, and the Dorn plasticity law. The relationship between the lithosphere stress distribution and Moho temperatures is examined. The extension factors, basin subsidence, heat flow, and sediment loading of the lithosphere are studied.

Houseman, G.↗

NASA NTRS1987

Ethynylated aromatics as high temperature matrix resins

Difunctional and trifunctional arylacetylenes were used as monomers to form thermoset matrix resin composites. Composites can be hot-pressed at 180 C to react 80 percent of the acetylene groups. Crosslinking is completed by postcuring at 350 C. The postcured resins are thermally stable to nominally 460 C in air. As a result of their high crosslink density, the matrix exhibits brittle failure when uniaxial composites are tested in tension. Failure of both uniaixial tensile and flexural specimens occurs in shear at the fiber-matrix interface. Tensile fracture stresses for 0-deg composites fabricated with 60 v/o Celion 6K graphite fiber were 827 MPa. The strain to failure was 0.5 percent. Composites fabricated with 8 harness satin Celion cloth (Fiberite 1133) and tested in tension also failed in shear at tensile stresses of 413 MPa.

Hurwitz, F. I.↗