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DOE OSTI2025

Long-term thermal aging behavior and strength reduction in a laser powder bed fusion 316H stainless steel

The long-term thermal stability of structural alloys is essential for ensuring the safe and reliable operation of nuclear reactors and other power plants. While extensive research has explored the effects of thermal aging on conventional stainless steels, the behavior of additively manufactured (AM) alloys remains less understood. This study examines the thermal aging response of laser powder bed fusion (LPBF) 316H stainless steel (SS) at temperatures ranging from 550 °C to 750 °C over durations of up to 10,000 h (approximately 1.14 years). Advanced characterization techniques, including electron microscopy and synchrotron X-ray diffraction, were used to investigate dislocation recovery and phase evolution. Based on these findings, a time-temperature-precipitation (TTP) diagram was developed for LPBF 316H SS, revealing a 10- to100-fold acceleration in precipitation kinetics compared to wrought 316H SS. A physics-informed model was calibrated using the short-term experimental data, enabling predictions of average precipitate sizes, volume fractions of M 23 C 6 and Laves phases, and changes in molybdenum solute concentration for aging up to 1 × 10⁶ h (114 years). These microstructural insights were further utilized to estimate yield strength and extrapolate strength reduction factors over the extended aging period. Despite the accelerated aging kinetics, LPBF 316H SS demonstrated superior yield strength retention compared to its wrought counterpart. In conclusion, this study establishes a framework for evaluating long-term performance using short-term experimental data and supports the accelerated qualification of AM materials for high-temperature structural applications.

Laser powder bed fusion↗

DOE OSTI2025

Kinetics of amorphous defect phases measured through ultrafast nanocalorimetry

Recognition of the role of extended defects on local phase transitions has led to the conceptualization of the defect phase, localized thermodynamically stable interfacial states that have since been applied in a myriad of material systems to realize significant enhancements in material properties. Here, we explore the kinetics of grain boundary confined amorphous defect phases, utilizing the high temperature and scanning rates afforded by ultrafast differential scanning calorimetry to apply targeted annealing/quenching treatments at high rates capable of capturing the kinetic behavior. Four Al-based nanocrystalline alloys, including two binary systems, Al–Ni and Al–Y, and two ternary systems, Al–Mg–Y and Al–Ni–Y, are selected to probe the materials design space (enthalpy of mixing, enthalpy of segregation, chemical complexity) for amorphous defect phase formation and stability, with correlative transmission electron microscopy applied to link phase evolution and grain stability to nanocalorimetry signatures. A series of targeted isothermal annealing heat treatments is utilized to construct a Time–Temperature-Transformation curve for the Al–Ni system, from which a critical cooling rate of 2400 °C/s was determined for the grain boundary confined disordered-to-ordered transition. Finally, a thermal profile consisting of 1000 repeated annealing sequences was created to quantify the recovery of the amorphous defect phase following sequential annealing treatments, with results indicating remarkable microstructural stability after annealing at temperatures above 90% of the melting temperature. This work contributes to a deeper understanding of grain boundary localized thermodynamics and kinetics, with potential implications for the design and optimization of advanced materials with enhanced stability and performance.

Amorphous defect phases↗

DOE OSTI2026

Functional Nano-to-Microstructures by Jet Printing and Direct Ink Writing

Jet-based printing techniques and direct ink writing have emerged as complementary, convergent technologies serving as key platforms in additive manufacturing for functional nano- to microscale architectures. This review highlights how these approaches enable fine feature resolution and three-dimensional structures in advanced electronics and biointerfacing applications. The interplay of fluid mechanics, viscoelastic ink rheology, droplet–substrate interactions, and drying dynamics is examined as a critical determinant of printing fidelity. Application-focused case studies, from flexible thin-film transistors to bioprinted artificial tissues, demonstrate how precise structural control via printing translates to enhanced device performance and new functionality in electronic and biological systems. Finally, we discuss the challenges and future opportunities driving the evolution of these printing platforms toward autonomous, adaptive, and intelligent manufacturing systems.

Luo, Junchen [Sichuan Univ. of Arts and Science (C↗

DOE OSTI2026

Effects of high-dose neutron irradiation at light-water reactor relevant temperature on the mechanical properties of SiC/SiC composites

For this study, the neutron dose-dependent evolutions and the underlying mechanisms of properties of SiC fiber-reinforced SiC matrix (SiC/SiC) composites at a temperature relevant to light-water reactors (∼600 K) were investigated and analyzed. Chemical vapor infiltrated (CVI) SiC/SiC composites reinforced with Hi-Nicalon Type S or Tyranno SA3 fiber were neutron-irradiated to doses up to 30 dpa. The irradiated composites retained their flexural strengths. The thermal diffusivity and dimensional changes were mostly retained from 2.0 to 30.2 dpa. Discrepancies in irradiation responses among CVI SiC/SiC composites from different sources were found. Additional microstructural analysis using Raman spectroscopy and numerical analysis on irradiation effect on residual stress were used to explain how the microstructural variables, especially of carbon interphases, affect the mechanical properties in the 30–40 dpa dose range.

Continuous fiber-reinforced ceramic matrix composi↗

DOE OSTI2026

Radiation damage in tungsten under high-energy He-ion irradiation

Tungsten (W) is a primary candidate for plasma-facing components (PFCs) in fusion reactors and hybrid fission-fusion reactors. However, W suffers from severe microstructural damage under Helium (He) ion irradiation in operation conditions. Key irradiation parameters, including incident ion energy, fluence, and irradiation temperature, are known to determine the formation of He bubbles and dislocation loops, which ultimately lead to the degradation of mechanical properties, such as radiation hardening and ductile-to-brittle transition temperature (DBTT) shifts. Various strategies, for instance, interface engineering and alloying, have been developed to enhance He irradiation tolerance in W to address these challenges. Studies in the recent two decades have enhanced the understanding of the underlying mechanisms that drive defect evolution and mechanical performance degradation, thereby offering more insights into the design of more resilient W-based materials for extreme environments.

Liu, Yinghang [Purdue University]↗

DOE OSTI2026

Reduced‐Order Modeling of Energetic Materials Using Physics‐Aware Recurrent Convolutional Neural Networks in a Latent Space (LatentPARC)

Physics-aware deep learning (PADL) has gained popularity for use in spatiotemporal dynamics simulations, such as those in computational modeling of energetic materials (EM). We show that the challenge PADL methods face while learning complex field evolution problems can be simplified and accelerated by decoupling it into two tasks: learning complex geometric features in evolving fields and modeling dynamics over these features in a lower-dimensional feature space. We build upon our previous work on physics-aware recurrent convolutional neural networks (PARC). PARC embeds knowledge of underlying physics into its neural network architecture for more robust and accurate prediction of evolving physical fields. PARC was shown to effectively learn complex nonlinear features such as the formation of hotspots and coupled shock fronts in various initiation scenarios of EMs, as a function of microstructures, serving effectively as a microstructure-aware burn model. Here, we further accelerate PARC and reduce its computational cost by projecting the original dynamics onto a lower-dimensional invariant manifold, or “latent space.” The projected latent representation encodes the complex geometry of evolving fields (e.g., temperature and pressure) in a set of data-driven features. The reduced dimension of this latent space allows us to learn the dynamics during the initiation of EM with a lighter and more efficient model. We observe a significant decrease in training and inference time while maintaining results comparable to PARC at inference. This work takes steps towards enabling rapid prediction of EM thermomechanics at larger scales and characterization of EM structure–property–performance linkages at a full application scale.

Mathematics and Computing↗

DOE OSTI2025

Modulation of thermal conductivity of iron-doped ß-Ga2O3 by helium-ion irradiation

This study examines the impact of helium-ion irradiation on the thermal conductivity of ß-Ga2O3. A laser-based spatial domain thermoreflectance technique is used to investigate thermal conductivity map for both un-irradiated and irradiated ß-Ga2O3, which are then validated against simulation results derived from density functional theory-based phonon transport simulations. Since helium bubble evolution was ob- served at the nanoscale using transmission electron microscopy, the simulation study was carried out on eight distinct helium-induced sites in ß-Ga2O3. Our findings indicate a reduction in thermal conductivity for the irradiated samples. Experimental results show a significant reduction in thermal conductivity in irradiated samples, with de- creases of approximately 25% along the [100] direction and 40% along [001] directions. Phonon transport simulations closely replicate these findings, particularly when helium occupying interstitial sites, predicting reductions of ˜53% along [100] and ˜50% along [001] directions. This work underscores the role of irradiation-induced microstructural changes in the heat transport properties of ß-Ga2O3 which is crucial for its application in sensor devices in extreme environments.

36 - MATERIALS SCIENCE↗

DOE OSTI2025

Experimental and Theoretical Thermokinetic Analysis of the Na 3 VO 4 –CO 2 Reaction System under Different Physicochemical Conditions

Sodium vanadate (Na 3 VO 4 ) was synthesized, structural and microstructurally characterized as well as tested as possible carbon dioxide (CO 2 ) captor through thermodynamic calculations in addition to thermogravimetric dynamic and isothermal analyses. Ceramic structural characterization evidenced the formation of the Na 3 VO 4 crystal phase, while microstructural features evidenced dense agglomerates with a poor specific surface area, although synthesis temperature (600 °C) was not as high as that for other sodium ceramics. Na 3 VO 4 was investigated for the CO 2 capture process through dynamic and isothermal experiments, in the presence or absence of oxygen. All these experiments showed that Na 3 VO 4 possesses interesting CO 2 capture properties in a specific temperature range (520 and 600 °C). Isothermal products characterization allowed to elucidate the reaction pathway, implying the Na 4 V 2 O 7 formation, as possible reactive intermediate. In fact, reaction path evolution was supported with theoretical thermodynamic data. Moreover, the kinetic analysis, performed using the Avrami-Erofeev mathematical model and subsequent thermodynamic data obtention, probed the positive influence of the temperature, in both CO 2 superficial and bulk chemical sorption processes, while oxygen addition did not enhance the superficial process. Additionally, as it would be expected, kinetics were enhanced as a function of the CO 2 concentration.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Scan‐Path‐ and Initial‐State‐Dependent Superdomain Switching in (111)‐Oriented PZT

Polarization switching in ferroelectric materials arises from the collective evolution of complex domain hierarchies, yet deterministic control over these processes remains challenging. Here, we investigate scan-path- and initial-state-dependent switching in epitaxial (111)-oriented PbZr 0.2 Ti 0.8 O 3 thin films using automated AFM-based writing combined with quantitative 3D piezoresponse force microscopy. We show that the scan trajectory acts as an experimentally accessible control parameter for superdomain formation. Box-in-box raster scans reproducibly stabilize ordered stripe superdomains with a reduced subset of symmetry-allowed variants, whereas spiral trajectories generate frustrated mixed-variant states with a broader distribution of final microstructures. Automated pulsing experiments further show that the local superdomain configuration at the nucleation site strongly influences the final written morphology. Phase-field modeling qualitatively reproduces the contrast between representative initial-state geometries and supports the role of compatibility constraints among competing ferroelastic pathways. These findings establish scan-path and initial-state engineering as practical handles to program ferroic order in hierarchical ferroelectric domain structures.

Vasudevan, Rama K. [Oak Ridge National Laboratory ↗

DOE OSTI2025

Cross-scale modeling and experimental integration for advancing cathode electrolyte interphase studies in high energy density lithium-ion batteries

Electrochemical interfaces are critical to the performance and durability of lithium-ion batteries (LIBs). The solid electrode-electrolyte interphase (SEI and CEI) structures that form during cycling can passivate reactive surfaces, ensuring safe operation, but also may contribute to performance degradation. Understanding the microscopic factors influencing interphase formation, growth, and evolution is essential for balanced battery design. While significant research has focused on the anode-electrolyte interphase (SEI), the cathode-electrolyte interphase (CEI) remains less explored, despite its importance in high-voltage and advanced battery technologies. Challenges in conducting in-situ or operando experiments arise from the occluded nature of these interfaces and the long timescales involved, often leading to biased interpretations. A validated multi-scale, multi-physics modeling approach, integrated with advanced characterization techniques, can effectively elucidate the intrinsic stability of electrolyte and cathode surfaces, the impact of chemical heterogeneity, and the role of microstructural features on CEI performance. In conclusion, this article reviews current modeling and simulation strategies for studying CEI in advanced LIBs and highlights opportunities for future methodological advancements and experimental integration.

Cathode-electrolyte interphase↗

DOE OSTI2026

Morphology-driven oxygen evolution performance of NiO x nanostructures and implications for hole transport in perovskite solar cells

Morphology-controlled nanostructures provide an effective strategy to modulate both oxygen evolution reaction (OER) activity and photovoltaic performance in perovskite solar cells (PSCs). However, achieving low OER overpotentials and high power conversion efficiency (PCE) simultaneously through morphology engineering remains challenging. In this work, nickel oxide (NiO x ) nanostructures with spindle-like (NiO x -NS) and plate-like (NiO x -NP) morphologies were synthesized and evaluated as bi-functional OER catalysts and hole transport layers (HTLs) in inverted PSCs. Structural and thermal analyses reveal that NiO x -NS crystallizes into a cubic phase at a lower temperature (300 °C), whereas NiO x -NP requires higher calcination temperatures, reflecting differences in precursor microstructure. Electrochemical measurements indicate that NiO x -NS calcined at 300 °C delivers the lowest OER overpotential (395 mV at 10 mA cm −2 ), outperforming NiO x -NP calcined at 400 °C (565 mV) and 500 °C (474 mV). This enhanced activity is ascribed to favorable surface strain, increased defect density, and advantageous facet exposure. When used as HTLs, NiO x -NS also delivers the highest PCE (13.25%) among all tested devices, exceeding those based on NiO x -NP and commercial NiO x , owing to improved hole extraction and interfacial contact. Overall, this study highlights the importance of morphology control and thermal processing in tailoring NiO x for multifunctional nanomaterials in electrocatalytic and photovoltaic applications.

36 MATERIALS SCIENCE↗

DOE OSTI2027

A multi-region approach for the analysis of porous materials and gas-solid reactions using USAXS-SAXS-WAXS: application to CaO carbonation

The reaction rate of gas-solid non-catalytic reactions is typically investigated using reactant conversion data over time and ex-situ measurements of the porous solid reactant textural properties; these data enable the experimental estimation of the initial intrinsic reaction rate, whereas the evolution of the textural properties and the reaction rate over time are evaluated theoretically using reaction models. In this work, a different methodology is presented, based on: a) in-situ time-resolved USAXS-SAXS-WAXS measurements of the solid sample, and b) a multi-region modeling approach; this methodology allows for the estimation of the textural properties and the intrinsic reaction rate at any time during the reaction. Referring to a reaction in which a solid product is obtained from a solid reactant and a gaseous reactant, the porous particle is described as consisting of several distinct regions with different microstructural properties, and both a gas-solid reaction model and a SAXS model are derived and applied to the carbonation of porous CaO. The proposed reaction model highlights the role of the inaccessible reactant and accurately predicts the solid reactant conversion versus time profile. The SAXS model accurately predicts the measured linear trends of the Porod invariant and of the pre-factor of the power law scattering profile versus CaO mass fraction; in the absence of chemical reactions, the proposed equations extend classical SAXS theory to porous materials containing macropores and nonporous solid phases in addition to standard nanoscale inhomogeneous regions.

CO2 solid sorbents↗

DOE OSTI2025

Investigation of the Sensitivity of Tropical Cyclogenesis to Aerosol Intervention

Abstract As risks from tropical cyclones (TCs) are fueled by climate change escalation, there is an urgent need for transformational solutions to complement traditional approaches. Seeding TCs using aerosols can be a promising method to reduce cyclone intensity, supported by theoretical understanding of the microphysical effects of aerosols on TC clouds. The ideal time to intervene effectively in TCs is likely during their initial stage, before TC wind speeds reach their peak. However, studies exploring potential aerosol effects on TC formation remain scarce. This study investigates how a TC embryo responds to the addition of aerosols of varying sizes using the Weather Research & Forecasting (WRF) model coupled with a spectral‐bin microphysics model. We found that aerosols of different sizes and concentrations distinctively affect the pre‐TC vortex's microstructure and dynamics. Fine and ultrafine aerosols enhance the latent heat of condensation, freezing, deposition, and riming, initially intensifying the vortex. However, this results in enhancement of the cold pool, thereby reducing inflow and surface fluxes, subsequently weakening the vortex. Coarse aerosols produce the opposite effect to that of fine and ultrafine aerosols. Coarse aerosols lead to a slower initial acceleration owing to enhanced warm rain. However, the resulting weaker cold pool is insufficient to effectively reduce the strength of the vortex at the later stage. This study provides critical insights into how aerosols of varying sizes and concentrations modulate the energy cascade and impact the evolution of a TC embryo, laying the groundwork for further research on TC risk management through aerosol intervention.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2026

The porosity surrounding carbides and second phase stringers in monolithic U-10Mo fuel plate after irradiation

Post-irradiation microstructure characterization plays an important role in qualifying the low-enriched uranium (LEU) monolithic U-10 wt%Mo plate-type fuel for United States high-performance research reactors (USHPRRs) program. Inhomogeneous features resulting from manufacturing and irradiation processes, including carbides, second phase stringers, and extensive void spaces caused by the combining of small porosities, may increase the risk of heat concentration in local regions of the fuel plate over the operating conditions. In this study, characteristics of carbides, stringers, and porosity after multiple levels of irradiation at varying fission densities were studied by electron microscopes to decipher the morphology of pores and the porosity evolution in U-10 wt%Mo. For carbides, the result shows that porosities start forming on UMo grain boundaries, then on UMo/carbides interfaces as the burn-up going higher. However, the porosities surrounding carbides grow larger than the ones on UMo grain boundaries. The porosities around the uranium carbides could interconnect to form larger void space. The study revealed that the void spaces larger than 5 µm were found around uranium carbides after high burnup, while no evidence was observed to support the similar voids formed near second phase stringers even though the size of the stringers (> 50 µm) was much larger than uranium carbides (< 20 µm). The evolution of porosities suggests that the formation of second phase stringers may not create more significant porosities compared to regular uranium carbides regions during fuel operating conditions.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2026

Forensic characterization of surrogate nuclear explosion debris: radiochemical and spectroscopic strategies for method validation

Surrogate nuclear explosion debris (SNED) has emerged as a critical platform for advancing post-detonation nuclear forensic analysis in the absence of readily accessible historic materials. SNED enables controlled investigation and validation of analytical methodologies used to interrogate the chemical, isotopic, radiological, and microstructural signatures preserved in nuclear explosion debris. This review presents an integrated assessment of destructive and non-destructive analytical techniques commonly employed within decision-driven nuclear forensic workflows. Each technique is discussed individually while highlighting how it contributes to different stages of post-detonation analysis. Core methods – including gamma and alpha spectrometry, ICP-MS, TIMS, SIMS, SEM-EDS, XRF, LIBS, vibrational spectroscopy, and X-ray absorption spectroscopy – are critically evaluated with respect to forensic maturity, information content, and matrix limitations. Emphasis is placed on the role of SNED in benchmarking multi-modal workflows and identifying gaps in reproducing heterogeneity, fractionation, and radiation-driven evolution relevant to forensic attribution.

X-ray spectroscopic methods↗

DOE OSTI2024

Transforming an Ionic Conductor into an Electronic Conductor via Crystallization: In Situ Evolution of Transference Numbers and Structure in (La,Sr)(Ga,Fe)O 3–x Perovskite Thin Films

Mixed-conducting perovskites are workhorse electrochemically active materials, but typical high-temperature processing compromises their catalytic activity and chemo-mechanical integrity. Low-temperature pulsed laser deposition of amorphous films plus mild thermal annealing is an emerging route to form homogeneous mixed conductors with exceptional catalytic activity, but little is known about the evolution of the oxide-ion transport and transference numbers during crystallization. Here the coupled evolution of ionic and electronic transport behavior and structure in room-temperature-grown amorphous (La,Sr)(Ga,Fe)O 3-x films as they crystallize is explored. In situ ac-impedance spectroscopy with and without blocking electrodes, simultaneous capturing-synchrotron-grazing-incidence X-ray diffraction, dc polarization, transmission electron microscopy, and molecular dynamics simulations to evaluate isothermal and non-isothermal crystallization effects and the role of grain boundaries on transference numbers is combined. Ionic conductivity increases by ≈2 orders of magnitude during crystallization, with even larger increases in electronic conductivity. Consequently, as crystallinity increases, LSGF transitions from a predominantly ionic conductor to a predominantly electronic conductor. The roles of evolving lattice structural order, microstructure, and defect chemistry are examined. Grain boundaries appear relatively nonblocking electronically but significantly blocking ionically. The results demonstrate that ionic transference numbers can be tailored over a wide range by tuning crystallinity and microstructure without having to change the cation composition.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Correlation between microstructure and residual stress formation in friction stir welded armor steels characterized by neutron diffraction

Friction stir welding (FSW) is a solid-state joining process that minimizes the heat-affected zone (HAZ) compared with fusion-based arc welding, making it well suited for joining martensitic armor steels where hardness and ballistic resistance are critical. This study investigates residual stress formation in three defect-free FSW butt-joint configurations relevant to armored-vehicle fabrication: similar rolled homogeneous armor (RHA–RHA, Case 1), similar high-hardness armor (HHA–HHA, Case 2), and dissimilar HHA–RHA (Case 3) joints produced under temperature-controlled conditions (770 °C). Neutron diffraction was employed to quantify the magnitude and spatial distribution of residual stresses in the longitudinal, transverse, and normal directions and to correlate them with weld microstructure and hardness. Tensile residual stresses were concentrated in the softened HAZ, reaching approximately 300 MPa for Case 2 and 400 MPa for Case 1 (≈50–70 % of the base-metal yield strength; ∼581 MPa for RHA and ∼566 MPa for HHA), while compressive residual stresses dominated the stir zone. The spatial extent of tensile stresses scaled with the width of the softened HAZ, which was largest in the dissimilar HHA–RHA joint and smallest in the HHA–HHA joint. Full-width-at-half-maximum (FWHM) analysis revealed low microstrain in overtempered HAZ regions and high microstrain in the stir zone associated with severe plastic deformation and fresh martensite formation. This work demonstrates that residual stress evolution in FSW of martensitic armor steels is governed not primarily by peak temperature or thermal contraction, as inferred from fusion-welding analogies, but by the competition between transformation-induced volumetric expansion and tempering-induced stress relaxation. The relative dominance of these mechanisms is shown to depend on alloy hardenability and local thermal history, leading to more extensive HAZ softening and broader tensile stress regions in the lower-hardenability RHA steel. These findings establish a transferable mechanistic framework for optimizing solid-state joining strategies in high-strength steels and other transformation-hardening alloys beyond armor applications.

Friction stir welding↗

DOE OSTI2025

Temperature and dose effects on dislocation loops in self-ion irradiated high-purity iron

Body-centered cubic (BCC) Fe-based alloys are promising candidate materials for advanced nuclear reactors. However, a detailed understanding of irradiation induced dislocation loop microstructure development remains unresolved. It is a widespread belief that 〈001〉 loops become increasingly favorable over ½〈111〉 loops as irradiation temperature rises above ∼300 C. Unfortunately, the temperature effects on 〈001〉 loop have been primarily examined in in-situ irradiation on TEM thin foils but poorly explored on bulk Fe due to exceedingly limited experimental studies on bulk specimens, raising concerns about the potential influence of TEM thin foil artifacts on observed results. Here, in this study, we conducted experiments on ultra-high purity BCC Fe specimens irradiated with 6.7–8 MeV Fe ions over a wide temperature range on bulk samples. We investigated the effects of temperature (T irr = 250–500 °C), dose rate (10⁻⁵ to 10⁻³ dpa/s), and dose (0.35 to 3.5 dpa) on the formation and evolution of 〈001〉 and ½〈111〉 loops as well as cavity (void) formation. Post-irradiation Burgers vector analysis via g•b method on dislocation segments and loops revealed that 〈001〉 loop fraction does not show a monotonic positive correlation with irradiation temperature. Combined with previous and current theoretical as well as experimental findings, we explore the temperature effects on all existing models of 〈001〉 loop formation. We conclude that the prevailing reports regarding the dominance of 〈001〉 loops in Fe at elevated temperatures are mainly attributable to the loss of glissile ½〈111〉 clusters in TEM thin foil experiments.

36 MATERIALS SCIENCE↗