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At least 1,081 records · Page 60

Unlocking superplasticity in medium and high-entropy alloys

Superplasticity, the capacity of materials to sustain extraordinary tensile elongations at elevated temperatures, underpins a range of advanced metal-forming technologies. Conventionally, it is achieved in fine-grained alloys where deformation is dominated by grain-boundary sliding, accommodated by diffusion and dislocation activity. The advent of medium- and high-entropy alloys (M/HEAs), with their high chemical complexity and unconventional phase stability, offers new pathways to superplastic behavior beyond traditional alloy systems. Although investigated only recently, several M/HEAs already exhibit elongations that rival or exceed those of classical superplastic materials, particularly when ultrafine or metastable microstructures are engineered. Here, we review progress in understanding superplastic deformation in M/HEAs, emphasizing the interplay among composition, initial microstructure, thermomechanical processing, and microstructural evolution during high-temperature deformation. We discuss approaches to generating the fine-grained structures necessary for grain-boundary sliding, including severe plastic deformation and tailored heat treatments. We further highlight dynamic phenomena such as phase transformations, evolving grain-boundary chemistry, and deformation-induced grain refinement that can enhance plasticity in these systems. These mechanisms often shift the balance of deformation processes, enabling large elongations even outside classical criteria. Finally, we outline key challenges for application, including cost, scalability, recyclability, and microstructural stability.

klenam, Desmond [University of the Witwatersrand, ↗

Fatigue crack growth mechanisms at the microstructure scale in as-fabricated and heat treated Ti-6Al-4V ELI manufactured by electron beam melting (EBM)

Electron beam melting (EBM) is a metal powder bed fusion additive manufacturing (AM) technology that fabricates parts by selectively scanning consecutive powder layers with an electron beam. Additive manufacturing technologies are increasing in importance for aerospace and medical applications, where the demand for a fundamental understanding and predictability of static and dynamic material properties are high. Ti-6Al-4V is the most widely used and studied alloy for this technology, and is the focus of this work in its Extra Low Interstitial (ELI) variation. The layered manufacturing of metallic components by EBM creates a unique directional microstructure, and consequently, anisotropic properties. Microstructure evolution, and its influence on mechanical properties of the alloy in the as-fabricated condition, has been documented by various researchers. However, fatigue crack propagation and the effects of the directional structure have not been sufficiently studied, imposing a barrier for this technology’s potential extension to high-integrity applications. Here in this study, fatigue crack growth (FCG) both parallel and perpendicular to the build directions was studied for different stress ratios and crack growth stages. The interaction between the directional as-fabricated EBM microstructure and FCG was investigated and compared to that of the equiaxed β annealed microstructure obtained by annealing above the β transus temperature. Finally, the FCG threshold, ΔK th , was analytically modeled for the two relative crack propagation directions at different stress ratios, and FCG microstructural mechanisms were established for all three regions of crack propagation.

36 MATERIALS SCIENCE↗

Visualizing Uranium Crystallization from Melt: Experiment-Informed Phase Field Modeling and Machine Learning

The focus of this project was to observe and simulate the solidification of uranium metal at the crystallographic level from its molten state. Melting experiments were conducted at two different scales to observe microstructural evolution using either a laboratory-scale induction furnace (hundreds of grams of metal) or a microscope heating stage (hundreds of milligrams of metal), respectively. Experimental parameters and characterization data were then used to inform a phase field model of gamma-U crystal growth as dendrites with or without secondary phase impurities in the form of uranium carbide particles. Finally, training datasets were generated by the phase field model as inputs to a neural network, developed with the aim of providing a faster, cheaper surrogate model for microstructural simulations within a given parameter space. Progress is reported herein for each of these task areas. Ultimately, 1) an optical microscope heating stage capability has been stood-up for uranium metal solidification studies, 2) a phase field model was advanced to simulate multiple uranium grains growing in the presence of carbide impurity particles and 3) a neural network was constructed and optimized to predict the microstructure features of individually growing uranium crystals.

36 MATERIALS SCIENCE↗

Microstructure Optimization of Austenitic Alloy 800H (Fe-21Cr-32Ni)

The microstructural evolution, specifically of grain boundaries, precipitates, and dislocations in thermomechanically processed (TMP) Alloy 800H samples was characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), electron backscattered diffraction (EBSD), transmission electron microscopy (TEM), and atomic force microscopy (AFM). The TMP not only significantly increased the fraction of low-{Sigma} coincidence site lattice boundaries, but also introduced nanoscale precipitates in the matrix and altered the distribution of dislocations. Statistical analysis indicates that the morphology and distribution of grain boundary precipitates were dependent on grain boundary types. The microstructure optimization played a synergistic effect on the significantly increased strength with comparable ductility and enhanced intergranular corrosion resistance and creep-fatigue life compared to the as-received samples.

36 MATERIALS SCIENCE↗

Coupling Experiments and Simulations to Understand Metallic Fuel Behavior

The development of metal alloy fuels for minor actinide transmutation in fast reactor systems is of high importance. However, it faces numerous technical challenges such as: i) fuel behavior has to be benign during core off-normal events; ii) fuel has to maintain integrity to high burnup; iii) low minor actinide fabrication loss under remote handling conditions; and iv) fuel has to lend itself to low-loss recycling process. Limited experimental fuel performance data is currently available to support the selection of a fuel type for a transmutation system. Metallic fuels are being considered for application in fast reactor environment due to the high burn-up, high fissile and fertile density capability, inherent safety characteristics, favorable thermal response, and relatively easy recycling process. The uranium-plutonium-zirconium (U-Pu- Zr) based alloys are considered as one of the most promising metallic fuels for such application. In this work, we present results of microstructural characterization of Pu-Zr and U-Pu-Zr alloys and provide much needed linkage between thermal properties and microscopic scale observation. A firm understanding of microstructural evolution in reactor materials is imperative and will lead to deeper understanding of in-reactor degradation behavior, creating a new generation of radiation-resistant materials and fuels with the potential for significant increases in burn-up.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Effect of Multiple Reflow Cycles and Al{sub 2}O{sub 3} Nanoparticles Reinforcement on Performance of SAC305 Lead-Free Solder Alloy

The effect of Al{sub 2}O{sub 3} nanoparticles reinforcement on melting behavior, microstructure evolution at the interface and joint shear strength of 96.5Sn3Ag0.5Cu (SAC305) lead-free solder alloy subjected to multiple reflow cycles was investigated. The reinforced SAC305 solder alloy compositions were prepared by adding Al{sub 2}O{sub 3} nanoparticles in different weight fractions (0.05, 0.1, 0.3 and 0.5 wt.%) through mechanical dispersion. Cu/solder/Cu micro-lap-shear solder joint specimens were used to assess the shear strength of the solder joint. Differential scanning calorimetry was used to investigate the melting behavior of SAC305 solder nanocomposites. The solder joint interfacial microstructure was studied using scanning electron microscopy. The results showed that the increase in melting temperature (T{sub L}) and melting temperature range of the SAC305 solder alloy by addition of Al{sub 2}O{sub 3} nanoparticles were not significant. In comparison with unreinforced SAC305 solder alloy, the reinforcement of 0.05-0.5 wt.% of Al{sub 2}O{sub 3} nanoparticles improved the solder wettability. The addition of nanoparticles in minor quantity effectively suppressed the Cu{sub 6}Sn{sub 5} IMC growth, improved the solder joint shear strength and ductility under multiple reflow cycles. However, the improvement in solder properties was less pronounced on increasing the nanoparticle content above 0.1 wt.% of the solder alloy.

36 MATERIALS SCIENCE↗

Tailoring Thermal and Mechanical Performance Through Multimaterial Laser Powder Directed Energy Deposition of Copper and 17-4PH Stainless Steel

This study investigates the additive manufacturing (AM) processing, microstructural evolution, and resulting mechanical and thermal properties of multimaterial components combining 17-4PH stainless steel and pure copper (Cu) fabricated via laser powder directed energy deposition (LP-DED). Conventional tooling steels exhibit limited thermal conductivity, significantly constraining production throughput in high-volume processes. Incorporating Cu, with its superior thermal conductivity, could significantly enhance tool performance, though Cu and steel present metallurgical incompatibilities when processed via AM. A systematic investigation was conducted across compositions ranging from 0 to 100 wt% Cu, revealing critical thresholds influencing solidification behavior, defect formation, microstructure, hardness, and thermal transport. Optical microscopy, electron backscatter diffraction (EBSD), hardness testing, and thermal conductivity measurements provided comprehensive process–structure–property correlations. Severe hot cracking occurred at low-Cu contents (6–25 wt%), aligning generally well with crack susceptibility modeling, with an unexpected discrepancy at 25 wt%. Porosity remained low (≥99% dense) throughout the compositional spectrum. EBSD analysis revealed a transformation from columnar martensitic structures at low-Cu contents to equiaxed FCC Cu-dominated structures at higher Cu concentrations, highlighting the complex microstructural transitions driven by Cu-induced changes in solidification and phase stability. Hardness decreased from 330 HV (pure 17-4PH) to 62 HV (pure Cu), consistent with microstructural changes. Concurrently, thermal conductivity improved substantially from 13.5 W/m K to 367.9 W/m K, emphasizing Cu’s dominant role in thermal transport. The findings highlight the feasibility of leveraging compositional gradients between 17-4PH and Cu to achieve tailored tooling with optimized thermal and mechanical performance.

17-4PH↗

Controlling reversible phase transitions in rare-earth nickelates for novel memory devices

Resistive switching in correlated complex oxides is lucrative for emerging applications in neuromorphic computing, and densely scaled non-volatile memory. Electrical conductance of such complex oxides can be controllable switched across multiple orders of magnitude by either (a) electroforming a conduction channel (e.g., in tungsten oxide), or (b) inducing Mott-Hubbard transition (e.g., in rare-earth nickelates)– both via controlled migration of defects (such as oxygen vacancies) under applied bias. Nevertheless, the promise of such defect-driven electronic transitions are far from realized due to a lack of fundamental understanding of the atomic-scale processes that underlie migration and spatiotemporal evolution of oxygen vacancies over nano-to-mesoscopic length/timescales under applied electric field. In this project, we employ a synergistic integration of density functional theory (DFT) calculations, ab initio/classical molecular dynamics (AIMD/CMD) simulations, machine learning (ML), precision synthesis, and multi-modal X-ray imaging experiments to address this knowledge gap. Such an integrated approach offers to elucidate the correlations between subtle structural distortion and oxidation states; treat localized charge carriers; describe defect/ion transport in the presence of electric field; and, in turn, greatly advance the current understanding of microstructural evolution in complex oxides under applied bias. The fundamental knowledge gained from this work will enable precise control over hierarchical defect structures and unravel new routes to manipulate resistance states in complex oxides. This, in turn, will accelerate design of novel devices with desired set of neural functionalities, and high-speed densely-scaled resistive random access memory technologies.

36 MATERIALS SCIENCE↗

High-resolution neutron diffraction study of microstructural changes in nanocrystalline ball-milled niobium carbide NbC{sub 0.93}

High resolution neutron diffraction was applied for elucidating of the microstructural evolution of nanocrystalline niobium carbide NbC{sub 0.93} powders subjected to high-energy ball milling. The diffraction patterns were collected with the high resolution Fourier diffractometer HRFD by using the reverse time-of-flight (RTOF) mode of data acquisition. The traditional single diffraction line analysis, the Rietveld method and more advanced Whole Powder Pattern Modeling technique were applied for the data analysis. The comparison of these techniques was performed. It is established that short-time milling produces a non-uniform powder, in which two distinct fractions with differing microstructure can be identified. Part of the material is in fact milled efficiently, with a reduction in grain size, an increase in the quantity of defects, and a corresponding tendency to decarburize reaching a composition NbC{sub 0.80} after 15 h of milling. The rest of the powder is less efficiently processed and preserves its composition and lower defect content. Larger milling times should have homogenized the system by increasing the efficiently milled fraction, but the material is unable to reach a uniform and homogeneous state. It is definitely shown that RTOF neutron diffraction patterns can provide the very accurate data for microstructure analysis of nanocrystalline powders. - Highlights: • The NbC{sub 0.93} powder was processed by high-energy ball milling. • The microstrain and dislocation density increase with milling time increase. • The corresponding decrease in crystallite size with milling time was observed. • The material exhibits the presence of two fractions after ball milling. • The RTOF neutron diffraction data are suitable for accurate microstructure analysis.

36 MATERIALS SCIENCE↗

Quasi-static to Dynamic Response and Microstructure Development of Tantalum-Tungsten Alloys

Lawrence Livermore National Laboratory (LLNL) has a need to understand the quasi-static to dynamic mechanical response and microstructure evolution of tantalum-tungsten (Ta-W) alloys made by conventional wrought processing and additive manufacturing (AM). This two-year work scope will be performed at the Colorado School of Mines (Mines) and will include quasi-static (e.g., 10 -3 s -1 ) mechanical testing in tension and compression, along with high strain rate (Kolsky) pressure bar testing in tension and compression (e.g., 10 3 s -1 ), without and with temperature variations. Gas gun experiments at higher strain rates (e.g., over 10 3 s -1 ) will also be pursued. Complementary microstructure characterization will be performed on undeformed and deformed samples to fundamentally understand the role of processing on the microstructure characteristics and resulting deformation mechanisms that dictate the mechanical response of these alloys with variations in strain rate, temperature, and strain state. Alloys of interest will be Ta-based, containing up to 10 wt.% W. LLNL will supply initial wrought-processed material for sample machining. LLNL will also supply samples built by AM during the project for testing. Arc melting and casting may also be performed at Mines to produce small quantities of different alloys for machining and exploratory testing on an as-needed basis. This project will support multiple postdocs and graduate students at Mines, training them with the knowledge, skills, and abilities needed to study materials under extreme conditions of interest to the National Nuclear Security Agency.

36 MATERIALS SCIENCE↗

On the Effect of Quenching on Postweld Heat Treatment of Friction-Stir-Welded Aluminum 7075 Alloy

This work focuses on the effect of postweld heat treatment (PWHT) on the mechanical properties and microstructural evolution of aluminum 7075 alloy processed via friction stir welding (FSW). FSW is known to be capable of grain refinement in the nugget zone (NZ). Two different quench media (water and air) were employed for PWHT. Regardless of the quench media, the PWHT led to the occurrence of grain growth in the NZ of the FSWed aluminum 7075 alloy. Abnormal grain growth occurred in the water quenched specimen. It is shown that ductility and strength of FSWed aluminum 7075 alloy are strongly dependent on the quenching rate. Changes in the mechanical properties and microstructure reveal that only at lower cooling rate this alloy is prone to the formation of precipitate-free zones (PFZs) in the vicinity of grain boundaries. Eventually, the PFZs deteriorate mechanical properties of this alloy.

36 MATERIALS SCIENCE↗

Creep Behavior of Friction Stir Processed Haynes 282

Haynes 282 is a nickel-based superalloy designed for use in hot sections of turbines for aircraft and power generation. In these applications, elevated temperature creep performance is critical. To that end, creep behavior of friction stir processed material was carried out to investigate the high-temperature performance of this alloy. Friction stir processing of Haynes 282 was successfully completed, and the processed region was found to be defect-free. Various mechanical property characterization approaches were carried out in post-heat treated condition. Transverse tensile samples repeatedly failed in the base metal indicating 100% joint efficiency. Creep property evaluation was completed at 760 °C and at various stress levels. The creep-rupture lifetime of the processed material was similar to the base metal. Detailed electron microscopy analysis of the failed sample was carried out to understand the microstructural evolution in various locations of the sample during creep.

creep↗

Deformation, dislocation evolution and the non-Schmid effect in body-centered-cubic single- and polycrystal tantalum

A physically-informed continuum crystal plasticity model is presented to elucidate deformation mechanisms, dislocation evolution and the non-Schmid effect in body-centered-cubic (bcc) tantalum widely used as a key structural material for mechanical and thermal extremes. We show the unified structural modeling framework informed by mesoscopic dislocation dynamics simulations is capable of capturing salient features of the large inelastic behavior of tantalum at quasi-static (10 -3 s -1 ) to extreme strain rates (5000 s -1 ) and at low (77 K) to high temperatures (873 K) at both single- and polycrystal levels. Here we also present predictive capabilities of the model for microstructural evolution in the material. To this end, we investigate the effects of dislocation interactions on slip activities, instability and the non-Schmid behavior at the single crystal level. Furthermore, ex situ measurements on crystallographic texture evolution and dislocation density growth are carried out for polycrystal tantalum specimens at increasing strains. Numerical simulation results also support that the modeling framework is capable of capturing the main features of the polycrystal behavior over a wide range of strains, strain rates and temperatures. The theoretical, experimental and numerical results at both single- and polycrystal levels provide critical insight into the underlying physical pictures for micro- and macroscopic responses and their relations in this important class of refractory bcc materials undergoing large inelastic deformations.

36 MATERIALS SCIENCE↗

Current-Assisted Diffusion Bonding of Extruded Ti-22Al-25Nb Alloy by Spark Plasma Sintering: Interfacial Microstructure and Mechanical Properties

Spark plasma sintering (SPS) technology was used to current-assisted bond extruded Ti-22Al-25Nb alloy. The effects of bonding temperature (920-980 °C) and bonding time (10-30 min) on the microstructure evolution and shear strength of this alloy were investigated systematically. The temperature distribution in the specimen during the current-assisted bonding process was also analyzed by numerical simulation. It is noted that the highest temperature was obtained at the bonding interface. As the bonding temperature and bonding time increased, the voids in the interface shrank increasingly until they vanished. A complete metallurgical bonding interface could be produced at 960 °C/20 min/10 MPa, exhibiting the highest shear strength of 269.3 MPa. In addition, the shear strength of the bonded specimen depended on its interfacial microstructure. With increased bonding temperature, the fracture mode transformed from the intergranular fracture at the bonding interface to the cleavage fracture in the substrate.

36 MATERIALS SCIENCE↗

Time at Temperature Experiments on Neutron Irradiated Zircaloy-2 using Conventional & Flash DSC

Dryout events in Boiling Water Reactors (BWRs) are currently treated by NRC regulations as automatic disqualification for continued fuel rod operation, even though this criterion does not account for the rate or duration of power increases, associated changes in material behavior, or the possibility of rewetting. Operational history from Anticipated Operational Occurrences (AOOs) shows that short, transient power excursions often demand only modest heat removal, and industry experience suggests that fuel can briefly enter dryout yet return to safe, stable operation. The lack of detailed understanding of the material response during such events motivates the present series of experiments. This study uses unique and innovative methods to investigate microstructural evolution in irradiated Zircaloy-2 exposed to high temperatures in inert environments. Differential Scanning Calorimetry (DSC) and FlashDSC are combined to build a comprehensive experimental framework capable of identifying the a–ß phase transformation in zirconium and examining defect annealing under steep thermal gradients. FlashDSC enables rapid heating and cooling of Focused Ion Beam (FIB)–prepared large-area lift-outs (LALOs) of irradiated Zircaloy-2 at rates of 1,000 K/s to peak temperatures of 600°C, 750°C, and 900°C. The goal is to determine whether these conditions produce measurable microstructural changes that could influence cladding performance in typical BWR environments. Microstructural characterization includes quantifying dislocation density and assessing secondary phase particle (SPP) size and distribution using Transmission Electron Microscopy (TEM). Ongoing analysis, such as diffraction pattern indexing and 4D STEM processing, will further refine these observations.

36 - MATERIALS SCIENCE↗

Clarifying the formation of equiaxed grains and microstructural refinement in the additive manufacturing of Ti-Cu

Controlling microstructural evolution in metallic additive manufacturing (AM) is difficult, especially in producing refined as-built grains instead of coarse, directional grains. Traditional solutions involve adding inoculants to AM feedstocks, but titanium (Ti) alloys cannot employ this approach without producing detrimental secondary phases. Ti-Cu (Ti-copper) alloys offer a solution through constitutional supercooling and/or solid state thermal cycling under AM conditions. This work analyzes a compositionally graded directed energy deposition (DED) Ti-Cu build, single-melt laser tracks, and dilatometric heat treatments to evaluate if, when, and by what mechanism(s) microstructural refinement occurs. Refinement by inoculation of unmelted powder particles was also considered. Constitutional supercooling produced no net microstructural refinement as any equiaxed dendrites which form are remelted with new deposition. This finding agreed with solidification modeling of powder bed fusion-laser beam (PBF-LB) and DED builds. Solid state thermal cycling refined microstructures only during ex-situ dilatometric heat treatments, suggesting build parameter optimization is needed to achieve refinement in-situ. Accidental heterogeneous nucleation on unmelted Ti powder, originating from the different thermophysical properties of Ti and Cu, provided the most significant microstructural refinement. This work systematically assesses the microstructural refinement mechanisms of Ti-Cu in AM builds and offers insights into microstructural control in eutectoid alloys.

36 MATERIALS SCIENCE↗

Stochastic statistical theory of nucleation and evolution of nano-sized precipitates in alloys with application to precipitation of copper in iron

A consistent and computationally efficient stochastic statistical approach (SSA) is developed to study the kinetics of nucleation and evolution of nano-sized precipitates in alloys. To increase the accuracy of the method, many refinements of the previous simplified versions of this approach have been made. We consider a realistic vacancy-mediated exchange kinetics rather than the simplified direct-atomic-exchange model; use quantitative, cluster statistical methods rather than simple mean-field-type approximations; allow strong concentration and temperature dependences of generalized mobilities in the resulting kinetic equations; consider realistic alloy models based on first-principle calculations, and so on. We also introduce the 'maximum thermodynamic gain' principle to determine the key kinetic parameter of the SSA, the characteristic length of local equilibrium in the course of the nucleation process. For several realistic models of iron-copper alloys studied, the results of the SSA-based simulations of precipitation kinetics made in this work agree well with the kinetic Monte Carlo simulation results for all main characteristics of the microstructure. The approach developed is also used to study the kinetics of nucleation and changes in microstructural evolution under variations of temperature or concentration.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Hot Deformation Behavior of the 20 vol.% TiC/Cu-Al{sub 2}O{sub 3} Composites

Hot deformation behavior of the 20 vol.% TiC/Cu-Al{sub 2}O{sub 3} composite was studied using the Gleeble-1500D thermo-mechanical simulator with various strain rates at different deformation temperatures. The softening mechanism due to dynamic recrystallization was a feature of the high-temperature true stress–strain curves. The peak stress increased at the lower deformation temperature and the higher strain rate. Microstructure evolution was explored. Thermal deformation activation energy was calculated as 218.9 kJ/mol, and the constitutive equation was established. The processing map was constructed to obtain optimal processing domain of 700-850 °C and 0.001-0.04 s{sup −1} for hot working.

36 MATERIALS SCIENCE↗