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At least 379 records · Page 21
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Upcycling of aluminum Twitch scrap via Shear Assisted Processing and Extrusion (ShAPE)

Aluminum is publicly perceived as recyclable, but mixed alloys and impurities in aluminum scrap require dilution via energy-intensive primary aluminum or downcycling to low-quality castings. In this study, cast billets of shredded aluminum scrap (Twitch) were blended with pre-consumer AA 6061, extruded into tubes via Shear Assisted Processing and Extrusion (ShAPE), and aged to T1 and T6 tempers. Microscopy reveals that ShAPE refined and distributed the deleterious AlFeSi phases. Furthermore, the Twitch extrusions had tensile properties comparable to AA 6061 yet without homogenizing or adding primary aluminum. Energy savings were 85% compared to conventional extrusion of primary aluminum alloys.

ShAPE↗
DOE OSTI2020

Relationship between ductility and the porosity of additively manufactured AlSi10Mg

Additive manufacturing via selective laser melting can result in variable levels of internal porosity both between build plates and within components from the same build. In this work, sample porosity levels were compared to tensile properties for 176 samples spanning eight different build plates. Sample porosity was measured both by Archimedes density, which provided an estimation of overall porosity, and by observation of voids in the fracture surface, which provided an estimation of the porosity at the failure plane. The porosity observed at the fracture surface consistently demonstrated higher porosity than that suggested by Archimedes density. The porosity values obtained from both methods were compared against the mechanical results. Sample porosity appears to have some correlation to the ultimate tensile strength, yield strength, and modulus, but the strongest relationship is observed between porosity and ductility. Three different models were used to relate the fracture surface porosity to the ductility. The first method was a simple linear regression analysis, while the other two models have been used to relate porosity to ductility in cast alloys. It is shown that all three models fit the data well over the observed porosity ranges, suggesting that the models taken from casting theory can extend to additively manufactured metals. Finally, it is proposed that the non-destructive Archimedes method could be used to estimate an approximate sample ductility through the use of correlations realized here. Such a relationship could prove useful for design and for a deeper understanding of the impact of pores on tensile behavior.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Co-, Ni- and Fe-rich grain-boundary phases enhance creep resistance in θ'-strengthened Al-Cu alloys

Here, microstructural evolution and creep response were investigated in the cast Al-5.0Cu-0.3Mn-0.2Zr (wt.%) alloy with and without addition of slow-diffusing, intermetallic-forming elements Fe, Ni, or Co. Baseline Al-5.0Cu-0.3Mn-0.2Zr alloy exhibits high creep resistance at 300 °C, up to ~75 MPa, which is attributed to high-aspect-ratio, intragranular θ'-Al 2 Cu precipitates that effectively suppress dislocation climb. However, θ'-Al 2 Cu precipitate-free zones form along grain boundaries upon heat treatment, whose extent is amplified during subsequent creep. Such weak regions experience dislocation creep, leading to strain localization and acceleration of grain-boundary sliding. Adding Ni and Co, individually or in combination, leads to the formation of grain-boundary precipitates (Al 9 Co 2 , Al 3 Ni 2 ) which are resistant to coarsening, thus suppressing the formation of θ'-Al 2 Cu precipitate-free zones. This microstructure provides high creep resistance at stresses up to 75–80 MPa, with strain rates much lower than in unmodified Al-5.0Cu-0.3Mn-0.2Zr. Adding Fe, which results in extensive decoration of grain boundaries with coarsening-resistant Al 7 Cu 2 Fe, and then increasing the Cu content to compensate for the Cu loss to this new phase, leads to a new Al-7.4Cu-1.6Fe-0.3Mn-0.2Zr alloy with creep resistance at 300 °C that surpasses known cast aluminum alloys. Adding Fe to improve the creep resistance of Al-Cu alloys is both cost-effective and sustainable. Our findings offer guidelines applicable to various alloy systems on controlling the evolution of precipitate-free zones and its ensuing effects on creep deformation.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Microstructural refinement of an Al-Ce-Mg alloy via Shear Assisted Processing and Extrusion

Al-Ce alloys have attracted recent interest because of their high thermal stability due to the low solubility of Ce in the Al matrix. The Al 11 Ce 3 eutectic phase gives excellent strain hardening behavior and moderate high-temperature strength in the as-cast state. However, its strengthening effect is limited by its coarse as-cast structure. Therefore, alternative manufacturing methods such as additive manufacturing or equal channel angular pressing have been applied to refine the Al 11 Ce 3 phase to good effect. However, these techniques are both expensive and time-consuming. Therefore, this study aims to use Shear Assisted Processing and Extrusion (ShAPE), an emerging solid phase processing technique that is more easily scalable than the previously mentioned methods. ShAPE can produce useful cross-sections of an Al-8Ce-4Mg alloy while refining the Al 11 Ce 3 phase to produce a higher strength material. It was found that a low temperature ShAPE process can improve the room temperature yield strength by ~60 % compared to a binary Al-4Mg alloy. Additionally, the high-temperature yield strength of the Al-Ce alloys increased by 20%, with a simultaneous 15% improvement in ductility compared to the binary Al-Mg alloy. Finally, these results highlight the potential for ShAPE as a processing technique for Al-Ce alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Influence of the as-built microstructure on the recrystallization of an additively manufactured Inconel939 Ni-based superalloy

This study investigates the influence of the as-built microstructure on the recrystallization (RX) behavior and mechanical properties of the Ni-based superalloy Inconel 939 produced by laser powder bed fusion (PBF-LB/M). Two distinct as-built microstructures were obtained by varying the hatch distance (h d ): a columnar, strongly textured condition (h d =50, termed h d 50) and an equiaxed, weakly textured condition (h d =70, termed h d 70)). Both were subjected to nine solution treatments combining three temperatures (1100, 1150, and 1200 °C) and three holding times (1, 4, and 8 h). Comprehensive microstructural characterization was conducted to assess grain morphology, texture, grain boundary character, dislocation density, and precipitate distribution. Recrystallization was found to be significantly slower than in cast counterparts, requiring higher temperatures and longer times for completion. The initial microstructure plays a decisive role: full RX was achieved only in hd70 specimens after treatment at 1200 °C for 8 h, whereas hd50 samples exhibited delayed and incomplete RX under identical conditions. This behavior is attributed to the finer grain size and higher fraction of high-angle grain boundaries in hd70, which promote recrystallization. Mechanical testing revealed that hd70 samples subjected to a 1200 °C/8 h treatment followed by standard double ageing show higher yield and tensile strengths across the investigated temperature range than both printed and cast Inconel939 processed under conventional conditions, albeit with slightly reduced ductility. The enhanced mechanical performance is attributed to the larger grain size, which limits grain boundary sliding. These results demonstrate the critical importance of controlling the as-built microstructure and tailoring post-processing strategies to optimize high-temperature performance of PBF-LB/M Inconel939.

Inconel939↗
DOE OSTI2022

Minimizing thickness variation in monolithic U-10Mo fuel foil and Zr interlayer during hot rolling: A microstructure-based finite element method analysis

Low-enriched uranium alloyed with 10 wt. % molybdenum (U-10Mo) has been identified as a promising alternative to highly enriched uranium fuel for the United States’ high performance research reactors. The monolithic U-10Mo fuel plate consists of a metallic U-10Mo fuel foil with a 25 µm Zr interlayer and a relatively thick cladding of aluminum alloy 6061. The Zr interlayer is typically applied during the hot co-rolling process, and this process dictates the uniformity of the Zr interlayer. Thickness variation observed in the U-10Mo and Zr interlayer has been attributed to several sources: the initial grain size of the U-10Mo castings, can materials, rolling temperature, inhomogeneous molybdenum content, and porosity in the cast U-10Mo. This thickness variation limits the ability to meet the dimensional specification; thus, a better understanding of the factors causing the nonuniform thickness is needed. In this work, we used a novel, microstructure-based finite element method to model the hot rolling process to address these concerns. Grain microstructures in U-10Mo were tessellated and explicitly considered in the finite element model. Each grain was assigned a random material property to mimic the grain strength variations induced by different grain orientations. Simulations were performed using six steel can thicknesses, four grain sizes, and with or without a Zr interlayer to investigate the influences of those variables on the thickness nonuniformity. The simulation results showed that a thinner steel can and finer U-10Mo grain size reduce thickness variations in both the U-10Mo fuel foil and Zr interlayer. The direct findings from the simulations and analysis can be used to optimize the hot rolling schedule, reduce fabrication defects, and meet the dimensional specifications. The proposed microstructure-based finite element model can be also coupled with experimental microstructure characterization data, images, and models to simulate multi-pass hot rolling.

36 MATERIALS SCIENCE↗
DOE OSTI2021

A Markov framework for generalized post-event systems recovery modeling: From single to multihazards

State-dependent models can be used to represent the system recovery process as a series of stochastic transitions from lower to higher functional states. However, the applications of these models have been limited in scope and there is a lack of a generalized recovery modeling framework. A generalized framework would permit a robust forecasting of systems and system-of-systems recovery under multiple hazards, and more broadly, would contribute to community disaster preparedness. This paper develops a generalized post hazard-event recovery modeling framework based on state-dependent Markov-type processes. We then apply the proposed framework to solve a spectrum of problems that range from hind-casting single-system recovery following a single hazard event to forecasting post-event trajectories under multiple hazards and modeling the recovery of a system-of-systems. First, Markov chains are used to hind-cast the observed recovery for a portfolio of buildings affected by the 2014 South Napa, California, earthquake. Next, Markov processes are used to formulate a parametric post hazard-event recovery model, which can be updated using Bayesian statistics when relevant datasets become available. Semi-Markov processes are then used to develop a more general model of single hazard recovery, which accounts for the intensity of the loading and level of damage caused by the event. Semi-Markov processes with non-renewal features are then used to account for multihazard interactions in a post-event recovery model, and applied to a case study that involves a community in Charleston, South Carolina. Lastly, Markov-type processes are combined with Bayesian networks to model the recovery of residential, commercial, educational, and industrial buildings (system-of-systems) following a hazard event. Overall, these applications demonstrate the versatility of the Markov framework towards handling recovery problems with varying levels of complexity.

42 ENGINEERING↗
DOE OSTI2021

Growth-Controlled Broad Emission in Phase-Pure Two-Dimensional Hybrid Perovskite Films

Two-dimensional hybrid metal halide perovskites (2D perovskites) are attractive for light-emitting devices and other applications because their emission is tunable across the visible spectrum. The emission profile of 2D perovskites can be broadened via a variety of mechanisms and is further complicated by the presence of impurities. Here, the challenge of making phase-pure films in Ruddlesden–Popper phases [(A') 2 (A) n–1 B n X 3n+1 structure] is overcome by using a single A/A'-site cation, ethylammonium (EA), whose optimal size also prohibits the formation of off-target phases. In the (EA) 2 (EA) n–1 Pb n Br 3n+1 family, the low-energy, broad emission observed in bulk crystals is reduced in spin-cast, polycrystalline films. This decrease in broad emission, attributed to phonon-mediated processes, is correlated with the strain in polycrystalline films that is observed by X-ray scattering. Photothermal deflection spectroscopy shows that strain also increases the electronic disorder near the free exciton absorbance. Broad emission in films can be recovered by slowing growth kinetics, which removes the strain acquired from spin-casting and increases the domain size. Furthermore, these results help extend the utility of 2D perovskites by suggesting design rules for the growth of thin films with the targeted phase and emission.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Cross-Linked Polyphosphazene Blends as Robust CO2 Separation Membranes

An effective cross-linking technique allows a viscous, highly gas permeable hydrophilic polyphosphazene to be cast as solid membrane films. By judicious blending with other polyphosphazenes to improve mechanical properties, a membrane exhibiting the highest CO2 permeability (610 barrer) combined with good CO2/N2 selectivity (35) among polyphosphazenes is described here. The material demonstrates performance stability after 500 hours of exposure to a coal-fired power plant flue gas, making it attractive for use in carbon capture applications. Its CO2/N2 selectivity under conditions up to full humidity is also stable, and although the gas permeability does decline, the performance is fully recovered upon drying. The high molecular weight of these heteropolymers also allows them to be cast as a thin selective layer on an asymmetric porous membrane, yielding CO2 permeance of 1200 GPU, CO2/N2 pure gas selectivity of 31, which does not decline over 2000 hours due to physical aging. In addition to gas separation membranes, this cross-linked polyphosphazene can potentially be extended to other applications such as drug delivery or proton exchange membranes which take advantage of the polyphosphazene’s versatile chemistry.

Kusuma, Victor↗
DOE OSTI2026

A Versatile Method for Creating Ultrathin Films of Polyzwitterions with Antifouling Properties

Protein repellent (i.e., antifouling) properties of ultrathin polymeric films have been ascribed to the formation of a dense layer of adsorbed polymers, which causes steric hindrance to protein adsorption on underlying substrates. The antifouling properties of the films are hypothesized to be independent of polymer hydrophilicity based on previous studies involving uncharged polymers. Here, to test the hypothesis and extend it to the realm of charged polymers, we have developed a grafting method for creating ultrathin layers of polyzwitterions on solid surfaces. To demonstrate the efficacy of this method, poly[1-(3-sulfopropyl-1)-2-vinylpyridinium betaine] (P2VPPS) was synthesized via free-radical polymerization and immobilized onto surfaces by using a photoreactive benzophenone derivative as the cross-linker, which was covalently bonded to either quartz or Si/SiOx substrates through a silane anchor. We found that ultrathin films with thicknesses of less than 10 nm can be obtained in dry states using 365 nm ultraviolet (UV) cured/cross-linked surface coatings. These films were found to be hydrophilic and undergo structural rearrangements in the presence of water. The antifouling performance of the films was evaluated using Pseudomonas aeruginosa strain PAO1 bacterium as the fouling agent and exhibited antifouling properties with a kinetic control via the coating method (i.e., spin-coating and drop-casting). In particular, the surface area coverages due to the PAO1 cell attachment on the quartz substrates coated with P2VPPS were found to be ∼5% and ∼0% for the spin-coated and drop-casted films, respectively, after 4 h. These results show that the grafting method can be used to generate surfaces with antifouling properties based on ultrathin films of polyzwitterions.

Pseudomonas aeruginosa↗
DOE OSTI2020

Edge States Drive Exciton Dissociation in Ruddlesden–Popper Lead Halide Perovskite Thin Films

Efficient photovoltaic cells based on thin films of solution-processed 2D Ruddlesden–Popper hybrid perovskites (RPPs) represent an exciting breakthrough due to their enhanced tunability and chemical stability relative to those fabricated from 3D phases. However, reports of efficient charge separation and current collection are in apparent contradiction with the well-known enhancement of the exciton binding energy in multilayered halide perovskites, which should lower the device’s internal quantum efficiency and voltage. This controversy has led to various proposals for the electronic and physical structure of RPP thin films, including phase inhomogeneity as the driving force for exciton dissociation and transport. We address this apparent paradox in high-quality hot-cast RPP films by correlating ultrafast transient absorption spectroscopy with X-ray scattering measurements. We show that a hot-casting fabrication method produces highly phase pure n = 3 (BA) 2 (MA) n-1 Pb n I 3n+1 RPP structures. The high-phase purity and large grain sizes allow us to observe vertical transport of excitons via a diffusive process and allow us to determine that charge separation is primarily driven by dissociation at surface localized subgap electronic states. Furthermore, we analyze the differential absorption kinetics in films of varying thickness to directly determine that the excitonic diffusion constant is ~0.18 cm 2 s –1 . We propose that a surface localized structural distortion, observed using surface selective grazing incidence X-ray scattering measurements, is responsible for the creation of the surface localized defect states. We find that the density and spatial distribution of these defect states is a function of preparation conditions.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2025

On-Demand Selection of the Latent Domain Orientation in Spray-Deposited Block Copolymer Thin Films

With their ability to self-assemble spontaneously into well-defined nanoscale morphologies, block copolymer (BCP) thin films are a versatile platform to fabricate functional nanomaterials. An important challenge to wider deployment of BCPs in nanofabrication is combining precise control over the nanoscale domain orientation in BCP assemblies with scalable deposition techniques that are applicable to large-area, curved, and flexible substrates. Here, in this study, we show that spray-deposited smooth films of a nominally disordered BCP exhibit latent orientations, which can be prescriptively selected by controlling solvent evaporation during spray casting. Subsequent solvent vapor annealing triggers assembly toward highly ordered cylindrical morphologies along the pathway determined by solvent evaporation in the prior spray deposition stage. Faster evaporation promotes assembly of vertically oriented cylinders spanning the entire film thickness (100–300 nm). In comparison, slow solvent evaporation permits intermicellar aggregation and incipient cylinder formation in solution, which induces horizontal cylinder assembly upon annealing. The evaporatively controlled latent orientation mechanism presented herein elucidates how nonequilibrium phenomena during casting govern successive self-assembly pathways and facilitates a versatile method to dictate the domain orientation of BCP thin films on demand on flexible and highly curved substrates or in distinct pattern areas on the same substrate.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Structural complexity biases vegetation greenness measures

Vegetation ‘greenness’ characterized by spectral vegetation indices (VIs) is an integrative measure of vegetation leaf abundance, biochemical properties and pigment composition. Surprisingly, satellite observations reveal that several major VIs over the US Corn Belt are higher than those over the Amazon rainforest, despite the forests having a greater leaf area. This contradicting pattern underscores the pressing need to understand the underlying drivers and their impacts to prevent misinterpretations. Here we show that macroscale shadows cast by complex forest structures result in lower greenness measures compared with those cast by structurally simple and homogeneous crops. The shadow-induced contradictory pattern of VIs is inevitable because most Earth-observing satellites do not view the Earth in the solar direction and thus view shadows due to the sun–sensor geometry. The shadow impacts have important implications for the interpretation of VIs and solar-induced chlorophyll fluorescence as measures of global vegetation changes. For instance, a land-conversion process from forests to crops over the Amazon shows notable increases in VIs despite a decrease in leaf area. In conclusion, our findings highlight the importance of considering shadow impacts to accurately interpret remotely sensed VIs and solar-induced chlorophyll fluorescence for assessing global vegetation and its changes.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2025

Pressure induced irreversible phase transformation in an ordered high-entropy alloy

We report on a pressure induced irreversible phase transformation in an ordered eutectic high-entropy alloy (EHEA) AlCoCrFeNi2.1. The suction cast sample was synthesized by arc melting of raw elements resulting in an ordered B2 and FCC phase mixture for eutectic AlCoCrFeNi2.1 alloy. This phase mixture was confirmed by transmission electron microscopy (TEM) where superlattice reflections corresponding to ordered B2 phase were observed while the FCC phase remains disordered. The B2 phase was observed to be enriched in Nickel and Aluminum while the surrounding FCC phase is enriched in Fe, Cr and Co. The suction-cast EHEA sample was studied by X-ray diffraction under high pressure in a diamond anvil cell with platinum pressure marker to 73 GPa at ambient temperature. The B2 to FCC phase transformation is completed by 3 GPa in sharp contrast to BCC to FCC phase transition of 21 GPa in additively manufactured EHEA samples. The X-ray diffraction and TEM studies of pressure recovered samples show presence of only FCC grains without any specific orientation with respect to starting sample. These results are consistent with molecular dynamics simulations that the presence of B2 phase aids in the formation of the B2 to FCC phase transition under high pressures.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Revealing temperature-dependent polymer aggregation in solution with small-angle X-ray scattering

We report that improving the morphology of bulk heterojunction active layers remains a primary challenge for organic photovoltaics (OPVs), and much research has been devoted to achieving this through modifying OPV casting solutions to control film formation and crystallinity. Yet, the solution conformation of conjugated polymers used in OPVs is largely unknown. Here, we report observations of temperature dependent aggregation (TDA) through small-angle X-ray scattering (SAXS) investigations of polymer conformation in chlorobenzene:dichlorobenzene casting solvent as a function of temperature for PffBT4T-2OD, a polymer known to display TDA, and its derivative PffBT3T-2OD which displays significantly reduced TDA. We find that, upon cooling below 80 °C, PffBT4T-2OD forms large crystalline aggregates in solution, while its derivative PffBT3T-2OD forms mostly amorphous aggregates of similar size with some evidence of short-range order. This change in solution aggregation behavior is reflected in the lack of gelation by PffBT3T-2OD upon film deposition by spin coating. Grazing-incidence wide-angle X-ray scattering (GIWAXS) revealed a preferred face-on π–π stacking orientation for PffBT3T-2OD films while PffBT4T-2OD's π–π stacking peak was isotropic. We combine these findings to suggest that the presence of crystalline seed aggregates in PffBT4T-2OD solution quickly form an isotropic crystallite network upon cooling while PffBT3T-2OD's amorphous aggregates more slowly crystallize resulting in improved processability of PffBT3T-2OD.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

3D printing of architected sulfur cathodes with dual-site atomic catalysts for accelerated polysulfide kinetics and Li-ion transport in high areal-loading lithium–sulfur batteries

The practical deployment of lithium–sulfur batteries (LSBs) is hindered by fundamental limitations in conventional slurry-cast cathodes, including poor sulfur utilization, sluggish ion transport, and low areal capacity, particularly in thick electrodes required for high energy density. To address these challenges, we present direct ink writing (DIW) as an additive manufacturing strategy to fabricate advanced current-collector-free, 3D-printed sulfur cathodes (3DP S@CoNi-DSACs/NC) with hierarchically porous architectures that enhance lithium-ion diffusion, promote electrolyte penetration, and reduce interfacial resistance. The synergistic effects of Co/Ni dual-atom sites accelerate redox kinetics and mitigate polysulfide shuttling. As a result, the optimized 3DP cathode with a sulfur loading of 5.4 mg cm −2 demonstrated excellent rate capability, delivering a high reversible capacity of 1041.4 mAh g −1 at 1C with 85.5% capacity retention after 1000 cycles, significantly outperforming its cast counterpart. Remarkably, even at a higher sulfur loading of 8.1 mg cm −2 , the 3DP cathode maintains outstanding performance, achieving a discharge capacity of 1538.4 mAh g −1 and an areal capacity of 12.5 mAh cm −2 at 0.1C. This study not only demonstrates the functional integration of catalytically active materials into 3D printable sulfur cathode architectures but also offers a scalable and transformative platform for building high-performance LSBs beyond conventional electrode manufacturing methods.

3D electrode↗
DOE OSTI2025

Dynamic response of 17-4 stainless steel as a function of manufacturing method and heat treatment

We present a series of plate-impact experiments on 17-4 stainless steel to study the effect of manufacturing method and heat treatment on the Hugoniot elastic limit (HEL), Hugoniot, phase transformation stress, and spallation strength. Two traditional manufacturing methods were considered, wrought processing and casting, as well as two additive manufacturing methods, laser powder-bed fusion (LPBF) and wire-fed electron beam (EBAM). For both LPBF and EBAM 17-4 stainless steel variants, two billets were printed, enabling the application of two unique heat treatments. The HEL stress depended heavily on the thermal history, with the HEL increasing after the formation of Cu-rich precipitates via heat treatment. The Hugoniot response both below and above the phase transition was unaffected by the manufacturing method or heat treatment. The phase transition stress depended heavily on the thermal history, with its variation being attributed to the presence of various microstructural features. This is supported by a marked increase in the phase transition stress after precipitation hardening. These results suggest that the notion of the phase transition stress being dictated by bulk composition is an oversimplification and the stress fields generated by the meso-scale structure are a dominant force. The spallation strength was lower in the cast material compared to all other 17-4 stainless steel variants due to the presence of brittle δ-ferrite inclusions. Additionally, a drop in the tensile strain-rate was observed in the spallation response above the phase transition stress, which was hypothesized to stem from the kinetics of the reversion to the low-pressure phase during spall.

Compressive stress↗