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At least 487 records · Page 27

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DOE OSTI2022

Intermediate-phase engineering via dimethylammonium cation additive for stable perovskite solar cells

Achieving the long-term stability of perovskite solar cells is arguably the most important challenge required to enable widespread commercialization. Understanding the perovskite crystallization process and its direct impact on device stability is critical to achieving this goal. The commonly employed dimethyl-formamide/dimethyl-sulfoxide solvent preparation method results in a poor crystal quality and microstructure of the polycrystalline perovskite films. In this work, we introduce a high-temperature dimethyl-sulfoxide-free processing method that utilizes dimethylammonium chloride as an additive to control the perovskite intermediate precursor phases. By controlling the crystallization sequence, we tune the grain size, texturing, orientation (corner-up versus face-up) and crystallinity of the formamidinium (FA)/caesium (FA) y Cs 1-y Pb(I x Br 1-x )3 perovskite system. A population of encapsulated devices showed improved operational stability, with a median T80 lifetime (the time over which the device power conversion efficiency decreases to 80% of its initial value) for the steady-state power conversion efficiency of 1,190 hours, and a champion device showed a T80 of 1,410 hours, under simulated sunlight at 65 degrees C in air, under open-circuit conditions. In conclusion, this work highlights the importance of material quality in achieving the long-term operational stability of perovskite optoelectronic devices.

14 SOLAR ENERGY↗

DOE OSTI2024

Realizing Steady-State Microbunching with Optical Stochastic Crystallization

Optical Stochastic Cooling (OSC) is a state-of-the-art beam cooling technology first demonstrated in 2021 at the IOTA storage ring at Fermilab's FAST facility. A second phase of the research program is planned to run in early 2025 and will incorporate an optical amplifier to enable significantly increased cooling rates and greater operational flexibility. In addition to beam cooling, an OSC system can be configured to enable advanced control over the phase space of the beam. An example operational mode could enable crystallization, where the particles in a bunch are locked into a self-reinforcing, regular microstructure at the OSC fundamental wavelength; we refer to this as Optical Stochastic Crystallization (OSX). OSX represents a new path toward Steady-State Microbunching (SSMB), which may enable light sources combining the high brightness of a free-electron laser with the high repetition rate of a storage ring. Such a source has applications from the terahertz to the extreme ultraviolet (EUV), including high-power EUV generation for semiconductor lithography. This contribution will discuss the status of the OSC experimental program and its potential to achieve the first demonstration of SSMB during the upcoming experimental run.

Wallbank, M.↗

DOE OSTI2025

Realizing Steady-State Microbunching with Optical Stochastic Crystallization

Optical Stochastic Cooling (OSC) is a state-of-the-art beam cooling technology first demonstrated in 2021 at the IOTA storage ring at Fermilab's FAST facility. A second phase of the research program is planned to run in 2026 and will incorporate an optical amplifier to enable significantly increased cooling rates and greater operational flexibility. In addition to beam cooling, an OSC system can be configured to enable advanced control over the phase space of the beam. An example operational mode could enable crystallization, where the particles in a bunch are locked into a self-reinforcing, regular microstructure at the OSC fundamental wavelength; we refer to this as Optical Stochastic Crystallization (OSX). OSX represents a new path toward Steady-State Microbunching (SSMB), which may enable light sources combining the high brightness of a free-electron laser with the high repetition rate of a storage ring. Such a source has applications from the terahertz to the extreme ultraviolet (EUV), including high-power EUV generation for semiconductor lithography. This contribution will discuss the integration of OSX development as part of the OSC program at IOTA. The design of an accelerator lattice to enable the mechanism and associated high fidelity simulations will be shown, and a path to realizing an experimental demonstration will be discussed.

Wallbank, Michael James [Fermilab]↗

DOE OSTI2025

Steady-State Microbunching using Optical Stochastic Cooling

Optical Stochastic Cooling (OSC) is a state-of-the-art beam cooling technology first demonstrated in 2021 at the IOTA storage ring at Fermilab's FAST facility. A second phase of the research program is planned to run in 2026 and will incorporate an optical amplifier to enable significantly increased cooling rates and greater operational flexibility. In addition to beam cooling, an OSC system can be configured to enable advanced control over the phase space of the beam. An example operational mode could enable crystallization, where the particles in a bunch are locked into a self-reinforcing, regular microstructure at the OSC fundamental wavelength; we refer to this as Optical Stochastic Crystallization (OSX). OSX represents a new path toward Steady-State Microbunching (SSMB), which may enable light sources combining the high brightness of a free-electron laser with the high repetition rate of a storage ring. Such a source has applications from the terahertz to the extreme ultraviolet (EUV), including high-power EUV generation for semiconductor lithography. This contribution will discuss the integration of OSX development as part of the OSC program at IOTA. The design of an accelerator lattice to enable the mechanism and associated high fidelity simulations demonstrating the beam dynamics will be shown, and a path to realizing an experimental demonstration will be discussed.

Wallbank, Michael James [Fermilab]↗

DOE OSTI2024

Realizing Steady-State Microbunching with Optical Stochastic Crystallization

43 PARTICLE ACCELERATORS↗

DOE OSTI2021

Coupling Thermomechanical Processing and Alloy Design to Improve Textures in Mg-Zn-Ca Sheet Alloys

Abstract The effect of Ca and Zn additions on the microstructure and texture evolution during thermomechanical processing of Mg-Zn-Ca sheet alloys was systematically investigated and quantified. Plane strain compression testing in a Gleeble thermomechanical simulator was used to physically simulate a 10-pass rolling schedule, while allowing for careful control and monitoring of the processing parameters. Textures in the as-deformed ternary alloy samples demonstrate a weak maximum basal intensity and spreading in the transverse direction. Increasing the Zn content to 3.2 wt.% in the ternary alloys resulted in samples that exhibited weak textures in the as-deformed state. Importantly, static recrystallization (SRX) during post-deformation annealing of these alloys promoted a desirable annular texture, with the c -axis tipped from the normal direction and a lower basal texture intensity. The evolution in texture during SRX is associated with as-deformed microstructures with broad grain orientation spreads and a low degree of recrystallization.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Microstructure refinement of hot deformed Dy-free NdFeB magnets through a novel cold sintering approach by pressure-assisted spark plasma sintering

Anisotropic fine-grained Dy-free NdFeB high-performance magnets were produced using a novel cold sintering approach by pressure-assisted spark plasma sintering (SPS). The NdFeB nanocrystalline ribbon powders were subjected to cold sintering below 450 °C using pressure-assisted SPS, followed by hot deformation at 710 °C and 810 °C via SPS. Results indicate that cold sintering below 450 °C effectively restricts grain growth in the NdFeB magnets, yielding sub-100 nm scale grains across both fine-grained regions and most coarse-grained regions. The refined grain structure achieved through cold sintering allows for a lower hot deformation temperature as compared with the magnet by conventional sintering, as finer grains allow easier deformation and grain sliding/rotation. This process produces a highly fine-grained and anisotropic microstructure to achieve high magnetic performance (i.e., high intrinsic coercivity, remanence, and maximum energy product) in the magnets. The cold sintering (at 350 °C) and lower hot deformation temperatures required (e.g., 710 °C) help control grain coarsening and limit grain size that is commensurate with the size of a single magnetic domain of the Nd 2 Fe 14 B magnetic matrix phase, resulting in high intrinsic coercivity (H ci =11.4 kOe). Furthermore, the reduced hot deformation temperature mitigates the formation of coarse grain bands, leading to improved magnetic properties, specifically an increased remanence (B r = 14.3 kGs) and a high maximum energy product ((BH) max = 48 MGOe). In conclusion, cold sintered hot deformed NdFeB magnet also shows good thermal stability with reversible temperature coefficient α(B r )= -0.097 %/K and α(H ci )= -0.616 %/K at elevated temperatures up to 400 K.

Cold Sintering↗

DOE OSTI2023

Nanoscale reshaping of resonant dielectric microstructures by light-driven explosions

Femtosecond-laser-assisted material restructuring employs extreme optical intensities to localize the ablation regions. To overcome the minimum feature size limit set by the wave nature of photons, there is a need for new approaches to tailored material processing at the nanoscale. Here, we report the formation of deeply-subwavelength features in silicon, enabled by localized laser-induced phase explosions in prefabricated silicon resonators. Using short trains of mid-infrared laser pulses, we demonstrate the controllable formation of high aspect ratio (>10:1) nanotrenches as narrow as ~ $λ / 80$. The trench geometry is shown to be scalable with wavelength, and controlled by multiple parameters of the laser pulse train, such as the intensity and polarization of each laser pulse and their total number. Particle-in-cell simulations reveal localized heating of silicon beyond its boiling point and suggest its subsequent phase explosion on the nanoscale commensurate with the experimental data. The observed femtosecond-laser assisted nanostructuring of engineered microstructures (FLANEM) expands the nanofabrication toolbox and opens exciting opportunities for high-throughput optical methods of nanoscale structuring of solid materials.

42 ENGINEERING↗

DOE OSTI2026

Mechanical behaviour of additively manufactured metals

Additive manufacturing is reshaping the production of engineering components in diverse industries, such as the automotive, aerospace, defense, and biomedical sectors, by offering unprecedented design flexibility. The non-equilibrium processing conditions of additive manufacturing generate materials with unique microstructures and tailored mechanical properties that are often unattainable through conventional routes. This review focuses on recent advances in additively manufactured metals that demonstrate distinctive mechanical behaviors, including strength-ductility synergy, microstresses and gradient plasticity, fracture and fatigue resistance, and high-temperature creep performance. Here, we examine the mechanisms and micromechanical effects arising from the heterogeneous microstructures fabricated by additive manufacturing, to guide the design of a wide range of high-performance structural materials. Furthermore, we discuss critical research needs and emerging opportunities in process control, alloy design, advanced characterization, high-fidelity computational modeling, and machine learning aimed at achieving exceptional mechanical properties in additively manufactured metals.

Additive Manufacturing↗

DOE OSTI2023

Hybrid Al Casting + AM Components for Automotive Applications

Although casting Aluminum (Al) alloys is widely used for automotive application, the conventional casting process is showing limitations for modern vehicle production. A hybrid manufacturing method that is capable of fabricating automotive structures with tailored functionality and tuned attributes at a high production rate is proposed in this project, utilizing the merits of conventional casting methods and additive manufacturing (AM) methods. Ford is interested in supplementing conventional casting processes (e.g., shape casting, high pressure die casting) with local modifications to geometry and microstructure using additive manufacturing techniques. Two additive manufacturing methods, wire-arc and laser hot-wire directed energy deposition AM process, were evaluated by deposition of 4043 filler wire onto high-pressure die cast and permanent mold cast Al-Si alloys. The feasibility of this hybrid manufacturing method was determined through trial deposition and evaluation of defects, microstructure, and mechanical properties. Laser hot-wire deposition was found to be beneficial for this application with low porosity, a refined microstructure, and mechanical properties similar to those reported in the literature for 4043. The mechanical properties of the interface between the A356 casting and deposited 4043 were found to be controlled by the weaker deposit material.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Fluid Induced Elemental and Mineralogy Alterations of Caney Shale

ABSTRACT: Studies were conducted on cores and rock cuttings recovered from two wells drilled in Caney shale in the Southern Oklahoma. Mineralogical compositions of these samples were obtained by X-Ray Diffraction (XRD) measurements using two methods of sample preparation: conventional powder (by crushing and grinding of rock fragments) and spray-drying of micronized rock powder method. Microstructure and microanalysis were acquired by Scanning Electron Microscopy/Energy Dispersive Spectroscopy (SEM/EDS). Batch experiments were then conducted using selected rock samples and fracturing fluid whilst deionized water was used as control sample for fluid/rock interaction. These were conducted at 95°C and ambient pressure for various time periods to assess the geochemical reactivity of the Caney shale. The rock samples were subsequently recovered from fluid, dried and analysis repeated using identical XRD and SEM/EDS measurements, following the same conditions. Preliminary experimental results show rock mineralogical compositions are predominantly quartz with relatively high clay content. The clay minerals are mainly illite. Carbonate content is less than 10% by weight for most samples, with other non-clay minerals pyrite, albite, dolomite, and some apatite. In general, sprayed samples showed more intense peaks and less full width at half maxima (FWHM) relative to conventional rock-powder samples. Post-experimental mineralogical changes were observed in samples with clay portions breaking down to amorphous entities. As expected, dissolution of carbonates (calcite and dolomite) was observed and newly detected dissolution of biogenic micro quartz resulted in formation of amorphous silica. 1.0 INTRODUCTION Formation of sedimentary rocks involves processes where rock sediments are emplaced with fluids starting interactions that persist over long periods. During the lithification process, sediments and fluids react and attain equilibrium state. This equilibrium is disturbed during drilling, completion, hydraulic fracturing and other operations that involve the introduction of engineered fluids into the subsurface. To return to equilibrium, dissolution and precipitation of minerals may occur. These reactions have implications on the petrophysical properties of the reservoir. Whiles dissolution and precipitation of minerals can enhance porosity and permeability, the reverse can also be true. For example, when acidic fluids are introduced into formations with high carbonate contents, carbonate minerals dissolve into solution thus increasing the porosity and permeability of the formation. In contrast, when alkaline fluids with pH above 11 are introduced into an illite-rich shale formation, the rock-fluid interaction leads to de-flocculation of illite platelets causing substantial increase in clay fines migration, consequently significant reduction in permeability (Salles et al., 2008).

Awejori, G.↗

DOE OSTI2022

Intermetallic particle heterogeneity controls shear localization in high-strength nanostructured Al alloys

The mechanical behavior of two nanocrystalline Al alloys, Al-Mg-Y and Al-Fe-Y, is investigated with in-situ micropillar compression testing. Both alloys were strengthened by a hierarchical microstructure including grain boundary segregation, nanometer-thick amorphous complexions, carbide nanorod precipitates with sizes of a few nanometers, and submicron-scale intermetallic particles. The maximum yield strength of the Al-Mg-Y system is measured to be 950 MPa, exceeding that of the Al-Fe-Y system (680 MPa), primarily due to a combination of more carbide nanorods and more amorphous complexions. Both alloys exhibited yield strengths much higher than those of commercial Al alloys, and therefore have great potential for structural applications. However, some micropillar specimens were observed to plastically soften through shear banding. Post-mortem investigation revealed that intermetallic-free deformation pathways of a few micrometers in length were responsible for this failure. Further characterization showed significant grain growth within the shear band. The coarsened grains maintained the same orientation with each other, pointing to grain boundary mechanisms for plastic flow, specifically grain rotation and/or grain boundary migration. Here, the presence of intermetallic particles makes it difficult for both matrix and intermetallic grains to rotate into the same orientation due to the different lattice parameters and slip systems. Therefore, we are able to conclude that a uniform distribution of intermetallic particles with an average spacing less than the percolation length of shear localization can effectively prevent the maturation of shear bands, offering a design strategy for high-strength nanocrystalline Al alloys with both high strength and stable plastic flow.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Mechanical Performance of Additively Manufactured ODS 316L and 316H Stainless Steels

This work package within the Advanced Materials and Manufacturing Technologies (AMMT) program focused on the mechanical and microstructural characterization of oxide dispersion strengthened (ODS) stainless steels produced using advanced manufacturing techniques. The research aimed to identify an accelerated development path for ODS alloys by integrating additive manufacturing (AM) technologies with recent advancements in ODS materials and traditional manufacturing methods. For FY 24, the research specifically targeted exploring an accelerated development path for ODS alloys by combining AM technologies with these advancements. Novel AM and post-build processing routes were developed for ODS austenitic alloys, including Fe-Cr-Ni alloys such as 316L and 316H. Electron microscopy and mechanical characterizations were conducted to evaluate the impact of process variables on microstructure and properties, with the goal of optimizing these properties economically. Traditionally, producing ODS alloys involves multi-day, high-energy mechanical milling of alloy powder with yttria powder, followed by milled-powder consolidation through extrusion or other methods, and additional thermomechanical processing (TMP) for property control. To overcome the challenges associated with this complex and costly approach, we propose exploring alternative, cost-effective processing routes that emphasize AM and traditional TMP methods. The new processing routes for ODS alloys have achieved significantly higher strengths—several times greater than those of wrought stainless steels—while maintaining substantial ductility and fracture toughness. This report outlines the novel and economical AM-based processing routes for ODS austenitic alloys, combined with post-build TMPs, and discusses the mechanical and microstructural characteristics of the developed materials.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Understanding the effect of friction stir processing on electrical steel: Microstructural changes and mechanical transformations

Raising Si beyond 3.5 wt% reduces core loss but embrittles electrical steels, constraining processing and application. Here we assess friction stir processing (FSP) as a solid‑state route to enable Fe–4.0 wt% Si with improved mechanical performance. Temperature‑controlled FSP with a PcBN tool produced a defect‑free processed zone. SEM/EBSD revealed dynamic recrystallization and grain refinement from an average 110 μm in the base material to ∼20 μm in the processed region, with ∼ 80% of grains < 40 μm and a reduction in high‑angle boundary fraction to ∼65% (vs >85% in the base). Comparative mechanical property analysis shows a moderate increase in yield strength in FSP samples relative to the base material, with a significant improvement in ductility (∼35–50%). Post‑fracture EBSD identified 60° twin boundaries in the base while sub-grain formation with elevated KAM in the FSP sample. Fractography revealed a shift from quasi‑cleavage in the Base-faceted planes with river patterns, steps, and occasional secondary cracks—to ductile micro void coalescence after FSP. Following FSP, the material retains soft‑magnetic behavior, with modest shifts in saturation magnetization consistent with grain refinement and stored strain, accompanied by a clear gain in formability. These results indicate that FSP provides a viable route to deploy higher‑Si electrical steels with concurrent gains in strength and ductility.

Electrical steel↗

DOE OSTI2023

Two-dimensional glass transition–like behavior of Janus particle–laden interface

Abstract Understanding the interactive behavior of Janus particles (JPs) is a growing field of research. The enhancement in binding energy, in comparison to homogenous particles, and the dual characteristic of JPs open up new possibilities for novel applications. In many such applications, interfacial materials become subjected to flows that produce dilational and shear stresses. Therefore, it is important to understand the impact that the Janus character brings to interfaces. In this work, we study the microstructure of two-dimensional (2D) JP monolayers formed at the air–water interface and examine the shear viscoelasticity with an interface rheometer that was adapted for in situ surface pressure control via a Langmuir trough. We extend concepts from bulk rheology to data obtained from interfacial rheology as a tool to understand and predict the monolayer’s viscoelastic behavior. Finally, by calculating the time relaxation spectrum from the measured 2D dynamic moduli, we conclude that a phenomenon similar to glass transition is taking place by analogy.

42 ENGINEERING↗

DOE OSTI2025

Electroslag additive manufacturing: A pathway for high throughput near net shape production

Electroslag Additive Manufacturing (ESAM), a new high-throughput additive manufacturing (AM) method that combines Electroslag Strip Cladding (ESC) and wire arc AM (WAAM) is introduced. This combination enables the high deposition rate of ESC (more than 20 kg/h with a 60 mm strip electrode) to benefit from the precise geometric control of WAAM. As a precursor to ESAM, the ESC process is investigated in an AM context independently by evaluating both direct and staggered bead-stacking strategies and analyzing the microstructural and mechanical properties of each. This is followed by an ESAM demonstration producing an annular geometry by pairing ESC with gas tungsten arc welding (GTAW), wherein GTAW is utilized to construct annular walls that are subsequently infilled via ESC. The microstructure and mechanical properties of ESC-only AM are compared with that of the ESAM method and it is shown that printed integral retaining walls do not impact the resulting mechanical properties of ESAM. Furthermore, results indicate that ESAM-produced Alloy 625 parts exhibit tensile properties on par with cast counterparts, supporting the method’s scalability to components exceeding one metric ton, and possibly making ESAM a viable future manufacturing approach for competitive production of large-scale components currently manufactured by casting and forging.

Additive manufacturing↗

DOE OSTI2022

A Comparative Tribo-Mechanical Behavior Analysis of Laser Cladded Nitronic 60 Coating Against Wrought Nitronic 60 Alloy

In this study the tribological and mechanical behavior of a laser cladded Nitronic 60 coating on maraging steel is compared to that of a wrought Nitronic 60 alloy. A multi-layer Nitronic 60 coating was deposited using laser directed energy deposition, and its microstructure, porosity, and microhardness were characterized. The microhardness of the coated region in the laser cladded Nitronic 60 varied between 270-300 HV whereas that for wrought form was 230 HV. Controlled tribological tests under motor oil lubricated conditions were conducted at both room and elevated temperatures. The laser cladded Nitronic coating exhibited poorer wear resistance at room temperature but higher wear resistance at elevated temperature as compared to the wrought Nitronic alloy. Severe plastic deformation and fracture was observed on the laser cladded coating after the wear tests at both temperatures. Wear mechanisms were investigated based on the morphological and compositional characterization of the wear tracks.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Corrosion Electrochemistry of Chromium in Molten FLiNaK Salt at 600 °C

The manuscript revisits the corrosion behavior of pure Cr in molten FLiNaK salt at 600 °C from the perspective of corrosion electrochemistry. In this work, the potential-dependent, rate-limiting charge-transfer, and salt film-mediated mass-transport controlled regimes of Cr corrosion in FLiNaK at 600 °C are investigated. The kinetic and thermodynamic parameters that limit electrodissolution and the consideration of grain orientation on these regimes are elucidated. At low Cr(III) concentrations, the corrosion process is governed by charge transfer control at low overpotentials and is crystal orientation dependent. However, when Cr(III) concentrations are high or when there is a high overpotential, the formation of a metal fluoride salt film on the Cr surface shifts the kinetic behavior to be governed by mass transport control at all anodic potentials with a surface morphology controlled by salt film deposition location and identity. Evan’s diagrams were developed to consolidate and elucidate these observations. These findings were supported by an examination of the post-corrosion microstructure, X-ray diffraction of solidified salts, and thermo-kinetics analysis in each corrosion regime.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗