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DOE OSTI2025

Rotary Inertia Friction Welding of Dissimilar High-Strength 422 Martensitic Stainless Steel and 4140 Low Alloy Steel for Heavy-Duty Engine Piston Fabrication

AISI 422 martensitic stainless steel with superior high temperature performance (oxidation resistance and strength) is under evaluation for replacing current heavy-duty piston crown materials, AISI 4140 martensitic steel and micro alloyed steel (MAS) 38MnSiVS5, to fabricate a multimaterial piston. This multimaterial piston concept further improved power density and fuel economy by allowing heavyduty diesel engines to operate at higher temperatures and pressures. Joining AISI 422 steel piston crowns with AISI 4140 steel piston skirts is a key manufacturing step for this multimaterial piston. However, the significant differences in strength, elevated temperature flow stress, alloy chemistry, and temper resistance between these two martensitic steels cause some weldability issues (cracking) and metallurgical challenges (alloying element migration/segregation) when using conventional fusion-based welding processes. Rotary inertia friction welding (RIFW), a solid-state welding process, has been the preferred method to join 4140 crowns to 4140 skirts (and MAS crowns to MAS skirts) in high-volume production of current heavy-duty diesel engine pistons. It has been used to join these two materials with relatively comparable alloy chemistry to fabricate pistons with MAS skirts and 4140 crowns. Meanwhile, RIFW has also been a preferred method of dissimilar metal welding. However, RIFW of dissimilar high-strength martensitic steels has yet to be widely pursued. The interfacial microstructure complexities created by the thermomechanical process and highly nonequilibrium phase transformations during RIFW are a significant challenge for understanding and predicting their joining behavior and have not been reported in detail. Here, in this work, defect-free AISI 422 steel-AISI 4140 multimaterial pistons were successfully fabricated using the RIFW process. The interfacial microstructure and mechanical properties of dissimilar 422/4140 steel RIFW in the as-welded condition were experimentally studied in detail. The results provide critical baseline information for understanding RIFW mechanisms and guiding subsequent postweld heat treatment (PWHT) practice.

36 MATERIALS SCIENCE↗

DOE OSTI2026

MoS 2 Catalysts Selectively Achieve High Yield of Liquid Oxygenate from Direct Conversion of Methane via Hydroxyl Radicals

Directly converting methane (CH 4 ) into liquid oxygenates (e.g., methanol) can circumvent the cost and engineering limits of natural gas transportation and storage. However, oxygenate yields from CH 4 remain low, and sulfur present in natural gas hinders activity in most catalysts. Here, to overcome these barriers, we employ bulk molybdenum disulfide (MoS 2 ), a low-cost, robust catalyst which selectively produces large quantities of liquid oxygenates (>900 µmol/g cat ∙hr) from methane in the presence of hydroxyl (OH • ) radicals produced from dilute hydrogen peroxide (H 2 O 2 ) at 75°C. Under realistic reaction conditions, MoS 2 partially and reversibly adopts a metastable, more electrically conductive phase (1T’) that can only be observed through in situ structural probes. Herein, we elucidate that redox synergy between H 2 O 2 and MoS 2 produces active OH • radical species that selectively transform CH 4 to surface methoxy species at the gas-solid liquid interface, leading to the unitary production of liquid oxygenate at a rate competitive with more costly precious metal catalysts, without additional catalyst preparation steps.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Coupled Chemical and Mechanical Control of Phase Stability in Lanthanide-Substituted BiVO 4

Doping is widely used to enhance the photoelectrochemical performance of BiVO 4 , yet solubility limits and polymorphic stability constrain compositional tuning. Here, in this study, the role of trivalent cation substitution (Ln = La, Nd, Dy, Ho, Y) on pressure-induced phase transformations in Bi 1–x Ln x VO 4 (x ≤ 0.5) is described. Powder X-ray and neutron diffraction reveal that increasing Ln content stabilizes the tetragonal zircon-type polymorph under ambient conditions, while applied pressures of up to ∼5 GPa promote conversion to the monoclinic fergusonite-type polymorph. In-situ neutron diffraction on Bi 0.8 La 0.2 VO 4 shows a reversible monoclinic to tetragonal transition near 2–3 GPa with a bulk modulus of 147 GPa. The extent of conversion depends strongly on dopant identity, concentration, and synthetic route, with mixed-phase solid-state samples converting more efficiently than phase-pure coprecipitated materials. These results demonstrate pressure as a viable pathway to access metastable, doped BiVO 4 compositions beyond conventional solubility limits.

Sypkes, Kathryn I. [University of Sydney, NSW (Aus↗

DOE OSTI2022

A mechanistic study of the dopant-induced breakdown in halide perovskites using solid state energy storage devices

Doping halide perovskites (HPs) with extrinsic species, such as alkali metal ions, plays a critical, albeit often elusive role in optimising optoelectronic devices. Here, we use solid state lithium ion battery inspired devices with a polyethylene oxide-based polymer electrolyte to dope HPs controllably with lithium ions. We perform a suite of operando material analysis techniques while dynamically varying Li doping concentrations. We determine and quantify three doping regimes; a safe regime, with doping concentrations of <10 20 cm –3 (2% Li : Pb mol%) in which the HP may be modified without detrimental effect to its structure; a minor decomposition regime, in which the HP is partially transformed but remains the dominant species; and a major decomposition regime in which the perovskite is superseded by new phases. We provide a mechanistic description of the processes mediating between each stage and find evidence for metallic Pb (0) , LiBr and LiPbBr 2 as final decomposition products. Combining results from synchrotron X-ray diffraction measurements with in situ photoluminescence and optical reflection microscopy studies, we distinguish the influences of free charge carriers and intercalated lithium independently. We find that the charge density is equally as important as the geometric considerations of the dopant species and thereby provide a quantitative framework upon which the future design of doped-perovskite energy devices should be based.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Structural transformation of dusty plasma crystal in dc discharge plasma by changing confinement ring bias

We report an experimental study of the structural transition of a stable complex plasma crystal to a solid-liquid phase coexistence by the controlled adjustment of the confinement potential, while keeping all other parameters constant. The experiments are carried out on a tabletop linear dusty plasma experimental device, which consists of a circular powered electrode and an extended grounded cathode plate. A stationary crystal of melamine formaldehyde particles is formed in a background of argon plasma inside a confining ring that is isolated from the cathode by a ceramic cover. The stable crystal structure breaks in the core region and transitions to a coexistent state by carefully changing the confining potential, thereby modifying the sheath structure. The transition is confirmed by evaluating the variation in different characteristic parameters such as the pair correlation function, local bond order parameter, and dust kinetic temperature as a function of confining bias potential. It is found that melting in the core is due to the onset of dust fluctuations in the layers beneath the topmost layer, which grow in amplitude as the confining bias potential is reduced below a threshold value. The present technique of changing confinement provides a unique feature to study structural transitions of plasma crystals without affecting the overall plasma parameters.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2024

Structural transformation of dusty plasma crystal in dc discharge plasma by changing confinement ring bias

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2021

Detailed in situ ATR-FTIR spectroscopy study of the early stages of C-S-H formation during hydration of monoclinic C3S

The early stages of tricalcium silicate hydration has been studied by in situ ATR-FTIR spectroscopy. A method for data reduction based on background correction and subtraction of spectra of pure components is presented, which makes it possible to describe the kinetic evolution of the calcium silicate hydrate phase upon hydration with great detail. The results obtained are in full agreement with recently reported, detailed solid-state NMR spectroscopy measurements. As ATR-FTIR spectroscopy does not require any isotope enrichment in order to increase the signal intensities and is a widely available technique, we suggest that our study opens up an avenue towards detailed in situ characterization of hydrating cementitious systems and hydrating systems in general.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Submodule-Level Decentralized Control for Cascaded Quadruple Active Bridge-Based Medium-Voltage Converters

High-power, low-voltage DC (LVDC) loads, such as AI data centers, electric vehicle fast-charging hubs, and hydrogen electrolyzers, are accelerating the deployment of solid-state transformers (SSTs) that directly interface medium-voltage AC (MVAC) to LVDC, streamlining power delivery. This paper proposes a submodule-level decentralized control strategy for an SST comprising a cascaded H-bridge (CHB) active rectifier on the MVAC side and per-module quadruple-active-bridge (QAB) converters on the LVDC side with local controllers. The proposed strategy eliminates the need for high-fidelity, real-time cross-isolation communication by synchronizing all active bridges to a common heartbeat signal and enabling the primary- and secondary-side controllers to generate independent local control signals (phase shifts). The resultant phase shifts naturally govern average and double-line frequency power transfer between active bridges, enabling each side to meet its control objectives using only local measurements. Detailed controller design considerations are presented based on a stability analysis. Comprehensive electromagnetic-transient simulations demonstrate tight DC-link voltage regulation, high-quality grid currents, and robust operation under load transients and grid disturbances, without real-time communication among the submodule controllers. These results indicate that the proposed scheme can significantly enhance the reliability, scalability, and flexibility of cascaded bridge-based medium-voltage converters.

24 POWER TRANSMISSION AND DISTRIBUTION↗

DOE OSTI2026

Submodule-Level Decentralized Control for Cascaded Quadruple Active Bridge-Based Medium-Voltage Converters: Preprint

24 POWER TRANSMISSION AND DISTRIBUTION↗

NASA NTRS1999

An Overview of the Electrostatic Levitation Facility at Nasa's Marshall Space Flight Center

Containerless processing represents an important area of research in microgravity materials science. This method provides access to the metastable state of an undercooled melt. Containerless processing provides a high-purity environment for the study of reactive, high-temperature materials. Reduced gravity affords several benefits for containerless processing; for example, greatly reduced positioning forces are required and therefore samples of greater mass can be studied. Additionally, in reduced gravity larger specimens will maintain spherical shape which will facilitate modeling efforts. Space Systems/LORAL developed an Electrostatic Containerless Processing System (ESCAPES) as a materials science research tool for investigations of refractory solids and melts. ESCAPES is designed for the investigation of thermophysical properties, phase equilibria, metastable phase formation, undercooling and nucleation, time-temperature-transformation diagrams, and other aspects of materials processing. These capabilities are critical to the research programs of several Principal Investigators supported by the Microgravity Materials Science Program of NASA. NASA's Marshall Space Flight Center (MSFC) recently acquired the ESCAPES system from LORAL. MSFC is now developing a levitation facility in order to provide a critical resource to the microgravity materials science research community and to continue and enhance ground-based research in the support of the development of flight experiments during the transition to Space Station.

Rogers, Jan R.↗

NASA NTRS1998

An Overview of the Electrostatic Levitation Facility at NASA's Marshall Space Flight Center

Containerless processing represents an important area of research in microgravity materials science. This method provides access to the metastable state of an undercooled melt. Containerless processing provides a high-purity environment for the study of reactive, high-temperature materials. Reduced gravity affords several benefits for containerless processing, for example greatly reduced positioning forces are required and therefore samples of greater mass can be studied. Additionally in reduced gravity, larger specimens will maintain spherical shape which will facilitate modeling efforts. Space Systems/LORAL developed an Electrostatic Containerless Processing System (ESCAPES) as a materials science research tool for investigations of refractory solids and melts. ESCAPES is designed for the investigation of thermophysical properties, phase equilibria, metastable phase formation, undercooling and nucleation, time-temperature- transformation diagrams and other aspects of materials processing. These capabilities are critical to the research programs of several Principal Investigators supported by the Microgravity Materials Science Program of NASA. NASA's Marshall Space Flight Center (MSFC) recently acquired the ESCAPES system from LORAL. MSFC is now developing a levitation facility to provide a critical resource to the microgravity materials science research community to continue and enhance ground-based research in the support of the development of flight experiments during the transition to Space Station.

Rogers, Jan R.↗

NASA NTRS1999

An Overview of the MSFC Electrostatic Levitation Facility

Containerless processing represents an important area of research in microgravity materials science. This method provides access to the metastable state of an undercooled melt. Containerless processing provides a high-purity environment for the study of reactive, high-temperature materials. Reduced gravity affords several benefits for containerless processing, for example greatly reduced positioning forces are required and therefore samples of greater mass can be studied. Additionally in reduced gravity, larger specimens will maintain spherical shape which will facilitate modeling efforts. Space Systems/LORAL developed an Electrostatic Containerless Processing System (ESCAPES) as a materials science research tool for investigations of refractory solids and melts. ESCAPES is designed for the investigation of thermophysical properties, phase equilibria, metastable phase formation, undercooling and nucleation, time-temperature- transformation diagrams and other aspects of materials processing. These capabilities are critical to the research programs of several Principal Investigators supported by the Microgravity Materials Science Program of NASA.

Rogers, J. R.↗

DOE OSTI2020

Kinetic pathways of ionic transport in fast-charging lithium titanate

Fast-charging batteries typically use electrodes capable of accommodating lithium continuously by means of solid-solution transformation because they have few kinetic barriers apart from ionic diffusion. One exception is lithium titanate (Li 4 Ti 5 O 12 ), an anode exhibiting extraordinary rate capability apparently inconsistent with its two-phase reaction and slow Li diffusion in both phases. Through real-time tracking of Li+ migration using operando electron energy-loss spectroscopy, we reveal that facile transport in Li 4+x Ti 5 O 12 is enabled by kinetic pathways comprising distorted Li polyhedra in metastable intermediates along two-phase boundaries. Our work demonstrates that high-rate capability may be enabled by accessing the energy landscape above the ground state, which may have fundamentally different kinetic mechanisms from the ground-state macroscopic phases. This insight should present new opportunities in searching for high-rate electrode materials.

25 ENERGY STORAGE↗

DOE OSTI2026

Formation of Non-Doped Cubic Lithium Lanthanum Zirconium Oxide Nanofibers: Insights from In Situ Synchrotron X-Ray Scattering

This study investigates the formation mechanism of non-doped cubic lithium lanthanum zirconium oxide (c-LLZO) nanofibers using in situ synchrotron X-ray scattering techniques. Electrospun polymer precursor nanofibers were annealed at temperatures up to 800 °C, enabling real-time tracking of phase transitions via simultaneous small-angle X-ray scattering (SAXS), wide-angle X-ray scattering (WAXS), and evolved CO 2 gas analysis. The results reveal a three-step transformation pathway: polymer decomposition, formation of La 2 Zr 2 O 7 (LZO), and direct conversion of LZO to c-LLZO without intermediate tetragonal phases detected within the sensitivity of our in situ WAXS measurement. Cryo-electron energy loss spectroscopy (EELS) further elucidates the role of lithium diffusion, showing Li enrichment at fiber surfaces and Li deficiency in the interior, which stabilizes the cubic phase. This Li segregation effect in nanostructured LLZO materials extends beyond the previously reported size effect. This work advances the understanding of c-LLZO formation mechanisms and provides practical insights for optimizing synthesis routes to achieve phase-pure c-LLZO for solid-state battery applications.

LLZO phase stability↗

NASA NTRS2009

NASA Tech Briefs, November 2009

Topics covered include: Cryogenic Chamber for Servo-Hydraulic Materials Testing; Apparatus Measures Thermal Conductance Through a Thin Sample from Cryogenic to Room Temperature; Rover Attitude and Pointing System Simulation Testbed; Desktop Application Program to Simulate Cargo-Air-Drop Tests; Multimodal Friction Ignition Tester; Small-Bolt Torque-Tension Tester; Integrated Spacesuit Audio System Enhances Speech Quality and Reduces Noise; Hardware Implementation of a Bilateral Subtraction Filter; Simple Optoelectronic Feedback in Microwave Oscillators; Small X-Band Oscillator Antennas; Free-Space Optical Interconnect Employing VCSEL Diodes; Discrete Fourier Transform Analysis in a Complex Vector Space; Miniature Scroll Pumps Fabricated by LIGA; Self-Assembling, Flexible, Pre-Ceramic Composite Preforms; Flight-speed Integral Image Analysis Toolkit; Work Coordination Engine; Multi-Mission Automated Task Invocation Subsystem; Autonomously Calibrating a Quadrupole Mass Spectrometer; Determining Spacecraft Reaction Wheel Friction Parameters; Composite Silica Aerogels Opacified with Titania; Multiplexed Colorimetric Solid-Phase Extraction; Detecting Airborne Mercury by Use of Polymer/Carbon Films; Lattice-Matched Semiconductor Layers on Single Crystalline Sapphire Substrate; Pressure-Energized Seal Rings to Better Withstand Flows; Rollerjaw Rock Crusher; Microwave Sterilization and Depyrogenation System; Quantifying Therapeutic and Diagnostic Efficacy in 2D Microvascular Images; NiF2/NaF:CaF2/Ca Solid-State High-Temperature Battery Cells; Critical Coupling Between Optical Fibers and WGM Resonators; Microwave Temperature Profiler Mounted in a Standard Airborne Research Canister; Alternative Determination of Density of the Titan Atmosphere; Solar Rejection Filter for Large Telescopes; Automated CFD for Generation of Airfoil Performance Tables; Progressive Classification Using Support Vector Machines; Active Learning with Irrelevant Examples; A Data Matrix Method for Improving the Quantification of Element Percentages of SEM/EDX Analysis; Deployable Shroud for the International X-Ray Observatory; Improved Model of a Mercury Ring Damper; Optoelectronic pH Meter: Further Details; X-38 Advanced Sublimator; and Solar Simulator Represents the Mars Surface Solar Environment.

Source record↗

DOE OSTI2025

Mapping causal patterns in crystalline solids

The evolution of the atomic structures of the combinatorial library of Sm-substituted thin film BiFeO 3 along the phase transition boundary from the ferroelectric rhombohedral phase to the non-ferroelectric orthorhombic phase is explored using scanning transmission electron microscopy. Localized properties, including polarization, lattice parameter, and chemical composition, are parameterized from atomic-scale imaging, and their causal relationships are reconstructed using a linear non-Gaussian acyclic model. This approach is further extended to explore the spatial variability of the causal coupling using the sliding window transform method, which revealed that new causal relationships emerged at both the expected locations, such as domain walls and interfaces, and at additional regions forming clusters in the vicinity of the walls or spatially distributed features. While the exact physical origins of these relationships are unclear, they likely represent nanophase-separated regions in the morphotropic phase boundaries. Overall, we posit that an in-depth understanding of complex disordered materials away from thermodynamic equilibrium necessitates understanding not only the generative processes that can lead to observed microscopic states but also the causal links between multiple interacting subsystems.

Causal inference↗

DOE OSTI2021

Shock melting and the hcp-bcc phase boundary of Mg under dynamic loading

The high-temperature and high-pressure response of magnesium has been investigated through shock-release experiments performed up to shock melting. The longitudinal and bulk sound speeds of Mg are reported along the Hugoniot from 25 to 56 GPa and used to determine the elastic properties and Grüneisen parameter. The hexagonal close-packed (hcp)–body-centered cubic (bcc) phase transition is marked by a reduction in the determined shear wave speed. Thermal softening is observed to begin between 40 and 44 GPa, with incipient melt at 55.5 GPa, in close agreement with previous diffraction measurements under laser shock loading. Examination of the release profiles showed that two different responses were observed, depending on the peak stress. When plotted in a stress-energy phase diagram, the two responses are observed to form separate lines that intersect the static hcp-bcc phase transition and incipient melt. The results indicate that the hcp-bcc transition occurs on the Hugoniot at 28.4 GPa and place the hcp-bcc-liquid triple point ~20 GPa. In conclusion, a multiphase equation of state is developed which places the melt boundary below the previously reported static measurements.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Aluminum/SmCo 5 composites for structural and magnetic applications

Metal-bonded magnetic composites (MBMCs) present a promising alternative to dense sintered magnets, particularly for intricate components. Compared to polymer-based bonded magnets, MBMCs have wider applicability in harsh environments. In this paper, we demonstrate a solid-state shear-based manufacturing technique to introduce localized magnetization into a paramagnetic aluminum matrix by embedding SmCo5 permanent magnet particles. Our magnetic composites display hard magnetic behavior with a coercivity of 13 kOe and a remanent magnetization of 4.32 emu/g. In addition to magnetization, we also report a 9% improvement in Young’s modulus. Despite the local temperature rise during processing, the magnetic phases didn’t decompose into unwanted phases, preserving the composite's hard magnetic properties. Creation of an interfacial metallurgical bond with the matrix ensured the suitability of the composites for structural applications. Our study investigates the mechanical, and functional properties of composites, paving the way for lightweight structural magnetic composites with a transformative potential in the aerospace, nuclear, and automotive applications. This work underscores the potential for further optimization and development to drive innovations in magnet and equipment design.

36 MATERIALS SCIENCE↗