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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Atomic structure and formation mechanism of a newly discovered charge density wave in the m = 2 monophosphate tungsten bronze

The m = 2 member of the monophosphate tungsten bronze family had been thought to be the only one without an electronic instability at low temperature. In this paper, we report the discovery of a charge density wave phase in this compound, with a transition temperature of 290 K and an incommensurate modulation vector q = 0.245b* + ξc*, which reaches a lock-in with a commensurate vector at 130 K. The presence of this new phase is confirmed by diffraction and resistivity measurements. Pre-transitional dynamics are investigated using diffuse and inelastic X-ray scattering, revealing a clear Kohn anomaly. We analyze both structural and electronic contributions to the phase transition, providing a comprehensive picture of the mechanism driving this newly identified instability.

Minelli, Arianna [ORNL] (ORCID:0000000283103712)↗
DOE OSTI2026

Effects of Polymer Morphology on Solvent and Catalyst Accessibility during Polyethylene and Polystyrene Autoxidation

Efficient catalytic deconstruction of plastics requires facile solvent and catalyst access to polymer substrates to minimize mass transfer effects. Autoxidation using Co(II) acetate, Mn(II) acetate, and a radical carrier in acetic acid is a promising strategy to deconstruct mixed plastic waste, yet the role of polymer morphology in governing solvent and catalyst accessibility remains poorly understood. Here, in situ simultaneous small- and wide-angle X-ray scattering (SAXS/WAXS), complemented by X-ray fluorescence (XRF) imaging and high-pressure differential scanning calorimetry (DSC), were used to elucidate interactions between acetic acid, a Co/Mn catalyst solution, and semicrystalline polyethylene (PE) and amorphous polystyrene (PS) from room temperature to 160 °C. In PE, acetic acid and catalyst access were confined to amorphous regions and cryomilled particle interfaces at room temperature, while crystalline lamellae remained intact after soaking for up to 34 h. Increasing temperature enabled solvent uptake into PE, followed by solvent-assisted softening above 100 °C, and a modest melting-point depression that removed lamellar transport barriers upon melting. Conversely for PS, acetic acid penetrated the glassy polymer without inducing chain mobility until the glass transition was reached, above which the observed structural changes were consistent with enhanced segmental mobility which enabled bulk penetration. These results suggest that polymer morphology and thermally activated physical transitions arising from diffusion and polymer–solvent interactions can influence whether autoxidation of plastics is transport-limited or kinetically controlled, providing a framework for aligning reaction conditions with reaction outcomes.

09 BIOMASS FUELS↗
DOE OSTI2026

Evaluating multi-slice ptychography tomography for X-ray imaging

X-ray ptychography typically relies on single-slice reconstruction approaches that assume minimal beam propagation through the specimen. However, this approximation breaks down for thick samples or when using high numerical aperture optics, leading to reconstruction artifacts due to multiple scattering. Multi-slice ptychographic tomography (MSPT) addresses this limitation by explicitly modeling beam propagation through the specimen while reducing angular sampling requirements for tomography, but its performance depends critically on reconstruction parameters and experimental conditions. Here, we systematically evaluate MSPT using numerical simulations and experimental X-ray datasets to understand how factors such as object thickness, optical parameters, and initialization strategies affect reconstruction accuracy. We demonstrate that informed object initialization significantly improves depth resolution and enables accurate projection extension, reducing the angular sampling requirements for tomographic reconstruction. Experimental demonstration confirms that MSPT produces reconstructions with reduced artifacts, establishing it as a robust approach for nanoscale imaging at modern synchrotron facilities.

Luktuke, Amey [Argonne National Laboratory (ANL), ↗
DOE OSTI2026

Uncertainty-Aware Machine Learning for Small-Angle X-ray Scattering Analysis in Autonomous Experimentation

Small-angle X-ray scattering (SAXS) is a powerful high-throughput characterization tool for probing nanoscale structure in native sample environments, providing real-time morphological information such as nanoparticle size and shape during synthesis. However, automated SAXS data analysis for extracting meaningful structural parameters is non-trivial and remains a bottleneck in closed-loop experimentation towards autonomous materials discovery, which demands fast, reliable, and uncertainty-aware data analysis. Here, we develop a machine-learning approach for automated SAXS analysis tailored to closed-loop nanoparticle synthesis. A Random Forest (RF) regression model is trained on 100,000 synthetic SAXS curves generated from polydisperse spherical nanoparticles with realistic background contributions. Using normalized one-dimensional SAXS intensity profiles as input, the RF model directly predicts nanoparticle radius, size polydispersity, and background parameters, while the ensemble standard deviation across trees provides built-in uncertainty quantification (UQ). On synthetic data, we show that combining fit-quality metrics (R 2 , MAE) with thresholds on prediction uncertainty reliably identifies accurate parameter estimates without access to ground truth. We then apply the trained model to 365 experimental SAXS profiles of citrate-reduced gold nanoparticles synthesized using an automated droplet-flow microreactor with in situ SAXS at a synchrotron beamline, classifying the results into high- and low-confidence subsets based on UQ metrics. Finally, we integrate RF-based SAXS analysis into a simulated closed-loop optimization campaign using Gaussian process Bayesian optimization to minimize nanoparticle polydispersity, benchmarking against conventional automated Levenberg–Marquardt fitting. The RF-guided campaign exhibits substantially faster convergence and lower relative opportunity cost (∼0.07 vs ∼0.3), demonstrating that uncertainty-aware machine-learning SAXS analysis significantly enhances the efficiency and robustness of autonomous nanomaterials synthesis workflows.

Bayesian optimization↗
DOE OSTI2026

A Review of Advanced Characterization Methods and Techniques for Amorphous and Poorly Crystalline Materials Applicable to Cementitious Waste Forms

This review covers advanced characterization methods of cementitious materials. The particular focus is to understand cementitious compositions with amorphous content because conventional techniques such as X-ray diffraction are more applicable to materials with long range order. Also of interest is advanced characterization that provides deeper insights into properties such as porosity. There are five groups of characterization methods discussed in this review which are: electron beam/microscopy, X-ray, neutron diffraction and scattering, nuclear magnetic resonance, and optical techniques. The techniques can be further grouped by the categories of nanoscale structural understanding (transmission electron microscopy and pair distribution function), microscale structural understanding (focused ion beam and x-ray tomography), microscopic elemental distributions (energy dispersive spectroscopy and X-ray fluorescence), and chemical binding information (electron energy loss spectroscopy, x-ray absorption spectroscopy, nuclear magnetic resonance, Raman spectroscopy, and infrared spectroscopy), with advantages and disadvantages of each method discussed. The recommendation for further research is to begin with techniques that are easier to prepare samples for, measure, and analyze, such as the optical techniques of Raman and infrared spectroscopy. If more information is needed, pursue collaborations, other techniques, or proposals for beam time at the synchrotron sources.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2026

Few-femtosecond time resolution in optically pumped hard X-ray scattering at a free-electron laser

Capturing chemical dynamics in real time is a central goal of ultrafast science, necessitating measurements fast enough to track atomic motion on few-femtosecond timescales with high precision. We present time-resolved hard X-ray scattering that meets these criteria by combining 7 fs full-width at half maximum (FWHM) near-infrared laser pulses with sub10 fs FWHM hard X-ray pulses from a free-electron laser. Using heavy water’s electronic response to strong-field ionization as a benchmark, we achieve a sub-8 fs FWHM instrument response function. These optical pump X-ray probe measurements enable direct observation of chemical dynamics with angstrom spatial and few-fs temporal resolution.

Weckwerth, Eleanor [Stanford University, CA (Unite↗
DOE OSTI2026

Superconductivity Reinforces Charge-Density-Wave Phase Coherence across Cuprates

For decades, superconductivity in high-𝑇 c cuprates has been viewed as a competitor that suppresses charge-density-wave (CDW) order by reducing its amplitude and spatial extent. Here, in this study, we show that this picture is incomplete, as superconductivity is accompanied by a systematic enhancement of CDW phase coherence across multiple cuprate families. Using resonant soft x-ray scattering combined with a coherence-sensitive momentum-profile analysis, we uncover a BCS-like growth of phase coherence below 𝑇 c , which phenomenologically manifests as the absence of CDW peak broadening and near-perfect wave-vector locking. This enhancement remains visible even in a disorder-dominated regime created by long-term crystal aging and follows a common trend when compared with published data on Bi-, Hg-, Y-, and Nd-based cuprates. These results indicate that superconductivity reshapes CDW order in two distinct ways, suppressing its amplitude while strengthening its phase coherence, and reveal an additional phase-level interplay with lattice coupling in high-𝑇 c cuprates.

Lee, H. [SLAC National Accelerator Laboratory (SLA↗
DOE OSTI2026

Deciphering the Solvation Structure of Aqueous ZnCl 2 Solutions from X-ray Absorption Spectra Using the Interpretable Graph Neural Network

Machine learning (ML) provides powerful pathways for predicting spectroscopic observables from atomic structures, but its broader impact depends on making model predictions interpretable in terms of physical and chemical principles. Here, we introduce a physics-guided graph neural network (GNN) model that predicts Zn K-edge X-ray spectroscopy (XAS) spectra of aqueous ZnCl 2 solutions. Training data are generated from ab initio XAS calculations on molecular dynamics snapshots obtained using a machine learning interatomic potential. The GNN reproduces experimental spectra across concentrations from dilute (<0.1 m) to highly concentrated (30 m, “water-in-salt”) regimes and scales efficiently to large, disordered liquid systems beyond the reach of conventional ab initio approaches. Gradient-based attribution analysis reveals that the model learns physically meaningful structure-spectrum relationships. Ligand-specific attributions reflect orbital hybridization patterns and the origin of the excitations derived from the density functional theory. Bond-length attributions recover spectral shifts consistent with multiple-scattering theory. Finally, this work bridges data-driven prediction with electronic-structure theory, establishing a general paradigm for interpretable ML that links atomic structure, electronic structure, and spectroscopic observables.

25 ENERGY STORAGE↗
DOE OSTI2026

Task Sharing of Proton Incorporation in Vertically Aligned Nanocomposite Triple Conductors: Growth, Structure, and Surface Exchange Kinetics

As protonic ceramic electrolysis cells emerge for efficient H 2 production, there is a need to develop air electrode materials enabling fast, durable steam splitting and proton incorporation. Single-phase triple conductors may fail to satisfy the myriad performance/stability requirements, and their critical charge-carriers (holes, oxygen vacancies, and protons) are in competition, limiting their concentrations. Instead, we propose task-sharing, vertically aligned nanocomposites (VANs), comprising a proton conductor (BaZr 0.9 Y 0.1 O 3-δ ) and a redox-active mixed ionic electronic conductor (Ce 0.9 Pr 0.1 O 2-δ ), that may enable rapid proton surface exchange at the solid–gas interface and transport along the solid–solid heterointerfaces. We grew VANs by pulsed laser deposition and investigated the interplay between their processing conditions, structure, and proton and oxygen surface exchange kinetics. We varied the substrate temperature, laser repetition rate, laser fluence, and processing oxygen pressure. The crystallinity and phases were characterized by grazing-incidence X-ray diffraction, and the strain and structural order as a function of depth were evaluated by angle-dependent synchrotron X-ray pair distribution function analysis. To evaluate the potential for interdiffusion, the formation energies of substitutional defects were simulated with density functional theory. Corresponding structural analysis and elemental mapping were performed by scanning/transmission electron microscopy, energy-dispersive X-ray spectroscopy, and electron energy-loss spectroscopy, indicating distinct nanoscale compositional regions with a hierarchical structure embedded in individual VANs columns and minimal interdiffusion across a bilayer film. Proton and oxygen surface exchange coefficients (k H , k O ) and polarization resistances were evaluated by electrical and optical relaxations and impedance spectroscopy of VAN-incorporated protonic ceramic electrochemical cells, respectively, at 400–500 °C, demonstrating values comparable to some of the best-known triple and mixed conductors.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Magnetic structure of topological nodal-line semimetal EuSb 2

Here, we investigated the magnetic structure of the magnetic topological nodal-line semimetal EuSb 2 using x-ray resonant magnetic scattering at the Eu 𝐿 3 absorption edge. Forbidden magnetic reflections confirm antiferromagnetic ordering with propagation vector 𝐪 = (0.5,0,0) below 𝑇 N ≈ 27 K. Azimuthal-angle-dependent measurements reveal that the Eu moments are aligned along the monoclinic 𝑏 axis. Comparison between the measured 𝐐-dependent magnetic Bragg peak intensities and calculations based on representation analysis identifies the magnetic structure as the A-type antiferromagnetic 𝛤 4 representation with a (++−−) arrangement along the 𝑎 direction. These results establish the microscopic magnetic structure of EuSb 2 and provide a basis for understanding the interplay between antiferromagnetism and topological electronic states in this system.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Excitations across the Equilibrium and Photoinduced “Hidden” States of Magnetoresistive Manganites

“Hidden” phases, generated using ultrafast laser pulses (few hundred femtoseconds), with distinct properties than at the thermodynamic equilibrium, are appealing for technologies, as they can be long-lived, with a lifetime of hours or weeks, and reversible with temperature sweeping or extra pulses. In this regard, La 2/3 ⁢Ca 1/3⁢ MnO 3 (LCMO) stands out due to its tunability through epitaxial strain, which can drive the bulk ferromagnetic metal into an antiferromagnetic insulator (AFI), and its susceptibility to photoinduced transitions. Indeed, AFI LCMO displays a long-lived photoinduced transition into a putative hidden phase whose exact nature and excitations are still largely unknown. Here, we combine ultrafast photoexcitation in the near infrared with in situ transport, x-ray absorption, and resonant inelastic x-ray scattering (RIXS) to investigate the excitations (polarons, phonons, and orbital) of the photoexcited phase of LCMO and contrast them with the thermodynamic phases achieved through strain and temperature. In the thermodynamic regime, we establish the correlation between polarons and transport placing them in the “strong coupling” regime of the Holstein model. Upon photoexcitation of LCMO-AFI, we uncover a long-lived phase characterized by the softening of the polaron excitations, the partial suppression of the Jahn-Teller distortion, and nearly unchanged phonons, showing the emergence of a photoexcited state absent in the equilibrium phase diagram. Finally, by varying temperature, epitaxial strain, and photoexcitation fluence, we construct a polaron phase diagram and identify the key spectroscopic signatures of each phase. Our laser-RIXS approach establishes a versatile platform for exploring photoinduced hidden phases in quantum materials in nonstroboscopic conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Ion Transport and Crystal Rotation in Plastic Crystal Electrolytes Under Applied Electric Fields

Organic ionic plastic crystal electrolytes, containing a plastic crystal and lithium salt, offer a potential balance between mechanical and electrochemical properties for solid state lithium-ion battery electrolytes. These electrolytes contain multiple mobile ionic species (three or four), resulting in complex transport mechanisms which have not yet been established. Plastic crystals are defined by long-range positional order and short-range rotational disorder. It is therefore necessary to quantify changes in the local crystal structure of the electrolyte as current flows through it. Herein, we examine the electrochemical properties of pyrrolidinium-based plastic crystal electrolytes containing lithium salt and zwitterion additives, including measurements of current fraction and limiting current. We obtain species-specific insight into electrolyte transport using pulsed-field gradient nuclear magnetic resonance spectroscopy and find that, while the zwitterion additive increases ionic conductivity, it decreases lithium diffusivity with respect to other ionic components. With operando spatiotemporally resolved wide-angle X-ray scattering we observe location-specific crystal rotations due to the passage of ionic current. In conclusion, we posit that reducing energy dissipation due to rotation is essential for using plastic crystal electrolytes in practical applications.

Yap, Kyra M. K. [University of California, Berkele↗
DOE OSTI2026

Cooperative Charge Ordering Signature of Trimer Molecules in Infinite-Layer CaCoO 2

The infinite-layer compound CaCoO 2 provides a compelling platform to explore how local orbital distortions evolve into collective electronic order. Using resonant soft x-ray scattering (RSXS) and its time-resolved counterpart (tr-RSXS), we reveal a cooperative coupling between two intertwined orders at the same in-plane wave vector, 𝑞 ≈ (1/4, 1/4, 0), comprising a quasi-two-dimensional orbital order associated with the distorted Co (1) sites and a quasi-three-dimensional trimerlike charge order stabilized through Co-O-Ca hybridization. The charge-sensitive component exhibits a uniform relaxation time of ∼400 fs (391 ± 5 fs) across multiple Co resonances, evidencing a collective charge response. A comparable timescale observed in the orbital order associated with the highly distorted Co (1) sites indicates that this collective behavior naturally originates from the same orbital framework that mediates both charge and orbital degrees of freedom. Together, these findings establish CaCoO 2 as a model system in which Jahn-Teller distortions, orbital hybridization, and geometric frustration cooperate to form molecular trimer units that dictate the macroscopic electronic behavior.

Lee, J.-S. [SLAC National Accelerator Laboratory (↗
DOE OSTI2026

Oligoether-Functionalized PEDOT: Combining an EDOT Backbone with Polar Side Chains for Solution Processability and High Electrical Conductivity

Conjugated polymers functionalized with oligoether (OE)-based side chains are a key class of materials for various organic electronic applications, including transparent electrodes, thermoelectrics, electrochromic displays, and electrochemical transistors. Herein, we report a highly soluble OE-functionalized poly(3,4-ethylenedioxythiophene) (PEDOT) homopolymer, prepared by direct (hetero)arylation polymerization, which allows solution processing to yield films with comparable redox properties to oxidatively polymerized PEDOT. This polymer, PEDOT(OE3), when optimally oxidatively doped, reaches among the highest electrical conductivities of any OE-functionalized polymer and is comparable to more synthetically complex OE-functionalized polymers. X-ray scattering and spectroscopy were utilized to rationalize the transport properties resulting from varying the doping level. Comparison of PEDOT(OE3) to a series of OE-functionalized dioxythiophenes with varying amounts of 3,4-ethylenedioxythiophene units allows for a deeper understanding of structure–property relationships through charge-transport models. Ultimately, PEDOT(OE3) is shown to be a material with exceptional charge-transport properties and is promising for various applications.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Long-range magnetic order with disordered spin orientations in a high-entropy antiferromagnet

Disorder in magnetic systems typically suppresses long-range order, promoting short-range states such as spin glasses and magnetic clusters. This is particularly prominent in high-entropy materials, characterized by the random distributions of local magnetic entities and exchange interactions. However, in rare exceptions, long-range magnetic order can persist in high-entropy systems, while the microscopic characters and underlying mechanisms remain elusive, especially the magnetic behaviors of individual elements. Here, combining neutron diffraction and resonant soft x-ray scattering, we have conducted an element-specific investigation into the magnetic order of a high-entropy honeycomb-lattice van der Waals material (Mn 1/4 Fe 1/4 Co 1/4 Ni 1/4 )PS 3 . Despite significant atomic disorder, long-range zigzag antiferromagnetic order is observed below 72 K, with all four transition-metal elements participating in a unified phase transition. However, the spin orientations of various elements are distinct, attributed to the competition between single-ion anisotropies and exchange interactions. Our findings showcase a novel form of long-range magnetic order with disordered spin orientations, which is synergically stabilized by distinct magnetic elements in a high entropy magnet, offering a new paradigm for understanding complex magnetic systems.

Shen, Yao [Chinese Academy of Sciences (CAS), Beij↗
DOE OSTI2026

Charge correlations and magnetoelastic coupling in intercalated transition metal dichalcogenides

The large van der Waals gap in transition metal dichalcogenides (TMDs) offers an avenue to tune the ground state of 2D materials through the intercalation of magnetic atoms. Here, we investigate the charge correlations in Fe 1/3 ⁢TaS 2 , Co 1/3 ⁢TaS 2 , and Fe 0.35 ⁢NbS 2 by combining angle-resolved photoemission spectroscopy (ARPES), x-ray scattering, magnetometry, and density functional theory (DFT). We find that, while short-range charge fluctuations develop in Ta-based compounds, Fe 0.35 ⁢NbS 2 exhibits long-range charge order which is strongly coupled with magnetic order and tunable by external magnetic field. Our electronic structure analysis reveals that intercalation reconstructs the Fermi surface via charge transfer and band renormalization, yet does not generate the nesting conditions compatible with the observed ordering vectors. Complementary phonon calculations further exclude a conventional electron-phonon origin of charge order. Together, these results establish magnetoelastic coupling as the dominant mechanism behind charge ordering in Fe 0.35 ⁢NbS 2 and highlight the contrasting role of Nb and Ta hosts in stabilizing correlated ground states in intercalated TMDs.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Formation of Bimetallic Nanoparticles via Exsolution Using a Reducible Metal Oxide Capping Layer

Bimetallic nanoparticles are promising catalysts that can improve performance in heterogeneous catalysis and solid-state electrochemistry. Exsolution is a useful method for forming such nanoparticles; however, it is limited by the elements present within the host oxide lattice. Here, in this work, we develop and demonstrate a strategy to form bimetallic particles from La 0.5 Sr 0.5 Ti 0.94 Ni 0.06 O 3 (LSTN) exsolution and using a reducible SnO 2 capping layer, expanding the range of elements available for bimetallic nanoparticle formation. Using this capping layer strategy, we formed nickel–tin (Ni 0 –Sn 0 ) bimetallic nanoparticles via exsolution. We used in situ near-ambient pressure X-ray photoelectron spectroscopy to monitor surface chemical changes during exsolution, showing that first, SnO 2 volatilized. This SnO 2 loss exposed the perovskite surface of LSTN to reducing conditions, which induced Ni exsolution, and compounded with SnO 2 reduction led to the formation of bimetallic Ni 0 –Sn 0 particles. To evaluate the associated microstructural evolution, we measured grazing incidence small-angle X-ray scattering (GISAXS), which confirmed the loss of the SnO 2 capping layer, and scattering simulations suggested the formation of bimetallic particles. We confirmed the bimetallic nanoparticle composition and morphology by Auger spectroscopy and scanning transmission electron microscopy. The resulting bimetallic nanoparticles were smaller and more thermally stable than the monometallic Ni counterparts on LSTN. This capping layer and exsolution approach allow synthesizing multimetallic nanoparticles and can be applied to other reducible metal oxides and perovskite hosts, broadening the compositional space for advanced catalytic materials.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Dynamic nanodomains dictate macroscopic properties in lead halide perovskites

Lead halide perovskites have emerged as promising materials for solar energy conversion and X-ray detection owing to their remarkable optoelectronic properties. However, the microscopic origins of their superior performance remain unclear. Here we show that low-symmetry dynamic nanodomains present in the high-symmetry average cubic phases, whose characteristics are dictated by the A-site cation, govern the macroscopic behaviour. We combine X-ray diffuse scattering, inelastic neutron spectroscopy, hyperspectral photoluminescence microscopy and machine-learning-assisted molecular dynamics simulations to directly correlate local nanoscale dynamics with macroscopic optoelectronic response. Our approach reveals that methylammonium-based perovskites form densely packed, anisotropic dynamic nanodomains with out-of-phase octahedral tilting, whereas formamidinium-based systems develop sparse, isotropic, spherical nanodomains with in-phase tilting, even when crystallography reveals cubic symmetry on average. We demonstrate that these sparsely distributed isotropic nanodomains present in formamidinium-based systems reduce electronic dynamic disorder, resulting in a beneficial optoelectronic response, thereby enhancing the performance of formamidinium-based lead halide perovskite devices. By elucidating the influence of the A-site cation on local dynamic nanodomains, and consequently, on the macroscopic properties, we propose leveraging this relationship to engineer the optoelectronic response of these materials, propelling further advancements in perovskite-based photovoltaics, optoelectronics and X-ray imaging.

Materials Science↗