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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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32 records · Page 2

Correlation-aware binning for small-angle neutron scattering via Gaussian-process inference

Binning in small-angle neutron scattering (SANS) is typically performed empirically, with fixed parameters chosen for convenience rather than statistical optimality. Such practices often fail to balance statistical precision and spatial resolution, leading to inconsistencies across instruments and datasets. Here we establish a correlation-aware framework that determines the optimal bin width from first principles by extending the classical Freedman–Diaconis (FD) rule to account for inter-bin correlations with a Gaussian process. In this formulation, the scattering intensity is treated as a smooth stochastic field whose statistical coherence is described by a covariance matrix. Analytical expressions of errors derived from this model yield closed-form criteria that separate the total deviation into contributions from counting noise, aliasing distortion and curvature-dependent correlation effects. Expressed in reduced variables, the resulting dimensionless error surface reveals a continuous transition from the uncorrelated FD regime to the correlation-dominated limit, providing a unified description of noise suppression and resolution control. Because the formulation depends only on the profile characteristics of scattering intensity I(Q), specifically its average intensity and first- and second-order derivatives, it applies generally to any SANS measurement regardless of sample, instrument or geometry. Experimental validation using small- and ultra-small-angle neutron scattering data confirms the predicted scaling behavior, demonstrating that correlation-aware inference systematically reduces mean-squared error and enables information-efficient reproducible data reduction across materials and instruments.

Tung, Chi-Huan [ORNL] (ORCID:0000000221972074)↗

Comparison of nanocomposite dispersion and distribution for several melt mixers

Breakup (dispersion) and distribution of nanoparticles are the chief hurdles towards taking advantage of nanoparticles in polymer nanocomposites for reinforcement, flame retardancy, conductivity, chromaticity, and other properties. Microscopy is often used to quantify mixing, but it has a limited field of view, does not average over bulk samples, and fails to address nano-particle hierarchical structures. Ultra-small-angle X-ray scattering (USAXS) can provide a macroscopic statistical average of nanoscale dispersion (breakup) and emergent hierarchical structure, as well as the distribution on the nanoscale. Here, this work compares several common mixer geometries for carbon black-polystyrene nanocomposites. Two twin-screw extruder geometries, typical for industrial processing of melt blends, are compared with a laboratory-scale single screw extruder and a Banbury mixer. It is found that for a given mixer, nanoscale distribution increases following a van der Waals function using accumulated strain as an analogue for temperature while macroscopic distribution/dispersion, using microscopy, does not follow this dependency. Breakup and aggregation in dispersive mixing follow expected behavior on the nanoscale. Across these drastically different mixing geometries an unexpected dependency is observed for nanoscale distributive mixing (both nano and macroscopic) as a function of accumulated strain that may reflect a transition from distributive turbulent to dispersive laminar mixing as the mixing gap is reduced.

36 MATERIALS SCIENCE↗

(U)SAXS characterization of porous microstructure of chert: insights into organic matter preservation

This study characterizes the microstructure and mineralogy of 132 (ODP sample), 1000 and 1880 million-year-old chert samples. By using ultra-small-angle X-ray scattering (USAXS), wide-angle X-ray scattering and other techniques, the preservation of organic matter (OM) in these samples is studied. The scarce microstructural data reported on chert contrast with many studies addressing porosity evolution in other sedimentary rocks. The aim of this work is to solve the distribution of OM and silica in chert by characterizing samples before and after combustion to pinpoint the OM distribution inside the porous silica matrix. The samples are predominantly composed of alpha quartz and show increasing crystallite sizes up to 33 ± 5 nm (1σ standard deviation or SD). In older samples, low water abundances (~0.03%) suggest progressive dehydration. (U)SAXS data reveal a porous matrix that evolves over geological time, including, from younger to older samples, (1) a decreasing pore volume down to 1%, (2) greater pore sizes hosting OM, (3) decreasing specific surface area values from younger (9.3 ± 0.1 m 2 g -1 ) to older samples (0.63 ± 0.07 m 2 g -1 , 1σ SD) and (4) a lower background intensity correlated to decreasing hydrogen abundances. The pore-volume distributions (PVDs) show that pores ranging from 4 to 100 nm accumulate the greater volume fraction of OM. Raman data show aromatic organic clusters up to 20 nm in older samples. Raman and PVD data suggest that OM is located mostly in mesopores. Observed structural changes, silica–OM interactions and the hydro­phobicity of the OM could explain the OM preservation in chert.

(U)SAXS↗

Pressure-Thresholded Response in Cylindrically Shocked Cyclotrimethylene Trinitramine (RDX)

We demonstrate a strongly thresholded response in cyclotrimethylene trinitramine (RDX) when it is cylindrically shocked using a novel waveguide geometry. Using ultrafast single-shot multi-frame imaging, we demonstrate that <100 μm diameter single crystals of RDX embedded in a polymer host deform along preferential planes for >100 ns after the shock first arrives in the crystal. We use in situ imaging and time-resolved photoemission to demonstrate that short-lived chemistry occurs with complex deformation pathways. Using scanning electron microscopy and ultra-small-angle X-ray scattering, we demonstrate that the shock-induced dynamics leave behind porous crystals, with pore shapes and sizes that change significantly with shock pressure. A threshold pressure of ~12 GPa at the center of convergence separated the single-mode planar crystal deformations from the chemistry-coupled multi-plane dynamics at higher pressures. Our observations indicate preferential directions for deformation in our cylindrically shocked system, despite the applied stress along many different crystallographic planes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

In Situ Structural and Electrical Conductivity Characterization of Sr2MMoO6-δ Double Perovskite Solid Oxide Fuel Cell Anode Materials

In this study, a series of Sr 2 MMoO 6-δ double perovskite solid oxide fuel cell (SOFC) anode materials (where 0 <= δ <= 0.041 and M = Fe, Co, or Ni) were synthesized, and the changes in their morphologies under relevant SOFC operating conditions were explored. Ultra-small-angle X-ray scattering (USAXS), small-angle X-ray scattering (SAXS), and wide-angle X-ray scattering (WAXS) were used to determine changes in the microstructures and phase compositions of the anode materials at high temperatures and under a reducing atmosphere. The stability of the double perovskite structure was found to be highly dependent on the identity of the cation M, such that when M = Fe, the material remained stable over the course of the experiments. However, when M = Co or Ni, significant changes in the microstructure and phase composition were observed. An in situ study of the M = Co sample, in which electrical conductivity and USAXS/SAXS/WAXS measurements were conducted simultaneously, revealed the structural degradation mechanisms and electrical conductivity changes over a range of temperatures. To conduct these measurements, a cell was developed that allowed for a sample mounted on Pt wires to be placed in the X-ray beam and heated under gas flow comprising 4% mass H 2 and 96% mass N 2 . The resulting measurements allowed for the direct comparison of the electrical and morphological changes occurring in the material under operating conditions, such that increases in conductivity could be attributed to the growth of new phases.

25 ENERGY STORAGE↗

Influence of Silane Coupling Agents on Filler Network Structure and Stress-Induced Particle Rearrangement in Elastomer Nanocomposites

Filled rubber materials are key in many technologies having broad impact on the economy and sustainability, the most obvious being tire technology. Adding filler dramatically improves the strength of rubber by reinforcement and tailoring the type of filler and the chemistry of the interface between filler and rubber matrix is important for optimizing performance metrics such as fuel efficiency. In a highly loaded, silica-filled, crosslinked model rubber closely mimicking commercial materials, both the filler network structure and the dynamics of the silica filler particles change when the silica surface is modified with silane coupling agents. Reduction in size scales characteristic of the structure are quantified using ultra-small-angle X-ray scattering (USAXS) measurements and the particle dynamics probed with X-ray photon correlation spectroscopy (XPCS). While the structure averaged over the scattering volume changes little with aging after step strain, the dynamics slow appreciably in a manner that varies with the treatment of the silica filler. The evolution of filler particle dynamics depends on the chemical functionality at the silica surface and observing these differences suggests a way of thinking about the origins of hysteresis in nanoparticle-reinforced rubbers. These microscopic filler dynamics are correlated with the macroscopic stress relaxation of the filled materials. The combination of static and dynamic X-ray scattering techniques with rheological measurements is a powerful approach for elucidating the microscopic mechanisms of rubber reinforcement.

36 MATERIALS SCIENCE↗

Probing Clustering Dynamics between Silicon and PAA or LiPAA Slurries under Processing Conditions

This work explores the complex interplay between slurry aggregation, agglomeration, and conformation (i.e., shape) of poly(acrylic acid) (PAA)- and lithiated PAA-based silicon slurries as a function of the shear rate and the resulting slurry homogeneity. These values were measured by small-angle neutron scattering (SANS) and rheology-coupled ultra-SANS at conditions relevant to battery electrode casting. Different binder solution preparation methods, either a ball milling (BM) process or a planetary centrifugal mixing (PCM) process, dramatically modify the resulting polymer dynamics and organization around a silicon material. This is due to the different energy profiles of mixing where the more violent and higher energy PCM causes extensive breakdown and reformation of the binder, which is now likely in a branched conformation, while the lower energy BM results in simply lower-molecular weight linear polymers. In conclusion, the breakdown and reorganization of the polymer structure affect silicon slurry homogeneity, which affects subsequent electrode architecture.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Unraveling the core of fuel cell performance: engineering the ionomer/catalyst interface

The biggest obstacle to the widespread implementation of polymer electrolyte membrane fuel cells (PEMFCs) is their cost, primarily due to the use of platinum catalysts. The high intrinsic catalyst activity exhibited on a rotating disk electrode (RDE) is rarely realized in a membrane electrode assembly (MEA), which is a long-standing challenge for PEMFCs and a cause of low catalyst utilization. To translate the high RDE performance of a catalyst into a MEA, the design of an ideal ionomer/catalyst interface is proposed: a thin, conformal ionomer film covers the maximum surface of a Pt nanoparticle and thus simultaneously maximizes catalyst utilization, (i.e., high mass activity and electrochemically active surface area) and O 2 diffusion rate (i.e., high current density performance) without compromising proton conduction. Building such an interface is a long-standing challenge due to the lack of interaction between the ionomer and catalyst particles, resulting in large ionomer agglomerates and inhomogeneous ionomer coverage over the catalyst nanoparticle, with consequent poor fuel cell performance. In this work, this ionomer/catalyst interface has been engineered, utilizing the electrostatic attraction between positively charged catalyst and negatively charged ionomer particles in a catalyst ink and preserved in a solid catalyst layer. As a result, this interface leads to previously unachieved proton exchange membrane fuel cell performance in terms of both catalyst utilization (75% vs. 45%) and peak/rated power density (i.e., 1.430/0.930 W cm -2 , H 2 /air, cathode Pt loading: 0.1 mgPt cm -2 ) for pure Pt catalysts, even better than those of Pt alloy catalysts. This work demonstrates the formation of an interface in the liquid phase (using ultra-small-angle X-ray scattering in combination with cryo-TEM, isothermal–titration–calorimetry) and the preservation of the interface in the solid catalyst layer (using TEM) and estimates the effective coverage and thickness of the ionomer film (using limiting current density, RDE and fuel cell performance).

25 ENERGY STORAGE↗

Microstructural investigation of PBX 9501: Comparing wet slurry and resonant acoustic mixing techniques

The microstructure of a high explosive (HE) material directly influences the reactive behavior under a variety of insults. Furthermore, the preparation method of polymer-bonded explosives (PBX), as well as the constituent material particle size distribution and consolidation parameters, will dominate the microstructural features that are observed. Here, we compare batches of PBX 9501 prepared by the typical wet slurry process and those prepared by resonant acoustic mixing. The “prills” produced by the wet slurry process leads to an inherently different microstructure than the coated powder produced by resonant acoustic mixing. Additionally, we observed that the conditions required to consolidate (press) the material to the nominal PBX 9501 density varied depending on the preparation technique, which also dictates the observed binder distribution. Furthermore, X-ray microcomputed tomography and ultra-small-angle X-ray scattering analyses revealed distinct differences in the void structure and distribution.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

X-Ray Characterization of Real Fuel Sprays for Gasoline Direct Injection

Here, the effects of fuel blend properties on spray and injector performance has been investigated in a side-mount injector for gasoline direct injection (GDI) using two certification fuel blends: Euro 5 and Euro 6. Several X-ray diagnostic techniques were conducted to characterize the injector and spray morphology. Detailed internal geometry of the GDI injector was resolved to 1.8 μm, through the use of hard X-ray tomography. The geometry characterization of this six-hole GDI, side mount injector, quantifies relevant hole and counterbore dimensions and reveals the intricate details within the flow passages, including surface roughness and micron-sized features. Internal valve motion was measured with a temporal resolution of 20 μs and a spatial resolution of 2.0 μs, for three injection pressures and several injector energizing strategies. The needle motion for both fuels exhibits similar lift profiles for common energizing commands. A combination of X-ray radiography and ultra-small-angle X-ray scattering (USAXS) was used to characterize the fuel mass distribution and the droplet sizing, respectively. Tomographic spray radiography revealed the near-nozzle distribution of fuel mass for each of the fuels and the asymmetry produced by the angled nozzles. Under evaporative conditions, the two fuels show minor differences in peak fuel mass distribution during steady injection, though both exhibit fluctuations in injection during the early, transient phase. USAXS measurements of the path-specific surface area of the spray indicated lower peak values for the more evaporative conditions in the near nozzle region.

09 BIOMASS FUELS↗

Super-swelling behavior of stacked lipid bilayer systems

Bilayer systems comprising lipid mixtures are the most well-studied model of biological membranes. While the plasma membrane of the cell is a single bilayer, many intra- and extra-cellular biomembranes comprise stacks of bilayers. Most bilayer stacks in nature are periodic, maintaining a precise water layer separation between bilayers. That equilibrium water separation is governed by multiple inter-bilayer forces and is highly responsive. Biomembranes re-configure inter-bilayer spacing in response to temperature, composition, or mass transport cues. In synthetic bilayer systems for applications in cosmetics or topical treatments, control of the hydration level is a critical design handle. Herein we investigate a binary lipid system that leverages key inter-bilayer forces leading to unprecedented levels of aqueous swelling while maintaining a coherent multilamellar form. We found that combining cationic lipids with bicontinuous cubic phase-forming lipids (lipids with positive Gaussian modulus), results in the stabilization of multilamellar phases against repulsive steric forces that typically lead to bilayer delamination at high degrees of swelling. Using ultra-small-angle X-ray scattering alongside confocal laser scanning microscopy, we characterized various super-swelled states of 1,2-dioleoyl-3-trimethylammonium-propane (DOTAP) and glycerol monooleate (GMO) lipids, as well as other analogous systems, at varied concentration and molar ratios. Through these experiments we established swelling profiles of various binary lipid systems that were near-linear with decreasing lipid volume fraction, showing maximum swelling with periodicity well above 200 nanometers.

42 ENGINEERING↗

Synthesis and Characterization of Mesoporous Silica Nanoparticles Loaded with Pt Catalysts

Coating the catalyst with a nanoporous layer has been demonstrated to be an effective approach to improve catalyst stability. Herein, we systematically investigate two types of core-shell mesoporous silica nanoparticles with a platinum nanocatalyst using a variety of characterization methods. One of the mesoporous particles has a unique amine ring structure in the middle of a shell (Ring-mSiO 2 /Pt-5.0/SiO 2 ), and the other one has no ring structure (mSiO 2 /Pt-5.0/SiO 2 ). Brunauer–Emmett–Teller/Barrett–Joyner–Halenda (BET/BJH) presented a similar surface area for both particles, and the pore size was 2.4 nm. Ultra-Small-Angle X-ray Scattering (USAXS)/ Small-Angle X-ray Scattering (SAXS) showed the size of mSiO 2 /Pt-5.0/SiO 2 and Ring-mSiO 2 /Pt-5.0/SiO 2 were 420 nm and 272 nm, respectively. It also showed that the ring structure was 30 nm above the silica core. Using high-resolution Transmission Electron Microscopy (TEM), it was found that the platinum nanoparticles are loaded evenly on the surface of the silica. In situ SAXS heating experiments and Thermogravimetric Analysis (TGA) indicated that the mSiO 2 /Pt-5.0/SiO 2 were more stable during the high temperature, while the Ring-mSiO 2 /Pt-5.0/SiO 2 had more change in the particle.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Pair distribution function analysis of nano-object assemblies

The atomic pair distribution function (aPDF) analysis technique, also known as the total scattering method, which considers both Bragg and diffuse scattering, has been used extensively to probe local atomic arrangements in crystalline and disordered materials. In contrast, there have been limited applications of the PDF in self-assembled nanomaterials, which represent a class of materials built from nanoscale objects, such as nano-colloids, micelles and proteins. As distinguished from atoms, nano-objects have polydispersity in size and shape, and such form-factor effects complicate the application of PDF analysis to nano-systems. Here, in this paper, the application of the PDF is extended to spherical nano-object assemblies and the formulae for the nano-PDF (nPDF) are derived, showing some differences from the aPDF. By numerical simulations, the properties of the nPDF (peak broadening and pattern profile) are studied systematically as a function of structural features, such as nano-object parameters (size and size polydispersity) and assembly structural features (size, shape, structure type and lattice disorder), and of data processing parameters ( q cut-off and `missing' data in ultra-small-angle regions). The nPDF analysis method is found to provide an effective route to revealing not only nanoscale but also mesoscale structural properties, for example the morphology of a nano-assembly.

77 NANOSCIENCE AND NANOTECHNOLOGY↗