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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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At least 73 records · Page 4

Imaging analysis of LDEF craters

Two small craters in Al from the Long Duration Exposure Facility (LDEF) experiment tray A11E00F (no. 74, 119 micron diameter and no. 31, 158 micron diameter) were analyzed using Auger electron spectroscopy (AES), time-of-flight secondary ion mass spectroscopy (TOF-SIMS), low voltage scanning electron microscopy (LVSEM), and SEM energy dispersive spectroscopy (EDS). High resolution images and sensitive elemental and molecular analysis were obtained with this combined approach. The result of these analyses are presented.

Radicatidibrozolo, F.↗

Influence of microstructure on replacement and porosity generation during experimental dolomitization of limestones

Replacement reactions commonly alter the multiscale pore structures of rocks during fluid-rock interactions. Analysis of these processes in various model fluid-rock systems during controlled laboratory experiments provides insights into the origins of microstructures found in natural materials. This study focused on understanding the effects of initial starting material permeability and resultant differences in transport pathways on porosity and mineralogical changes during limestone dolomitization.A series of replacement experiments (32–317 days in duration) have been conducted in which 1.59 cm (5/8 in.) diameter cores of two different limestones were reacted with saturated MgCl2 solutions at 200 °C. The Texas Cream (Austin Chalk) is a high-porosity, high-permeability limestone, whereas both the porosity and permeability of the Carthage Marble (Burlington Limestone) are relatively low. Altered limestones were imaged using scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX), Time-of-Flight Secondary Ion Mass Spectrometry (ToF–SIMS) and electron microprobe analysis (EMPA). A representative grain boundary of the low-porosity limestone was targeted for a focused ion beam (FIB) lift-out and characterized using transmission electron microscopy (TEM). These results were coupled with analyses of radial changes in the porosity distribution of the core derived from X-ray and neutron small- and ultra-small angle scattering ((U)SANS/(U)SAXS).The high-porosity/permeability limestone showed a four times faster bulk replacement rate than the lower-porosity/permeability material, and a different mechanism of porosity development. For the low-porosity limestone, a two-stage replacement occurred, with the reacted region of the core consisting of an inner rim in which the limestone was replaced by two calcite-dolomite solid solutions, and an outer rim in which the dolomite was replaced by magnesite. Elongated pores formed along grain boundaries at the initial limestone/dolomite reaction interface, and additional nanometer-scale porosity was formed at the secondary magnesite replacement rim. Grain boundaries were identified as preferential pathways for transport leading to dolomitization and a grain boundary diffusion rate was calculated based on microstructural characterization. In contrast, replacement in the high-porosity limestone was accompanied by porosity generation through replacement of individual grains by dolomite throughout the sample and, in longer runs, magnesite in outer parts of the core. These observations emphasize that both the mechanisms of the replacement reaction and the microstructure and chemistry of the replaced product are contingent on the initial structure of the starting material.

36 MATERIALS SCIENCE↗

Ultracold Electrons via Near-Threshold Photoemission from Single-Crystal Cu(100)

Achieving a low mean transverse energy or temperature of electrons emitted from the photocathode-based electron sources is critical to the development of next-generation and compact x-ray free electron lasers and ultrafast electron diffraction, spectroscopy, and microscopy experiments. In this Letter, we demonstrate a record low mean transverse energy of 5 meV from the cryo-cooled (100) surface of copper using near-threshold photoemission. Further, we also show that the electron energy spread obtained from such a surface is less than 11.5 meV, making it the smallest energy spread electron source known to date: more than an order of magnitude smaller than any existing photoemission, field emission, or thermionic emission based electron source. Overall, our measurements also shed light on the physics of electron emission and show how the energy spread at few meV scale energies is limited by both the temperature and the vacuum density of states.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Optimization of submicron Ni/Au/Ge contacts to an AlGaAs/GaAs two-dimensional electron gas

We report on fabrication and performance of sub-micrometer Ni/Au/Ge contacts to a two-dimensional electron gas in an AlGaAs/GaAs heterostructure. Utilizing scanning transmission electron microscopy, energy dispersive x-ray spectroscopy, and low temperature electrical measurements, we investigate the relationship between contact performance and the mechanical and chemical properties of the annealed metal stack. Contact geometry and crystallographic orientation significantly impact performance. Our results indicate that the spatial distribution of germanium in the annealed contact plays a central role in the creation of high transmission contacts. We characterize the transmission of our contacts at high magnetic fields in the quantum Hall regime. Our work establishes that contacts with an area of 0.5 μm2 and resistance less than 400 Ω can be fabricated with high yield.

Physics↗

Abrupt orthorhombic relaxation in compressively strained ultrathin SrRuO 3 films

Lattice structure can dictate electronic and magnetic properties of a material. Especially, reconstruction at a surface or heterointerface can create properties that are fundamentally different from those of the corresponding bulk material. In this work, we have investigated the lattice structure on the surface and in the thin films of epitaxial SrRuO 3 with the film thickness up to 22 pseudo-cubic unit cells (u.c.), using the combination of surface sensitive low energy electron diffraction and bulk sensitive scanning transmission electron microscopy. Our analysis indicates that, in contrast to many perovskite oxides, the RuO6 tilt and rotational distortions appear even in single unit cell SrRuO 3 thin films on cubic SrTiO 3 , while the full relaxation to the bulk-like orthorhombic structures takes 3-4 u.c. from the interface for thicker films. Yet the TiO 6 octahedra of the substrate near the interface with SrRuO 3 films show no sign of distortion, unlike those near the interface with CaRuO 3 films. Two orthogonal in-plane rotated structural domains are identified. These octahedral distortions are essential for the understanding of the thickness dependent transport and magnetism in ultrathin films.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

High-Entropy Alloys for Accelerator Beam Window Applications

Development of novel high-entropy alloys (HEAs) is currently underway for potential use as beam windows in future multi-megawatt target systems at Fermilab. HEAs encompass a new class of materials with a vast design space allowing for material properties to be tailored for particular applications and to potentially offer improved resistance to beam-induced radiation damage and thermal shock effects. The alloy systems being studied consist of several compositions of AlCoCrMnTiV with 4 6 component elements. These alloys are all predicted by CALPHAD simulation to have a single-phase BCC crystal structure and low density, with some compositions displaying ordered, nanoscale precipitates. This presentation will briefly discuss alloy design and synthesis before giving a detailed description of the characterization studies of these HEAs in both the pristine state and post-irradiation by low-energy heavy ions to high damage levels. Electron microscopy techniques to quantify elemental homogeneity and composition, determine grain size, shape, and orientation, and quantify lattice parameters, defect structures and precipitate phases are all being used to study alloy microstructures. Mechanical properties of the alloys at the microscale will be reported. The evolution of these properties as a function of radiation damage will also be described. Bulk thermal characteristics of these HEAs have been tested to measure specific heat capacity and coefficient of thermal expansion as a function of temperature. To determine bulk tensile properties a miniature tensile testing apparatus is under development; it s commissioning will be covered briefly. The talk will conclude with our plans for alloy down-selection.

Burleigh, A. [Fermilab]↗

Use of LEED, Auger emission spectroscopy and field ion microscopy in microstructural studies.

The studies reported were conducted to gain a fundamental understanding of adhesion and dynamic friction on an atomic or microscopic level. Fundamental aspects of low energy electron diffraction (LEED), Auger emission spectroscopy (AES), and field ion microscopy (FIM) are discussed. Typical results of studies conducted are considered, giving attention to LEED-AES experiments, pin and disk experiments, and field ion microscope investigations.

Ferrante, J.↗

An in situ ambient and cryogenic transmission electron microscopy study of the effects of temperature on dislocation behavior in CrCoNi-based high-entropy alloys with low stacking-fault energy

Temperature is known to affect deformation mechanisms in metallic alloys. As temperature decreases, the stacking-fault energy in many face-centered cubic (fcc) alloys decreases, resulting in a change of deformation mode from dislocation slip to deformation twinning. Such an impact of temperature can be more complex in compositionally heterogeneous microstructures that exhibit, for example, local concentration fluctuation such as that in multi-principal element alloys. In this work, we compare the dislocation behavior and mechanical properties of a fcc Cr 20 Mn 10 Fe 30 Co 30 Ni 10 high-entropy alloy at ambient and liquid-nitrogen temperatures. We find that a network of stacking faults is formed by uniformly extended dislocations at ambient temperatures with low stacking-fault energy, whereas at lower temperatures, uneven dissociation of dislocations becomes significant, which results in severe dislocation pile-ups together with their pronounced entanglement. Our findings indicate that as the stacking-fault energy decreases with decreasing temperature, the heterogeneity of the distribution of elements becomes more dominant in tuning the local variation of lattice resistance. As a result, the change in dislocation behavior at low temperatures strongly affects microstructural evolution and consequently leads to significantly more pronounced work hardening.

36 MATERIALS SCIENCE↗

Identification, isolation, and characterization of a novel type of Fukushima-derived microparticle

Abstract In the course of the Fukushima nuclear accident, radionuclides were released in various forms, including so-called radiocesium-bearing microparticles (CsMP). So far, four types of CsMP were described: Type A is smaller in size (< 10 μm), Types B, C, and D are larger (> 100 μm). In this work, we present a novel type of CsMP (proclaimed Type E). Three particles of Type E were extracted from a contaminated blade of grass that was sampled 1.5 km from the Fukushima Daiichi nuclear power plant in late 2011. They were located using autoradiography, isolated using an optical microscope and micromanipulator, and characterized using scanning electron microscopy, energy dispersive x-ray spectroscopy, and low-level gamma-ray spectrometry. Type E CsMPs are 10–20 μm in size and exhibit an unusually low and barely detectable 137 Cs activity of only ≤ 10 mBq per particle. Their brittle and fragile character may indicate a high surface tension.

137Cs↗

Structure and properties of solid surfaces

Difficulties in experimental studies of crystalline surfaces are related to the fact that surface atoms have an intrinsic tendency to react with their environment. A second problem is connected with the effective thickness of surfaces, which ranges from one to several atom layers. The phenomenology of surface interactions with gases are considered, taking into account physical adsorption, chemisorption, and the oxidation of surfaces. Studies of the surface structure are discussed, giving attention to field emission microscopy, field-ion microscopy, electron diffraction techniques, Auger spectroscopy, scanning electron microscopy, electron probe microanalysis, ion microprobe methods, and low-energy backscattering spectroscopy. Investigations of semiconductor surfaces are also described.

Gatos, H. C.↗

Tunable Plasma Linearizer for Compensation of Nonlinear Energy Chirp

The removal of undesired nonlinear time-energy correlation (energy chirp) present in relativistic electron beams is crucial for many accelerator-based scientific applications, such as free-electron lasers, high-energy electron radiography, and MeV ultrafast electron microscopy. Here, we propose and demonstrate that a low-density plasma section can be used as a passive “linearizer” to significantly compensate for the nonlinear energy chirp imprinted on a beam by the curvature of the radio-frequency field in a conventional accelerator. Physically, the passage of the beam through the plasma excites a strong quasi-cosinoidal longitudinal decelerating wakefield that acts to mitigate the beam’s nonlinear energy chirp by superimposing a reverse chirp on the beam. Time-resolved phase-space measurements, combined with high-fidelity three-dimensional particle-in-cell simulations show that the longitudinal phase space of the beam core is almost completely linearized, leading to a fourfold reduction of the beam overall energy spread from 0.148% to 0.036% (FWHM).

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Argon broad ion beam sectioning and high resolution scanning electron microscopy imaging of hydrated alite

Highlights: • The native fibrous outer and dense inner C-S-H structure are preserved by using low energy argon broad ion beam sectioning. • Possible artefacts of the preparation and imaging of hydrated alite are shown and discussed. • An approach for a semi automated pore analysis of the obtained high resolution images is demonstrated. Scanning electron microscopy (SEM) imaging is able to visualize micro- to nano-structures of cement and concrete. A prerequisite is that the sample preparation preserves the native structure of the specimen. In this study, argon broad ion beam (BIB) sectioning is compared to state-of-the-art sample preparation (resin embedding, polishing) for hydrated alite. Additionally, it is investigated if during BIB, sample cooling is beneficial to avoid deterioration of cement hydrates. The aim is to quantitatively measure pore size distributions in hardened alite pastes. Therefore, not only optimized sample preparation but also optimized imaging conditions are investigated. Finally, it is demonstrated that by image analysis pores down to a diameter of 5 nm in hydrated alite pastes can be quantitatively analysed.

36 MATERIALS SCIENCE↗

Structural Origins of High MoO 3 Solubility in Peraluminous Borosilicate Glasses

Molybdenum (Mo) imposes strict loading limits in conventional borosilicate nuclear waste glasses due to the tendency of tetrahedral molybdate [MoO 4 ] 2− species to phase-separate and crystallize as alkali molybdates. Here, we demonstrate an unprecedented 13.96 wt % (7.51 mol %) MoO 3 solubility in peraluminous sodium aluminoborosilicate glasses a ∼15× increase over their peralkaline counterparts. Using Raman spectroscopy, multinuclear and dipolarcorrelation magic angle spinning nuclear magnetic resonance (MAS NMR), electron paramagnetic resonance (EPR), and scanning transmission electron microscopy (STEM)-energy dispersive spectroscopy (EDS), we reveal that Nadeficient, low optical basicity conditions stabilize octahedral MoO 6 units, which polymerize into molybdite-like Mo−O clusters dispersed within the glass matrix. These Mo-rich clusters suppress the formation of depolymerized [MoO 4 ] 2− environments typically responsible for Na 2 MoO 4 precipitation and instead promote the formation of Na 2 Mo 2 O 7 as the saturation phase. Concurrently, Mo solubility drives the conversion of AlO 4 − to higher-coordination AlO 5 species, liberating Na + that is subsequently sequestered in molybdate-rich domains. The combined evolution of Mo coordination, modifier redistribution, and network depolymerization provides a mechanistic basis for the markedly enhanced Mo solubility in peraluminous compositions. These findings establish new structural guidelines for designing aluminoborosilicate waste forms with substantially greater capacity to incorporate Mo-rich nuclear waste streams.

Amorphous materials↗

LDEF impact craters formed by carbon-rich impactors

Two small craters (number 74, 119 microns, and number 31, 158 microns in diameter) with depth to diameter ratios of about 0.59 and 0.8, respectively, were found in Al from the Long Duration Exposure Facility (LDEF) experiment tray A11EOOF). Both craters have residues concentrated in the crater bottoms, along the walls, and on top of the overturned rims. Low voltage scanning electron electron microscopy, Auger electron spectroscopy, time of flight secondary ion mass spectroscopy and energy dispersive x-ray spectroscopy were used to obtain high resolution imagery and elemental analysis. Analyses indicate that the impactor for both craters was carbon-rich, as the residues contain mostly C. Silicon, S, and F in low concentrations are present on the Al surface away from the craters and may be, in part, contaminants.

Bunch, T. E.↗

Ice-rule driven vertex frustration in a stretched pentagonal spin ice

We introduce the stretched pentagonal spin ice and study low-energy configurations achieved after thermal annealing. Using synchrotron-based photoemission electron microscopy, we reveal highly disordered configurations dominated by short-range order. Real-space observations reveal that an adherence to local order, in the form of a strict ice-rule obedience, acts as a main factor in enforcing vertex frustration and hindering long-range order. Our results open up pathways to create forms of frustrated systems that have seemed elusive thus far. Published by the American Physical Society 2024

Crater, Davis (ORCID:0009000168933822)↗

Synthesis and Characterization of the First Liquid Single Source Precursors for the Deposition of Ternary Chalcopyrite (CuInS2) Thin Film Materials

Molecular engineering of ternary single source precursors based on the [{PBu3}2Cu(SR')2In(SR')2] architecture have afforded the first liquid CIS ternary single source precursors (when R = Et, n-Pr), which are suitable for low temperature deposition (< 350 C). Thermogravimetric analyses (TGA) and modulated-differential scanning calorimetry (DSC) confirm their liquid phase and reduced stability. X-ray diffraction studies, energy dispersive analyzer (EDS), and scanning electron microscopy (SEM) support the formation of the single-phase chalcopyrite CuInS2 at low temperatures.

Banger, Kulbinder K.↗

Self-Assembled BaTiO 3 –Au x Ag 1– x Low-Loss Hybrid Plasmonic Metamaterials with an Ordered “Nano-Domino-like” Microstructure

Metallic plasmonic hybrid nanostructures have attracted enormous research interest due to the combined physical properties coming from different material components and the broad range of applications in nanophotonic and electronic devices. However, the high loss and narrow range of property tunability of the metallic hybrid materials have limited their practical applications. In this study, a metallic alloy-based self-assembled plasmonic hybrid nanostructure, i.e., a BaTiO 3 –Au x Ag 1– x (BTO) vertically aligned nanocomposite, has been integrated by a templated growth method for low-loss plasmonic systems. Comprehensive microstructural characterizations including high-resolution scanning transmission electron microscopy (HRSTEM), energy-dispersive X-ray spectroscopy (EDS), and three-dimensional (3D) electron tomography demonstrate the formation of an ordered “nano-domino-like” morphology with Au 0.4 Ag 0.6 nanopillars as cylindrical cores and BTO as square shells. By comparing with the BTO–Au hybrid thin film, the BTO–Au 0.4 Ag 0.6 alloyed film exhibits much broader plasmon resonance, hyperbolic dispersion, low-loss, and thermally robust features in the UV–vis–NIR wavelength region. This study provides a feasible platform for a complex alloyed plasmonic hybrid material design with low-loss and highly tunable optical properties toward all-optical integrated devices.

36 MATERIALS SCIENCE↗

Optical Scattering and Microstructure of Ion Beam Deposited Metal Coatings

Thin films of gold and platinum have been deposited onto super-polished fused silica substrates using thermal evaporation, ion assisted deposition (IAD), sputtering and ion assisted sputtering. The influence of ion beam flux, coating material and deposition rate on the films microroughness have been investigated. Coatings of gold and platinum have been bombarded with low energy (10-20 eV) Ar ions from an electron cyclotron resonance (ECR) ion source during deposition. Short range surface microroughness of coated surfaces has been examined using scanning tunneling microscopy (STM) and atomic force microscopy (AFM), while long range surface microroughness has been characterized using an angle resolved optical scatterometer. Results indicate that bombardment with low energy ions causes significant reduction in microroughness of metal coatings.

metal↗