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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 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
NASA NTRS1994

Bench-scale synthesis of nanoscale materials

A novel flow-through hydrothermal method used to synthesize nanoscale powders is introduced by Pacific Northwest Laboratory. The process, Rapid Thermal Decomposition of precursors in Solution (RTDS), uniquely combines high-pressure and high-temperature conditions to rapidly form nanoscale particles. The RTDS process was initially demonstrated on a laboratory scale and was subsequently scaled up to accommodate production rates attractive to industry. The process is able to produce a wide variety of metal oxides and oxyhydroxides. The powders are characterized by scanning and transmission electron microscopic methods, surface-area measurements, and x-ray diffraction. Typical crystallite sizes are less than 20 nanometers, with BET surface areas ranging from 100 to 400 sq m/g. A description of the RTDS process is presented along with powder characterization results. In addition, data on the sintering of nanoscale ZrO2 produced by RTDS are included.

Buehler, M. F.↗
NASA NTRS1988

Dual-Cathode Electron-Beam Source

Beam from either cathode electromagnetically aligned with exit port. Electron beam from either of two cathodes deflected by magnetic and electric fields to central axis. Mechanical alignment of beam easy because cathode axes, anode apertures, and electron trajectories coplanar. Applications where uninterrupted service needed: scanning electron microscopes, transmission electron microscopes, electron-beam lithography equipment, Auger instruments, and microfocused x-ray sources.

Bradley, James G.↗
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↗
NASA NTRS1978

The calibration of photographic and spectroscopic films: 1: A microscopic analysis of IIaO films. 2: The effects of agitation and soaking on IIaO films. 3: The effects of electric field on IIaO films. 4: The effects of X-ray radiation on IIaO films

The grain structure of the emulsion using both reflected and transmission light was examined along with the effects of soaking. The effect of a static charge by a Tesla-coil, and the effects of airport equipment, and dental X-rays on the film were also analyzed.

Hammond, E. C., Jr.↗
NASA NTRS1980

The effects of titanium impurities in N/+//P silicon solar cells

Microscopic and electrical measurements were performed to explain the degradation mechanisms associated with the presence of titanium impurities in silicon. The measurements included X-ray topography, transmission electron microscopy, and deep level transient spectroscopy, before and after processing. The results indicated the presence of TiO2 precipitates, the density of which increased after phosphorus diffusion. A majority carrier trapping level was observed in the wafers before processing. It was concluded that 10% of the Ti in the N(+)/P silicon solar cells formed electrically active centers which caused degradation of the cell junction. 14% of the remaining Ti precipitated out as TiO2, forming electrically active defects, which also caused junction degradation.

Salama, A. M.↗
NASA NTRS1987

Morphometrics of cellular damage in mice testis receiving X-ray and high-energy particle irradiation

Murine tests were exposed to single, low doses of either X-ray, helium, or argon radiation. Animals were sacrificed seventy-two hours later. Testes were fixed for transmission electron microscopy (TEM) and sectioned at either 60 nm for TEM observation or at 2 micron for counting using routine light microscope methods. Counts of the total population of surviving spermatogonia, including all type A cells, intermediate, and type B cells, were taken from tubule cross sections identified as Stage 6 and Stage 1 according to spermatogonial configuration. The surviving fraction of spermatogonia as compared to control, S/S sub o, was calculated for each dose. For both ions and X-rays, there was a rapid decline in survival at dose levels of .10 to .15 Gy in Stage 6 tubules. This was followed by a more gradual decrease in population. At higher doses, 0.30 Gy for argon and 0.80 Gy for helium and X-rays, the cell survival rates declined rapidly. Pre-leptotene spermatocytes in Stage 1 tubules exhibited a different survival curve indicating the extreme radio-sensitivity of type B spermatogonia. Data verify that the seminiferous tubules are composed of a heterogeneous population of cells with different radio-sensitivities and that these differences are manifested even at very low doses.

Sapp, Walter J.↗
DOE OSTI2026

Crystal Orientation and Defect Mapping in Electron-Beam-Sensitive Zeolites with Near-Axis Transmission Kikuchi Diffraction

Porous materials are vital in catalysis, energy conversion, and environmental remediation. Understanding structural heterogeneity in zeolites is key to linking synthesis, framework intergrowths, and catalytic performance, yet current methods for phase identification and spatial mapping lack sufficient resolution or throughput. We present a high-throughput approach using near-axis transmission Kikuchi diffraction in a scanning electron microscope, achieving high phase and spatial resolution for electron-beam-sensitive zeolites, including ZSM-5 and, for the first time, Zeolite A. Here, this method enables direct visualization of intergrowth features that critically affect catalytic and adsorption behavior, bridging the gap between ensemble-averaged X-ray diffraction and high-resolution but low-throughput transmission electron microscopy. Combining nanoscale mapping with statistical sampling is highly suited for machine-learning pipelines guiding new structure function understanding and could be extended to other beam-sensitive porous materials such as metal–organic or covalent–organic frameworks.

crystallography↗
NASA NTRS1993

Electron microscope observations of impact crater debris amongst contaminating particulates on materials surfaces exposed in space in low-Earth orbit

Debris particles extracted from a small sampling region on the leading edge of the Long Duration Exposure Facility (LDEF) spacecraft have been examined by analytical transmission electron microscopy and the elemental frequency observed by energy-dispersive X-ray spectrometry and compared with upper atmosphere (Earth) particle elemental frequency and the average elemental compositions of interplanetary dust particles. A much broader elemental distribution was observed for the exposed spacecraft surface debris milieu. Numerous metal microfragment analyses, particularly aluminum and stainless steel, were compared with scanning electron microscope observations-of impact crater features, and the corresponding elemental spectra on selected LDEF aluminium tray clamps and stainless steel bolts. The compositions and melt features for these impact craters and ejecta have been shown to be consistent with microcrystalline debris fragments in the case of aluminum, and these observations suggest an ever changing debris milieu on exposed surfaces for space craft and space system materials.

Murr, L. E.↗
NASA NTRS1993

Tin-polyimide and indium-polyimide thin-film composites as soft X-ray bandpass filters

A tin-polyimide and an indium-polyimide soft X-ray bandpass filter were fabricated with thicknesses of 1400 and 1750 A for the metal and polyimide components, respectively. The transmission of each filter was measured at the Stanford Synchrotron Radiation Laboratory. The transmission of the tin-polyimide filter was found to be about 40 percent for radiation with wavelengths between 60 and 80 A. The transmission of the indium-polyimide filter was greater than 40 percent between 70 and 90 A. The indium was about 5 percent more transmissive than the tin and attained a maximum transmission of about 48 percent at 76 A. Such filters have potential applications to soft X-ray telescopes that operate in this region. They might also be of interest to investigators who work with X-ray microscopes that image live biological specimens in the 23-44-A water window.

Powell, Stephen F.↗
NASA NTRS1993

Below band-gap laser ablation of diamond for transmission electron microscopy

A 248 nm excimer laser was used to thin naturally occurring type 1a diamond substrates at normal and glancing (22 deg) incidence. Perforation of a 250-micron-thick substrate was achieved in about 15 min at normal incidence. While the substrate thinned at glancing incidence was found to have large electron-transparent areas, that thinned at normal incidence required additional argon-ion milling to achieve electron transparency. X-ray photoelectron spectroscopy of the back surface of the diamond failed to detect any graphite or glassy carbon, confirming that damage due to laser ablation occurs only at the incident surface. Samples prepared using this technique imaged in the transmission electron microscope were observed to have retained the nitrogen platelets characteristic of such type 1a diamonds.

George, T.↗
NASA NTRS1993

Below Band-Gap Laser Ablation of Diamond for Transmission Electron Microscopy

A 248-nm excimer laser was used to thin naturally occurring type 1a diamond substrates at normal and glancing (22 deg) incidence. Perforation of a 250 micron thick substrate was achieved in about 15 minutes at normal incidence. Whilst the substrate thinned at glancing incidence was found to have large electron-transparent areas, that thinned at normal incidence required additional argon milling to achieve electron transparency. X-ray photoelectron spectroscopy of the back surface of the diamond failed to detect any graphite or glassy carbon, confirming that damage due to laser ablation occurs only at the incident surface. Samples prepared using this technique imaged in the transmission electron microscope were observed to have retained the nitrogen platelets

Posthill, J. B.↗
DOE OSTI2025

Soft Nanoconfinement Nucleates and Stabilizes Ultrasmall Amorphous Calcium Carbonate from Aggregation

Organisms use soft confinement structures, such as vesicles and compartments, to direct the nucleation of calcium carbonate (CaCO 3 ) and its subsequent processes during biomineralization. Despite recent efforts elucidating confinement’s effects on CaCO 3 polymorph selection, we still poorly understand how the size and distribution of CaCO 3 are controlled within soft confinement. Here, using a size-controlled nanoemulsions system made from isooctane, Span 80, Tween 80, and aqueous solutions, we studied CaCO 3 formation in soft confinement. Small angle X-ray scattering (SAXS) confirmed that a 72 nm aqueous core in nanoemulsions served as the confined space for CaCO 3 formation. Unlike the ~ 50 nm CaCO 3 particles that formed in the unconfined solution, small angle neutron scattering (SANS) and transmission electron microscope (TEM) showed that ultrasmall and amorphous calcium carbonate precipitated within soft confinement and did not exhibit any aggregation/coalescence of nanoparticles even after 24 hrs of reaction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1983

Fungi and bacteria involved in desert varnish formation

Desert varnish is a coating of ferromanganese oxides and clays that develops on rock surfaces in arid to semi-arid regions. Active respiration but not photosynthesis was detected on varnished rock surfaces from the Sonoran Desert. Light microscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations, and cultivation experiments indicate that both fungi, primarily dematiaceous hyphomycetes, and bacteria are found on and within desert varnish coatings from the arid regions studied. Some fungi grow as microcolonial fungi (MCF) on rocks, and microscopic observations suggest MCF become incorporated in the varnish coating. SEM-EDAX (energy dispersive X-ray systems) analyses indicate the MCF contain 3 of the characteristic elements of varnish: iron, aluminum, and silicon. In some locations, MCF are also enriched in manganese relative to the rock substratum. Furthermore, some of the dematiaceous hyphomycetes that have been cultivated are able to oxidize manganese under laboratory conditions. It is possible that manganese-oxidizing bacteria, which are found in varnish, also play an important role in varnish formation.

Taylor-George, S.↗
DOE OSTI2025

In situ self-ion (Fe + ) irradiation of ODS-FeCrAl alloy fuel cladding materials with different Cr contents: The early stages of Cr-rich α’ phase precipitation

Oxide-dispersion-strengthened FeCrAl (ODS-FeCrAl) alloys are candidate accident-tolerant fuel cladding materials for light water reactors because they demonstrate satisfactory resistance to materials degradation effects such as high-temperature oxidation, radiation-induced swelling, and creep. Their perspective deployment to market is challenged, however, by their inherent susceptibility to irradiation embrittlement caused by the precipitation of the brittle Cr-rich α’ phase at relatively low temperatures (≤475 °C). This work used in situ self-ion irradiation (150 keV Fe + ) in a transmission electron microscope to elucidate the early stages of Cr-rich α’ phase precipitation in three candidate ODS-FeCrAl alloy fuel cladding materials with different Cr contents (10, 12, and 20 wt.%) and microstructures. The early stages of the process resulting in the precipitation of the Cr-rich α’ phase in these three ODS-FeCrAl alloys under Fe + irradiation were investigated at room temperature and 300 °C up to total fluences of 1.7 × 10 15 ions·cm -2 (2 dpa) and 3.4 × 10 15 ions·cm -2 (4 dpa), using three damage dose rates (5 × 10 –5 , 3.3 × 10 –4 , and 2 × 10 –3 dpa·s -1 ). Post-irradiation examination via scanning transmission electron microscopy, energy-dispersive X-ray spectroscopy and electron energy loss spectroscopy suggested that the precipitation of the Cr-rich α’ phase might be promoted by the phase separation of the alloy matrix into Cr-rich and Fe-rich regions. Interestingly, oxygen impurities segregated preferentially in the Cr-rich regions, possibly promoting the radiation-assisted formation of the Cr-rich α’ phase. α’ phase precipitation was more pronounced at room temperature when compared to 300 °C, and it was clearly promoted by the progressive increase in the Cr content of the ODS-FeCrAl alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Imaging nanoscale carrier, thermal, and structural dynamics with time-resolved and ultrafast electron energy-loss spectroscopy

Time-resolved and ultrafast electron energy-loss spectroscopy (EELS) is an emerging technique for measuring photoexcited carriers, lattice dynamics, and near-fields across femtosecond to microsecond timescales. When performed in either a specialized scanning transmission electron microscope or ultrafast electron microscope (UEM), time-resolved and ultrafast EELS can directly image charge carriers, lattice vibrations, and heat dissipation following photoexcitation or applied bias. Yet, recent advances in theoretical calculations and electron optics are often required to realize the full potential of ultrafast EEL spectrum imaging. Here, in this review, we present a comprehensive overview of the recent progress in the theory and instrumentation of time-resolved and ultrafast EELS. We begin with an introduction to the technique, followed by a physical description of the loss function. We outline approaches for calculating and interpreting ground-state and transient EEL spectra spanning low-loss plasmons to core-level excitations analogous to x-ray absorption. We then survey the current state of time-resolved and ultrafast EELS techniques beyond photon-induced near-field electron microscopy, highlighting abilities to image carrier and thermal dynamics. Finally, we examine future directions enabled by emerging technologies, including electron beam monochromation, in situ and operando cells, laser-free UEM, and high-speed direct electron detectors. These advances position time-resolved and ultrafast EELS as a critical tool for uncovering nanoscale dynamic processes in quantum materials and solar energy conversion devices.

Computational methods↗
DOE OSTI2025

Effect of stress on Laves phase precipitation in creep ruptured Grade 92 ferritic martensitic steel characterized by a novel accessible method

At high temperature conditions relevant to fossil and nuclear energy plants, Laves phase (Fe 2 X, X=Mo, W) precipitation is observed in common ferritic martensitic (FM) structural steels, with various reported effects on creep behavior. Despite being valuable metrics to correlate with mechanical properties and other precipitate phases, the volume fraction and number density of Laves phase precipitates has been difficult to quantify accurately using common techniques such as transmission electron microscopy (TEM) due to the relatively large size (∼0.25 μm) and low number density (∼10 11 cm −3 ) of Laves precipitates. Here, to address this characterization challenge, we developed and demonstrated a high-throughput and widely accessible method to quantify the volume fraction and number density of the Laves phase based on scanning electron microscope (SEM) images with a backscattered electron signal and the information depth (ID) of backscattered electrons. We applied this new technique in creep ruptured Grade 92 FM steel to study the effect of Laves phase on creep properties and determine the influence of stress on Laves phase precipitation. The quantitative accuracy of the SEM-based volume fraction and number density values was verified using synchrotron high energy X-ray diffraction and serial sectioning tomography. Stress did not significantly affect the Laves phase size or volume fraction during creep testing at 550 – 650°C and stress levels of 90 – 260 MPa (vs. unstressed conditions). Conversely, a moderate but statistically significant stress-enhanced increase in Laves phase number density, corresponding to an increase in nucleation rate, occurred during creep exposure above 110 MPa.

Creep↗
DOE OSTI2025

Growth and structure of alpha-Ta films for quantum circuit integration

Tantalum films incorporated into superconducting circuits have exhibited low surface losses, resulting in long-lived qubit states. The remaining loss pathways originate in microscopic defects that manifest as two level systems (TLSs) at low temperatures. These defects limit performance, so careful attention to tantalum film structures is critical for optimal use in quantum devices. In this work, we investigate the growth of tantalum using magnetron sputtering on sapphire, Si, and photoresist substrates. In the case of sapphire, we present procedures for the growth of fully-oriented films with α-Ta [1 1 1]//Al2O3 [0 0 0 1] and α-Ta [1 −1 0]//Al2O3 [1 0 −1 0] orientational relationships and having residual resistivity ratio (RRR) ∼ 60 for 220 nm thick films. On Si, we find a complex grain texturing with Ta [1 1 0] normal to the substrate and RRR ∼ 30. We further demonstrate airbridge fabrication using Nb to nucleate α-Ta on photoresist surfaces. For the films on sapphire, resonators show TLS-limited quality factors of 1.3 ± 0.3 × 106 at 10 mK (for a waveguide gap and conductor width of 3 and 6 μm, respectively). Structural characterization using scanning electron microscopy, x-ray diffraction, low temperature transport, secondary ion mass spectrometry, and transmission electron microscopy reveal the dependence of residual impurities and screw dislocation density on processing conditions. The results provide practical insights into the fabrication of advanced superconducting devices including qubit arrays and guide future works on crystallographically deterministic qubit fabrication.

42 ENGINEERING↗
DOE OSTI2025

Experimental and theoretical investigation of the crystalline surface, film, and interface properties of antiperovskite Mn 3 GaN grown by molecular beam epitaxy on MgO(001)

Here, we present a study of the epitaxial growth, characterization, and theoretical modeling of thin film antiperovskite Mn 3 GaN, an antiferromagnetic material with kagome structure which is grown on MgO (001) substrates using N-plasma-assisted molecular beam epitaxy. Reflection high energy electron diffraction is used to assess the in-plane evolution of the film structure during growth, and the surface is investigated in-situ using scanning tunneling microscopy and Auger electron spectroscopy. These results are combined with precision measurements done ex-situ determining the film lattice constants using a combination of x-ray diffraction with reciprocal space mapping and scanning transmission electron microscopy. Overall, a uniform, homogeneous film with an atomically smooth vacuum surface and atomically sharp substrate interface is found having very small in-plane tensile strain and mild out-of-plane compressive strain. First-principles theoretical calculations are applied in order to ascertain the lowest energy models for both the Mn 3 GaN surface and the Mn 3 GaN/MgO film/substrate interface. Models including MnGa versus MnN surface layers and MnGa versus MnN interfacial layers are considered as functions of both the Mn and Ga chemical potentials. The predictions are discussed in comparison to the experimental results. The overall findings suggest that Mn 3 GaN on MgO(001) is a viable epitaxial film which can be further explored in connection with antiferromagnetic spintronics.

Density functional theory↗