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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 271 records · Page 15
All sourcesNASA NTRSDOE OSTI
NASA NTRS2018

Portable Electron Microscopy for ISS and Beyond

Advances in space exploration have evolved in lockstep with key technology advances in diverse fields such as materials science, biological science, and engineering risk management. Research in these areas, where structure and physical processes come together, can proceed rapidly in part due to sophisticated ground-based analytical tools that help re-searchers develop technologies and engineering processes that push frontiers of human space exploration. Electron microscopes (EM) are an example of such a workhorse tool, lending a unique blend of strong optical scattering, high native resolution, large depth of focus, and spectroscopy via characteristic X-ray emission, providing exquisite high-magnification structural imaging and chemical analysis. Ground-based EM’s have been essential in NASA research for many years. In particular, in mineralogy and petrology, EM is used to understand the origin and evolution of the solar system, particularly rocky bodies. In microbiology, EM has helped visualize the architecture of tissues and cells. In engineering/materials science, EM has been used to characterize particulate debris in air and water samples, determine pore sizes in ceramics/catalysts, understand the nature of fibers, determine composition and morphology of new and existing materials, and characterize micro-textures of vapor deposited films. EM is highly effective at investigating a wide variety of nanoscale materials/biomaterials at the core of many of NASA’s inquiries. Despite exquisite optical performance and versatility, EM’s are traditionally large, heavy, and have high power consumption. They are also expensive so they tend to be housed at universities and large research institutions, or at major industrial laboratory sites with support staff, supplies, and skilled operators. Since most organizations cannot support their own EM, samples are often sent to these large institutions and service centers to be imaged, at great expense and of-ten with delay of weeks to months for complex analyses. Complexity, high cost, and maintenance associated with collecting EM image data has until now severely limited fields in which EM is used. Making EM accessible outside constrained terrestrial laboratory environments will bring EM’s performance and versatility to a much broader range of scientific and engineering endeavors, including in space.

Own, C. S.↗
NASA NTRS1973

Applications of cryogenics in electron microscopy

Description of research and development efforts which resulted in a high-voltage cryoelectron microscope system capable of consistent operation at 1.8 to 4.2 K. Attention is given to the design and operation of superconducting objective lenses providing enhanced resolution during longer exposure times at lower beam intensities (thus reducing radiation damage of specimens). A specific system described combines a closed-cycle superfluid helium refrigerator integrated with a modified 200 kV electron microscope. Consistent resolutions of 8 to 16 A are attained with significantly reduced radiation damage, contamination, and thermal noise in prolonged vibration-free examination of specimens at temperatures from 1.8 to 4.2 K. Applications in specific disciplines are discussed, including membrane ultrastructure, cryobiology, microelectronics, and general superconductivity research.

Fernandez-Moran, H.↗
NASA NTRS1989

Moessbauer spectroscopy and scanning electron microscopy of the Murchison meteorite

Meteorites provide a wealth of information about the solar system's formation, since they have similar building blocks as the Earth's crust but have been virtually unaltered since their formation. Some stony meteorites contain minerals and silicate inclusions, called chondrules, in the matrix. Utilizing Moessbauer spectroscopy, we identified minerals in the Murchison meteorite, a carbonaceous chondritic meteorite, by the gamma ray resonance lines observed. Absorption patterns of the spectra were found due to the minerals olivine and phyllosilicate. We used a scanning electron microscope to describe the structure of the chondrules in the Murchison meteorite. The chondrules were found to be deformed due to weathering of the meteorite. Diameters varied in size from 0.2 to 0.5 mm. Further enhancement of the microscopic imagery using a digital image processor was used to describe the physical characteristics of the inclusions.

Brown, Christopher L.↗
NASA NTRS1994

Laboratory Investigation of the Growth and Crystal Structure of Nitric Acid Hydrates by Transmission Electron Microscopy (TEM)

A great deal of recent laboratory work has focussed on the characterization of the nitric acid hydrates, thought to be present in type I Polar Stratospheric Clouds (PSCs). Phase relationships and vapor pressure measurements (1-3) and infrared characterizations (4-5) have been made. However, the observed properties of crystalline solids (composition, melting point, vapor pressure, surface reactivity, thermodynamic stability, extent of solid solution with other components, etc.) are controlled by their crystal structure. The only means of unequivocal structural identification for crystalline solids is diffraction (using electrons, X-rays, neutrons, etc.). Other observed properties of crystalline solids, such as their infrared spectra, their vapor pressure as a function of temperature, etc. yield only indirect information about what phases are present, their relative proportions, or whether they are crystalline or amorphous.

Blake, David F.↗
NASA NTRS2007

Irradiation Effects in Fosterrite and the Nature of Interstellar Grains: A Coordinated Spectroscopy and Electron Microscopy Study

Crystalline and amorphous silicates condense in the outflows of low mass evolved stars and massive red supergiant stars and are injected into the interstellar medium (ISM) where they are rendered almost completely amorphous by a multitude of destructive processes (e.g. shock, grain-grain collisions, and irradiation). Irradiation effects in particular may have played an important role in the genesis and modification of primitive grains in cometary dust, but unraveling those effects requires controlled experiments under appropriate conditions and with an emphasis on materials relevant to the ISM. Here we report our infrared (IR) microspectroscopy and trans-mission electron microscope (TEM) measurements on forsterite that was amorphized through irradiation by high energy heavy ions.

Keller, Lindsay P.↗
DOE OSTI2024

Correlation of Processing and Structure in an Ethylene‐Glycol Side‐Chain Modified Polythiophene via Combined X‐Ray Scattering and 4D Scanning Transmission Electron Microscopy

The results of a combined grazing incidence wide-angle X-ray scattering (GIWAXS) and 4D scanning transmission microscopy (4D-STEM) analysis of the effects of thermal processing on poly(3[2-(2-methoxyethoxy)ethoxy]-methylthiophene-2,5-diyl) are reported, a conjugated semiconducting polymer used as the active layer in organic electrochemical transistor devices. GIWAXS provides a measure of overall crystallinity in the film, while 4D-STEM produces real-space maps of the morphology and orientation of individual crystallites along with their spatial extent and distribution. The sensitivity of the 4D-STEM detector allows for collection of electron diffraction patterns at each position in an image scan while limiting the imparted electron dose to below the damage threshold. In conclusion, the effects of heat treatment on the distribution and type of crystallites present in the films is determined.

36 MATERIALS SCIENCE↗
NASA NTRS2013

Transmission Electron Microscopy of Itokawa Regolith Grains

Introduction: In a remarkable engineering achievement, the JAXA space agency successfully recovered the Hayabusa space-craft in June 2010, following a non-optimal encounter and sur-face sampling mission to asteroid 25143 Itokawa. These are the first direct samples ever obtained and returned from the surface of an asteroid. The Hayabusa samples thus present a special op-portunity to directly investigate the evolution of asteroidal sur-faces, from the development of the regolith to the study of the effects of space weathering. Here we report on our preliminary TEM measurements on two Itokawa samples. Methods: We were allocated particles RA-QD02-0125 and RA-QD02-0211. Both particles were embedded in low viscosity epoxy and thin sections were prepared using ultramicrotomy. High resolution images and electron diffraction data were ob-tained using a JEOL 2500SE 200 kV field-emission scanning-transmission electron microscope. Quantitative maps and anal-yses were obtained using a Thermo thin-window energy-dispersive x-ray (EDX) spectrometer. Results: Both particles are olivine-rich (Fo70) with μm-sized inclusions of FeS and have microstructurally complex rims. Par-ticle RA-QD02-0125 is rounded and has numerous sub-μm grains attached to its surface including FeS, albite, olivine, and rare melt droplets. Solar flare tracks have not been observed, but the particle is surrounded by a continuous ~50 nm thick, stuctur-ally disordered rim that is compositionally similar to the core of the grain. One of the surface adhering grains is pyrrhotite show-ing a S-depleted rim (~8-10 nm thick) with nanophase Fe metal grains (<5 nm) decorating the outermost surface. The pyrrhotite displays a complex superstructure in its core that is absent in the S-depleted rim. Particle RA-QD02-0211 contains solar flare particle tracks (~2x109 cm-2) and shows a structurally disordered rim ~100 nm thick. The track density corresponds to a surface exposure of ~103-104 years based on the track production rate of [1]. The dis-ordered rim is nanocrystalline with minor amorphous material between crystalline domains. Quantitative element maps show the outermost ~10 nm of the disordered rim is Si-rich. Discussion and Conclusions: Both particles record the ef-fects of space weathering processes on Itokawa. Noguchi et al. [2] proposed that the disordered rims they observed on Itokawa particles largely result from solar wind radiation damage and we arrive at a similar conclusion for the two particles we analyzed. The microstructure of the S-depleted layer on the pyrrhotite grain in RA-QD02-0125 is similar to that observed in troilite irradiated with ~1018 4 kV He+ [3, 4]. Prolonged irradiation has also been shown to disorder pyrrhotite such that the superstructure reflec-tions are lost [5].

Keller, Lindsay P.↗
DOE OSTI2025

Revealing Defect-Seeded and Interfacial Generation Mechanisms of Photoinduced Coherent Phonons with 4D Ultrafast Electron Microscopy

Ultrafast photoexcitation of coherent phonons is driven by an impulsive, collective displacement of constituent atoms from their average equilibrium lattice positions [1]. Models describing the generation of coherent acoustic modes typically invoke the creation of an anisotropic strain profile arising from the relatively instantaneous absorption of an ultrafast laser pulse [2]. If the skin depth is shallow relative to the specimen thickness, a steep tensile strain gradient perpendicular to the surface ($\frac{∂ε}{∂z}$) results. Initial relaxation occurs via rapid contraction of the surface layers followed by subsequent coherent oscillations of the lattice and launch of a train of coherent elastic strain waves [i.e., coherent acoustic phonons (CAPs)]. Macroscopically, responses are generally well-described by constitutive relations as gleaned from data gathered using ultrasonic methods or ultrafast spectroscopies. Furthermore, at the atomic to nanoscale level, individual lattice discontinuities and their impact on CAP behaviors can be modeled using multiscale methods [3,4]. Further, average unit-cell level responses on ultrafast timescales can be probed using femtosecond electron and X-ray scattering [5,6].

Flannigan, David J. [University of Minnesota, Minn↗
NASA NTRSDate not supplied

A Transmission Electron Microscopy Study of a Refractory Metal Grain from a Calcium-Aluminum-Rich Inclusion in the Leoville CV3 Chondrite

Introduction: Calcium-aluminum-rich inclusions (CAIs) are an important component of chondritic meteorites. They can contain materials that are thermodynamically predicted and isotopically age dated to be among the first-formed solids in our solar system [1-5]. Observed in some CAIs are micron to sub-micron sized inclusions rich in Fe, Ni, and high-Z elements such as Pt, Os, Ir and W, in the form of refractory metal nuggets (RMNs), fremdlinges, and ‘nugget like objects’ (NLOs) [1,6]. Refractory siderophile elements such as Os, Ir and Ru are thermodynamically predicted to condense at temperatures well in excess of the major CAI phases such as melilite, perovskite, spinel and hibonite [2,7-9]. These refractory metal inclusions in CAIs can therefore serve as probes into the thermodynamic landscape of the early solar protoplanetary disk. Here we report on a refractory grain identified in a CAI of the Leoville CV3 chondrite. This work is part of an ongoing effort to gain insight into the thermochemistry of the early solar system through systematic analyses of the structure and chemistry of various components in CAIs [10-13]. Sample and Analytical Techniques: A fluffy type A CAI (Fig. 1A) was identified in a section of the Leoville, CV3 chondrite (Center for Meteorite Studies, Arizona State University collection, #821_C_3) using a JOEL-JXA 8530F electron microprobe at Arizona State University. Backscattered electron (BSE) imaging and energy-dispersive X-ray spectroscopy (EDS) were used to identify refractory metal grains in the CAI using a Thermo Fisher (formerly FEI) Helios NanoLab 660 G3 focused-ion-beam scanning-electron microscope (FIBSEM) located at the Kuiper Materials Imaging and Characterization Facility (KMICF) at the Lunar and Planetary Laboratory, University of Arizona. The FIB is equipped with an EDAX EDS system. We selected one of the larger (micron-sized) refractory metal grains, designated as ‘Spud’ (Fig. 1B) for further analysis. ‘Spud’ was extracted and thinned to electron transparency (<100 nm) using the FIB-SEM located in KMICF, following methods described by [14- 15]. The FIB section was analyzed using a 200 keV Hitachi HF5000 scanning transmission electron microscope (S/TEM) located at KMICF. The HF5000 is equipped with cold-field emission gun, 3rd-order spherical aberration corrector for STEM imaging, and an Oxford Instruments X-Max N 100 TLE energydispersive spectroscopy (EDS) system with dual 100 mm2 windowless silicon-drift detectors (Ω = 2.0 sr). Selected-area electron-diffraction (SAED) patterns were acquired to aid in determination of crystallinity and phase. Results: The mineralogy, texture, and morphology of the CAI are consistent with that of a fluffy type A (FTA) CAI [16]. BSE imaging at high magnifications revealed grains with high contrast, indicative of compositions rich in elements of higher atomic number relative to surrounding material. These high-Z grains have sizes that range from ∼250 nm to 4 µm. EDS analyses confirm that the bright grains are metal-rich inclusions. A minor fraction of the grains are composed of only Fe and Ni, but the majority (∼60%) of the identified inclusions also contained various refractory siderophiles including Os, Ru, Zr, Ir and Mo. EDS analysis on the FIB-SEM of Spud shows that it contains Fe, Ni, Mo and Ru. High-angle annular dark-field (HAAFD) imaging and EDS mapping in the TEM (Fig. 2) show that Spud occurs in melilite (Ca1.9Al1.99Si1.06O7). Spud contains a subhedral to anhedral morphology and is compositionally heterogenous (polyphasic, Fig. 2). Local spatial correlation occurs among Fe, Ni, and Pt, and also among Os, Ru, and Mo. SAED patterns show that the Fe-Ni-Pt, Fe-Os-Mo-Ru and Fe-Pt regions are crystalline. Discussion: CAIs can contain various types of inclusions rich in Fe, Ni and refractory siderophiles such as Os, Ru, W and Pt [1]. RMNs are micron-sized, single phase alloy grains and can contain Os, Ir, Ru and Rh [1,7,17]. NLOs are also micron-sized inclusions, but contain two phases, a refractory metal, and an oxide [6]. Fremdlinge are the largest of such inclusions (tens of microns in size) and are complex aggregates of Fe-Ni alloy, silicates, oxides, and sulfides [1,17]. While the size of Spud matches previous descriptions of RMNs and NLOs, Spud is neither a single-phase alloy like RMNs, nor does it contain one metal phase and one oxide like NLOs. Spud does not match the above described categories of refractory metal inclusions. The presence of refractory siderophiles such as Mo, Os, Ru, and Pt suggests a high-temperature origin. Thermodynamic modelling by [7] indicates condensation temperatures of 1917 K, 1693 K, 1613 K and 1415 K for Os, Mo, Ru and Pt respectively. These models also show that following the initial condensation of a refractory metal, alloying of solutes such as Fe, Ni and W, occurs in levels proportional to their partial pressures in the surrounding gas. Such alloying occurs at temperatures above the condensation temperatures of common CAI phases such as melilite (1529 K), perovskite (1441 K), spinel (197 K) and forsterite (1354 K) [2]. The polyphasic nature of Spud could be the result of such high-temperature alloying, possibly shortly after the condensation of Mo and Ru at 1693 K and 1613 K respectively. That Spud occurs as an inclusion is consistent with it having formed prior to and at temperature above that of its host melilite in this FTA CAI, which is qualitatively consistent with such prior thermodynamic modeling. Further, the polyphasic nature of Spud is similar to refractory grains from a FTA CAI in the Northwest Africa (NWA) 8323, CV3 chondrite [11-13]. These data suggest that such refractory metal grains could have been widespread in the inner and early solar protoplanetary disk and represent some of the earliest formed solids to have condensed. Acknowledgments: Research and instrumentation supported by NASA grants #NNX12AL47G, #NNX15AJ22G and #80NSSC19K0509, and NSF grants #1531243 and #0619599. Fig 2. STEM data on ‘Spud’. HAADF Image (Top) False-color EDS Maps (Bottom) References: [1] MacPherson G. J. (2014) T. of Geochem. Vol I: Met. And Cosmochem. Processes, 139-179. [2] Lodders K. (2003) ApJ, 591, 1220-1247. [3] Ebel D. S. (2006) Met. & the Early S. Sys. II., 253- 277. [4] Amelin Y. (2002) Science, 297, 1678-1683. [5] Connelly J.N. et.al. (2012) Science, 338, 651-655. [6] Schwander D. et al. (2015) GCA, 18, 70-87. [7] Palme H. and Wlotzka F. (1976) EPSL, 33, 45-60. [8] Berg T. et al. (2009) ApJ, 702, 172-176. [9] Liffman K. et al. (2021) Icarus, 221, 89-105. [10] Zega T.J. et al. (2021) PSJ, 2, 115. [11] Ramprasad T. et al. (2020) LPSC LI, Abstract #2472. [12] Ramprasad T. et al. (2021) Microscopy & Microanalysis, S1, 2792-2794. [13] Ramprasad T. et al. (2021) 84th MetSoc, Abstract #6123. [14] Zega T.J. et al. (2007) MAPS, 42, 1373-1386. [15] Ramprasad T. et al. (2022) MAPS, in revision. [16] Grossman L. (1975), GCA, 39, 433-454. [17] El Goresy A. et al. (1978) LPSC IX, Abstract#1100

T. Ramprasad↗
NASA NTRS2024

Investigating Space Weathering of Ryugu Grains Using Electron Microscopy and X-Ray Computed Tomography

The effects of micrometeorite bombardment and solar wind ion irradiation – collectively known as space weathering – alter the microstructural, chemical, and spectral properties of airless surfaces. Characteristics of space weathering include vesiculated textures, amorphous grain rims (upper ~100 nm), and the production of Fe-bearing nanoparticles (npFe). The resulting modifications in the optical properties of the surface regolith include changes in spectral slope and overall reflectance of the surfaces as well as the attenuation of their characteristic absorption bands across VIS-NIR wavelengths. As the surface is continuously exposed to interplanetary space over time, the accrual of these features complicates the interpretation of remote sensing spectral data and the characterization of returned samples. Laboratory experiments that simulate solar wind irradiation and micrometeoroid impacts using carbonaceous analogs have revealed novel and complex microstructural and chemical changes, including the decrease in organic species concentrations and the reduction of Fe 3+ . In 2020, the Japan Aerospace Exploration Agency (JAXA)’s Hayabusa2 mission returned over 5 g of regolith particles from near- Earth C-type asteroid (162173) Ryugu – a unique opportunity to study space weathering on carbonaceous materials. Initial studies have established that the surface morphology and chemical signatures of space weathering in returned samples share characteristics with laser irradiation experiments simulating micrometeoroid bombardment, indicating that impacts are a significant space weathering mechanism operating on Ryugu. Here, we seek to improve our understanding of space weathering of carbonaceous asteroidal regolith grains by characterizing its effects directly on returned samples to determine the nature of space weathering on Ryugu. To do so, we performed coordinated analyses using electron beam techniques and X-ray computed tomography (XCT) to examine the effects of space weathering on grains returned from the surface of Ryugu by the Hayabusa2 mission.

L. E. Melendez↗
DOE OSTI2024

Fracture behavior of irradiation induced nanocrystalline UO 2 studied by in-situ mechanical testing in transmission electron microscopy

Uranium Dioxide (UO 2 ) is widely used as a fuel in current light water reactors (LWRs). Upon accumulation of radiation damage, LWR UO 2 fuel pellets start to develop a different microstructure at the pellet periphery when fuel burnup exceeds 45–50 GWd/tHM. The resulting porous, nanocrystalline microstructure is one of the most prominent microstructural changes occurring in such fuel. Its fracture mechanisms, which causes fuel fine fragmentation, could impact safety limits when the cladding breaches. Direct measurements of these properties are challenging, therefore a surrogate obtained via ion irradiation can be used. In this study, multiple microcantilevers were fabricated by focused ion beam from both fresh UO 2 and UO 2 irradiated with 84 MeV Xe 26+ ions to a peak dose of 1357 displacements per atom (dpa). Further, the irradiation produced a pseudo high burnup structure approximately 2 µm below the surface. In-situ nano-mechanical bending tests were conducted to investigate the fracture behavior and the effect of the surrogate UO 2 high burnup structure on local fracture properties. Fresh UO 2 fuel was observed to fracture in transgranular mode without nucleation or movement of dislocations. However, the Xe-irradiated nanocrystalline microcantilevers fractured along the grain boundaries, with no influence from the pre-existing micro-cracks in the microcantilever. Fracture toughness for this type of surrogate high burnup UO 2 structure is reported for the first time in literature. Both the fracture stress and toughness show degradation for UO 2 as a result of Xe-irradiation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗