Search NASASearch

SEARCH · Search NASA

Results for “Scanning Transmission Electron Microscopy”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 19 records

Methods of analyzing microsize particulate aerosols and contaminants.

Methods for analyzing atmospheric aerosols and particulate contaminants from natural and industrial sources are briefly described. Their development was spurred by interest in cosmic dust investigations. These methods make it possible to analyze individual particles ranging in size from 0.01 to 1000 microns for elemental and mineralogical content. The described methods include transmission electron microscopy, scanning electron microscopy, electron probe microanalysis, X-ray diffraction, optical mineralogy, and density measurement.

Blanchard, M. B.

The response of single human cells to zero gravity

The SO15 experiment was designed to extend observations of the effects of zero-gravity to living human cells during and subsequent to a 59-day flight on Skylab 3. A strain of diploid human embryonic lung cells, WI-38, was chosen for this purpose. The studies were concerned with observations designed to detect the effects of zero-gravity on cell growth rates and on cell structure as observed by light microscopy, transmission and scanning electron microscopy and histochemistry. Studies of the effects of zero-gravity on the cell function and the cell cycle were performed by time lapse motion picture photography and microspectrophotometry. Subsequent study of the returned living cells included karotyping, G- and C-banding, and analyses of the culture media used. Some of the living cells returned were banked by deep freeze techniques for possible future experiments.

Montgomery, P. O., Jr.

Thermochemical Stability of Ca2Yb8(SiO4)6O2 Apatite in Presence of Molten Calcium-Magnesium-Aluminosilicate (CMAS)

Thermochemical stability of ytterbium silicon oxyapatite Ca 2 Yb 8 (SiO 4 ) 6 O 2 (CYbS) in the presence of molten calcium-magnesium aluminosilicate (CMAS) has been investigated at elevated temperatures for consideration as a thermal and environmental barrier coating (T/EBC) material. CYbS apatite powder was synthesized from the constituent oxides via a solid-state reaction method. Hot-pressed apatite substrates were exposed to molten CMAS at 1200, 1300, and 1400 °C for 1, 10, and 50 h. Development of phases in the interaction region of the heat-treated specimens was monitored using scanning electron microscopy, transmission electron microscopy, high-angle annular dark-field imaging, selected area electron diffraction, and energy dispersive x-ray spectroscopy. Monoclinic cyclosilicate Ca 3 Yb 2 (Si 3 O 9 ) 2 formed from interaction of CYbS apatite with CaO in the CMAS melt at the apatite-CMAS reaction front and continued to nucleate and grow within the residual CMAS in diffusion couples annealed for 1 to 50 h at 1200 °C as well as in those heat treated at 1300 °C for 1 h. Residual CMAS was depleted of Ca when cyclosilicate was present. Dendritic wollastonite (CaSiO3) was observed within the residual CMAS in couples annealed at 1200 and 1300 °C. Ingress of molten CMAS, because of its exponential decrease in viscosity, occurred through open pores and along the grain boundaries of the apatite substrates without any detectable chemical reaction at 1300 and 1400 °C. Results of this study indicate that Ca 2 Yb 8 (SiO 4 ) 6 O 2 apatite has the potential to mitigate the CMAS corrosion up to about 1200 °C but not at higher temperatures.

Narottam P Bansal

Sporulation and ultrastructure in a late Proterozoic cyanophyte - Some implications for taxonomy and plant phylogeny

Electron microscopical studies of a morphologically diverse, coccoid, presumably late Proterozoic blue-green alga are here reported. They show, together with light microscopy, that the form studied is widespread in the Cordilleran geosyncline, extend the record of well-defined endosporangia perhaps 700 million years into the past, and reveal previously unrecorded ultrastructural details. Coming from northeastern Utah, southwestern Alberta, and east central Alaska, these minute fossils belong to the recently described, morphologically diverse taxon Sphaerocongregus variabilis Moorman, are related to living entophysalidaceans, and have affinities with both the chroococcalean and chamaesiphonalean cyanophytes. Included in the morphological modes displayed by this alga are individual unicells, coenobial clusters of unicells, and a range of endosporangia comparable to those described for living entophysalidaceans. Scanning and transmission electron microscopy reveal that the endospores are commonly embedded in a vesicular matrix, that some of them show what appears to be a bilaminate or perhaps locally multilaminate wall structure, and that some remain together to mature as coenobial clones or 'colonies'. Taxonomic classification and phylogeny are discussed.

Cloud, P.

Microscopic observations of X-ray and gamma-ray induced decomposition of ammonium perchlorate crystals

The X-ray and gamma-ray induced decomposition of ammonium perchlorate was studied by optical, transmission, and scanning electron microscopy. This material is a commonly used oxidizer in solid propellents which could be employed in deep-space probes, and where they will be subjected to a variety of radiations for as long as ten years. In some respects the radiation-induced damage closely resembles the effects produced by thermal decomposition, but in other respects the results differ markedly. Similar radiation and thermal effects include the following: (1) irregular or ill-defined circular etch pits are formed in both cases; (2) approximately the same size pits are produced; (3) the pit density is similar; (4) the c face is considerably more reactive than the m face; and (5) most importantly, many of the etch pits are aligned in crystallographic directions which are the same for thermal or radiolytic decomposition. Thus, dislocations play an important role in the radiolytic decomposition process.

Herley, P. J.

Metallurgical evaluation of factors influencing the ductility of aged T-111

The metallurgical factors influencing the ductility of T-111 (Ta-8W-2Hf) alloy following long-time exposures of GTA welds and tubing in the temperature range 982 C (1800 F) through 1316 C (2400 F) were evaluated by means of scanning and transmission electron microscopy, Auger electron emission spectroscopy, and optical metallographic procedures. No classical aging response occurs in the alloy over the temperature range studied. The ductility impairment implied by previous investigations is not the result of microstructural response of the alloy to thermal exposures. Intergranular failure in the GTA sheet welds appears the result of random contamination by silicon, potassium, and/or fluorine at the grain boundaries of the fusion zones. Exposure to lithium at high temperatures had no adverse effects on the ductility of T-111 tubing. These materials were, however, sensitive to post-age handling and testing procedures.

Gold, R. E.

Investigation of high temperature fracture of T-111 and ASTAR-811C

The high temperature deformation and fracture behavior of T-111 and ASTAR-811C were studied over the temperature range 982 to 2205 C (1800 to 4000 F). As-cast and wrought-recrystallized material as well as GTA welds in sheet and plate were evaluated using conventional tensile and creep tests. Post test examinations were performed using optical metallography, scanning electron microscopy and transmission electron microscopy. A high temperature region of reduced ductility, in terms of tensile elongation, was identified for both alloys. The reduction in tensile elongation became more severe with increase in grain size, being near catastrophic for the as-cast specimens. Optical and electron metallography indicated that even for failures at very low total strain, considerable deformation of a very localized nature had occurred prior to fracture.

Gold, R. E.

Some surface characteristics and gas interactions of Apollo 14 fines and rock fragments.

Comprehensive survey of the physical surface characteristics of Apollo 14 fines, two fragments of a breccia (14321), and a crystalline rock (14310). The survey was carried out with optical and both scanning and transmission electron microscopy and by studying the adsorption of a variety of gases including nitrogen, hydrogen, and water vapor. Our objective in the optical microscope study was to relate the visible geological and petrological features to the surface properties. Electron microscopy particularly helped relate surface roughness and particle fusion to gas adsorption and pore structure. The fine sample (14163,111) had a surface area of 0.210 sq m/g and a helium density of 2.9 g/cc. Similar values have been observed with breccia fragments. Other observations include physical adsorption of molecular hydrogen at low temperatures and of water vapor at ambient temperatures. It is concluded that these particular lunar materials, while capable of adsorbing water vapor, do not retain it for any significant time at low pressures, nor, under lunar conditions, is there any indication of absorption or penetration.

Cadenhead, D. A.

Microstructure of hot-pressed Al2O3-Si3N4 mixtures as a function of holding temperature

Powder mixtures of 40 m/o Si3N4-60 m/o Al2O3 were hot-pressed at 4000 psi at various holding temperatures from 1100 C to 1700 C. Scanning Electron Microscopy and Transmission Electro Microscopy results were correlated to X-ray phase analysis and density measurements. The progressively developed microstructure was used to interpret the densification behavior of SiAlON. Photomicrographs of microstructures are shown.

Yeh, H. C.

Microstructure of hot-pressed Al2O3-Si3N4 mixtures as a function of holding temperature

Powder mixtures of 40 m/o Si3N4-60 m/o Al2O3 were hot-pressed at 4000 psi at various holding temperatures from 1100 C to 1700 C. Scanning and transmission electron microscopy results were correlated to X-ray phase analysis and density measurements. The progressively developed microstructure was used to interpret the densification behavior of SiAlON.

Yeh, H. C.

Otoconial formation in the fetal rat

Otoconial formation in the fetal rat is examined by scanning and transmission electron microscopy, and by X-ray elemental analysis. The primitive otoconia appear highly organic, but are trigonal in cross section, indicating that they already possess a three-fold axis of symmetry and a complement of calcite. These otoconia develop into spindle-shaped and, subsequently, dumbbell-shaped units. Transmission electron microscopy of dumbbell-shaped otoconia not exposed to fluids during embedment showed that calcite deposits mimicked the arrangement of the organic material. X-ray elemental analysis demonstrated that calcium was present in lower quantities in the central core than peripherally. It is concluded that organic material is essential to otoconial seeding and directs otoconial growth.

Salamat, M. S.

Microstructural Evolution and Mechanical Properties of LP-DED NASA HR-1 – A Hydrogen Resistant AM Superalloy for Space Propulsion Applications

The National Aeronautics and Space Administration (NASA) has actively pursued metal additive manufacturing (AM) technologies for spaceflight applications since the late 2000s. AM offers transformative advantages in cost, schedule, part consolidation, and design flexibility. Among the various AM techniques, laser powder directed energy deposition (LP-DED) is particularly well suited for fabricating complex geometries with fine feature resolution. In propulsion systems that utilize high-pressure gaseous hydrogen—such as liquid hydrogen rocket engines—hydrogen environment embrittlement (HEE) presents a serious threat to material performance 1,2 . Mechanical property degradation under these conditions can compromise component reliability, especially under cyclic loading. To address this challenge, NASA developed NASA HR-1 (Hydrogen Resistant-1) as a solution for liquid rocket engine components operating in hydrogen-rich environments, using the LP-DED technique 3-9 . A key component in a liquid rocket engine is the exhaust nozzle, which is typically regeneratively cooled (regen) due to the high heat flux. NASA HR-1 was specifically developed for regen nozzle applications using hydrogen as a propellant, providing resistance to HEE, a critical issue for many materials. The AM version of NASA HR-1 was also formulated to achieve high ultimate tensile strength, along with high yield strength and ductility in this environment 5,6 . Low-cycle fatigue (LCF) is another important consideration in nozzle design, as components are expected to endure multiple starts and missions. Additionally, the LP-DED version of the alloy exhibits improved thermal conductivity compared to its wrought counterpart, which benefits nozzle cooling. Overall, NASA HR-1 offers an excellent balance of high strength, HEE resistance, LCF performance, thermal conductivity, and ductility to meet the demanding requirements of channel-cooled nozzles and other components used with hydrogen and other propellants. The LP-DED–processed NASA HR-1 requires several post-processing heat treatment steps to achieve the material properties desirable for its intended application 6 . These steps include stress relief, homogenization, solution annealing, and aging for precipitation hardening. The stress relief treatment mitigates residual stresses accumulated during the LP-DED process and minimizes the potential for distortion. Homogenization, a common step for AM materials, reduces elemental segregation and promotes recrystallization to develop a more equiaxed grain structure. The subsequent solution annealing treatment heats the part to a solid solution temperature to dissolve the undesirable η-phase that forms during cooling from homogenization, followed by rapid cooling to retain an η-phase–free microstructure. Finally, aging promotes precipitation of the strengthening γ′ phase in the alloy. The integration of compositional design and optimized thermal processing enables high-quality LP-DED NASA HR-1 components with excellent microstructural and mechanical stability. Improved chemical and microstructure homogeneity enhances ductility and fatigue resistance—both critical for safe and reliable operation in high-pressure hydrogen environments. NASA has successfully fabricated and hot-fire tested multiple subscale and full-scale channel wall nozzles using LP-DED NASA HR-1 5,6, 9-14 . These efforts included process refinements to support thin-wall construction and various channel geometries. Throughout development, several key observations emerged. After homogenization, the as-built columnar grain structure transforms into a fully equiaxed microstructure. However, subsequent treatments—such as solution annealing and aging—result in changes that are more difficult to track. The grain structure remains largely unchanged, and the γ′ precipitates, typically 5–10 nm in diameter, are beyond the resolution of scanning electron microscopy (SEM). While transmission electron microscopy (TEM) can resolve these fine precipitates, TEM sample preparation is time-consuming and difficult for LP-DED material. As an alternative, differential scanning calorimetry (DSC) offers a useful, qualitative approach to monitor precipitate evolution throughout different stages of heat treatment. The overall goal is to improve the understanding of how heat treatment affects the microstructure and mechanical performance of LP-DED NASA HR-1. This paper presents heat treatment design considerations, microstructural characterization, mechanical testing – including tensile and LCF testing in both air and hydrogen environments.

Superalloy

Lubrication with sputtered MoS2 films.

Sputtered MoS2 films (2000-6500 A) were deposited on highly polished metal surfaces. These films have a low coefficient of friction (0.03-0.04) at speeds of 40-80 rpm and loads of 250-1000 grams. At loads of 250 grams the wear lives are over 0.5 million cycles, but at 1000 gram loads, it decreases to 38,000 cycles. Friction experiments and tensile tests have indicated that sputtered films have a strong adherence to metal surfaces. Electron transmission, diffraction and scanning electron microscopy show that these films have an extremely small particle size, less than 30 A in diameter, and are very dense and free from observable pinholes. The high kinetic energy of these sputtered species, the submicroscopic particle size and the sputter-etched substrate surface is responsible for strong adhesion and cohesion of the sputtered film.

Spalvins, T.

Lubrication with sputtered MoS2 films.

Sputtered MoS2 films (2000-6500 A) were deposited on highly polished metal surfaces. These films have a low coefficient of friction (0.03-0.04) at speeds of 40-80 rpm and loads of 250-1000 grams. At loads of 250 grams, the wear lives are over 0.5 million cycles, but at 1000 gram loads, it decreases to 38,000 cycles. Friction experiments and tensile tests have indicated that sputtered films have a strong adherence to metal surfaces. Electron transmission, diffraction, and scanning electron microscopy show that these films have an extremely small particle size less than 30 A in diameter and are very dense and free from observable pinholes.

Spalvins, T.

Avoidance of stress corrosion susceptibility in high strength aluminum alloys by control of grain boundary and matrix microstructure

The relation of microstructure to the mechanical strength and stress corrosion resistance of highest strength and overaged tempers of BAR and 7050 aluminum alloys was investigated. Comparison is made with previously studied 7075 aluminum alloy. Optical microscopy, transmission electron microscopy, and differential scanning calorimetry were used to characterize the grain morphology, matrix microstructure, and grain boundary microstructure of these tempers. Grain boundary interparticle spacing was significant to stress corrosion crack propagation for all three alloys; increasing interparticle spacing led to increased resistance to crack propagation. In addition, the fire grain size in Bar and 7050 appears to enhance crack propagation. The highest strength temper of 7050 has a comparatively high resistance to crack initiation. Overall stress corrosion behavior is dependent on environment pH, and evaluation over a range of pH is recommended.

Adler, P.

Morphological growth of sputtered MoS2 films

Sputtered MoS2 films from 300 A to 20,000 A thick were deposited on metal and glass surfaces. The substrate effects such as surface temperature, finish, pretreatment and chemistry as they affect the film formation characteristics were investigated by optical, electron transmission, electron diffraction, and scanning electron microscopy. Substrate temperature and surface chemistry were found to be the prime variables as to the formation of a crystalline or amorphous film. The friction characteristics are strictly influenced by the type of film formed. Surface chemistry and surface pretreatment account for compound formation and corresponding grain growth, which directly affect the adhesion characteristics, resulting in poor adherence. The type of surface finish (topography) as related to scratches, impurities, inhomogeneities, etc., are favorable nucleation sites for the growth of isolated and complex nodules within the film, and various complex surface overgrowths on the film. These nodular growth features have progressively more undesirable effects on the film behavior as the film thickness increases.

Spalvins, T.

Morphological growth of sputtered MoS2 films

Sputtered MoS2 films from 300 A to 20,000 A thick were deposited on metal and glass surfaces. The substrate effects such as surface temperature, finish, pretreatment, and chemistry as they affect the film formation characteristics were investigated by optical, electron transmission, electron diffraction, and scanning electron microscopy. Substrate temperature and surface chemistry were found to be the prime variables as to the formation of a crystalline or amorphous film. The friction characteristics are strictly influenced by the type of film formed. Surface chemistry and surface pretreatment account for compound formation and corresponding grain growth, which directly affect the adhesion characteristics, resulting in poor adherence. Scratches, impurities, inhomogeneities, etc., are favorable nucleation sites for the growth of isolated and complex nodules within the film.

Spalvins, T.

Microstructural and wear properties of sputtered carbides and silicides

Sputtered Cr3C2, Cr3Si2, and MoSi2 wear-resistant films (0.05 to 3.5 microns thick) were deposited on metal and glass surfaces. Electron transmission, electron diffraction, and scanning electron microscopy were used to determine the microstructural appearance. Strong adherence was obtained with these sputtered films. Internal stresses and defect crystallographic growth structures of various configurations within the film have progressively more undesirable effects for film thicknesses greater than 1.5 microns. Sliding contact and rolling element bearing tests were performed with these sputtered films. Bearings sputtered with a duplex coating (0.1-micron-thick undercoating of Cr3Si2 and subsequently 0.6-micron coating of MoS2) produced marked improvement over straight MoS2 films.

Spalvins, T.