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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 379 records · Page 21

GraphEM

An unsupervised segmentation method for structural analysis of Scanning Transmission Electron Microscopy (STEM) images

Pope, Jenna↗

Influence of Process Parameter and Build Rate Variations on Defect Formation in Laser Powder Bed Fusion SS316L

Laser powder bed fusion (LPBF) is an additive manufacturing process that has gained interest for its material fabrication due to multiple advantages, such as the ability to print parts with small feature sizes, good mechanical properties, reduced material waste, etc. However, variations in the key process parameters in LPBF may result in the instantiation of porosity defects and variation in build rate. Particularly, volumetric energy density (VED) is a variable that encapsulates a number of those parameters and represents the amount of energy input from the laser source to the feedstock. VED has been traditionally used to inform the quality of the printed part but different values of VED are presented as optimal values for certain material systems. An optimal VED value can be maintained by changing the key process parameters so that various combinations yield a constant value. In this study, an optimal constant VED value is maintained while printing SS316L with variable key processing parameters. Porosity analysis is performed using optical microscopy, as well as X-ray computed tomography, to reveal the volume density and distribution of those pores. Two primary defect categories are identified, namely lack of fusion and porosity induced by balling defects. The findings indicate that, even at optimal VED, variations in process parameters can significantly influence defect type, underscoring the sensitivity of defect formation to the variation of these parameters. Furthermore, a minor change in the build rate, driven by adjustments in process parameters, was found to influence defect categories. These findings emphasize that fine tuning the process parameters and build rate is essential to minimize defects. Finally, fiducial marks have been identified as a source of unintentional porosity defects. These results enable the refinement of process parameters, ultimately optimizing LPBF to achieve enhanced material density and expedite the printing.

36 MATERIALS SCIENCE↗

Field Emission Properties of Cu-Filled Vertically Aligned Carbon Nanotubes Grown Directly on Thin Cu Foils

Copper-filled vertically aligned carbon nanotubes (Cu@VACNTs) were grown directly on Cu foil substrates of 0.1 mm thicknesses at different temperatures via plasma-enhanced chemical vapor deposition (PECVD). By circumventing the need for additional catalyst layers or intensive substrate treatments, our in-situ technique offers a simplified and potentially scalable route for fabricating Cu@VACNTs with enhanced electrical and thermal properties on thin Cu foils. Comprehensive analysis using field emission scanning microscopy (FESEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS) mappings, and X-ray diffraction (XRD) revealed uniform Cu filling within the VACNTs across a range of synthesis temperatures (650 °C, 700 °C, and 760 °C). Field emission (FE) measurements of the sample synthesized at 700 °C (S700) showed low turn-on and threshold fields of 2.33 V/μm and 3.29 V/μm, respectively. The findings demonstrate the viability of thin Cu substrates in creating dense and highly conductive Cu-filled VACNT arrays for advanced electronic and nanoelectronics applications.

36 MATERIALS SCIENCE↗

Fluid inclusions in quartz crystals from South-West Africa.

Quartz crystals from calcite veins of unknown age in Precambrian metasedimentary rocks at Geiaus No. 6 and Aukam farms in South-West Africa contain both primary and secondary inclusions filled with one substance or a combination of substances. These substances include organic liquid, moderately saline aqueous liquid, dark-colored solid, and a vapor. Analysis of these materials by microscopy and by gas chromatography and mass spectrometry shows the presence of constituents of both low and high molecular weights.

Kvenvolden, K. A.↗

Stress corrosion in titanium alloys and other metallic materials

Multiple physical and chemical techniques including mass spectroscopy, atomic absorption spectroscopy, gas chromatography, electron microscopy, optical microscopy, electronic spectroscopy for chemical analysis (ESCA), infrared spectroscopy, nuclear magnetic resonance (NMR), X-ray analysis, conductivity, and isotopic labeling were used in investigating the atomic interactions between organic environments and titanium and titanium oxide surfaces. Key anhydrous environments studied included alcohols, which contain hydrogen; carbon tetrachloride, which does not contain hydrogen; and mixtures of alcohols and halocarbons. Effects of dissolved salts in alcohols were also studied. This program emphasized experiments designed to delineate the conditions necessary rather than sufficient for initiation processes and for propagation processes in Ti SCC.

Harkins, C. G.↗

Effect of magnesium oxide content on oxidation behavior of some superalloy-base cermets

The effect of increasing magnesium oxide (MgO) content on the cyclic oxidation resistance of hot-pressed cermets of MgO in NiCrAlY, MgO in Hoskins-875, MgO in Inconel-702, and MgO in Hastelloy-X was investigated. The cermets with magnesium oxide levels of 5, 10, 20, and 40 vol percent were examined. The cyclic oxidation behavior of these cermets at 1100 and 1200 C in still air was determined by a thermogravimetric method supplemented by X-ray diffraction analysis and light and electron microscopy. In all instances, MgO prevented grain growth in the metallic phase. No evidence of oxidation along interphase boundaries was detected. Cermets of MgO in NiCrAlY and MgO in Hoskins-875 were superior to cermets of MgO in Inconel-702 and MgO in Hastelloy-X. Their oxidation resistance was degraded only when the MgO content was 40 vol percent. The oxidation behavior of MgO-in-Inconel-702 powder cermets containing 5- and 10-vol percent MgO was approximately similar to that of pure Inconel-702 compacts. The 20- and 40-vol percent MgO content reduced the oxidation resistance of MgO-in-Inconel-702 powder cermets relative to that of pure Inconel-702.

Zaplatynsky, I.↗

Erosion/corrosion of turbine airfoil materials in the high-velocity effluent of a pressurized fluidized coal combustor

Four candidate turbine airfoil superalloys were exposed to the effluent of a pressurized fluidized bed with a solids loading of 2 to 4 g/scm for up to 100 hours at two gas velocities, 150 and 270 m/sec, and two temperatures, 730 deg and 795 C. Under these conditions, both erosion and corrosion occurred. The damaged specimens were examined by cross-section measurements, scanning electron and light microscopy, and X-ray analysis to evaluate the effects of temperature, velocity, particle loading, and alloy material. Results indicate that for a given solids loading the extent of erosion is primarily dependent on gas velocity. Corrosion occurred only at the higher temperature. There was little difference in the erosion/corrosion damage to the four alloys tested under these severe conditions.

Zellars, G. R.↗

Airborne particle monitoring by electrostatic precipitation

For qualitative analysis of atmospheric particulates by microscopy, the sampling device should preserve the particles in the state existing at the moment of capture. A collector is described that uses electrostatic precipitation to capture and disperse specimens on various substrates for direct insertion into microscopes. Sampling runs in various atmospheres are described. Micrographs are presented to show particle morphology and distribution on the substrates. Chemical identification by X-ray energy probe and electron diffraction is illustrated.

Robinson, J. C.↗

Wear of aluminum and hypoeutectic aluminum-silicon alloys in boundary-lubricated pin-on disk sliding

The friction and wear of pure aluminum and a number of hypoeutectic aluminum-silicon alloys (with 3 to 12 wt %Si) were studied with a pin-on-disk apparatus. The contacts were lubricated with mineral oil and sliding was in the boundary-lubrication regime at 2.6 cm/sec. Surfaces were analyzed with photomicrographs, scanning electron microscopy, X-ray dispersive analysis, and diamond pyramid hardness measurements. There were two wear regimes for the alloys - high and low - whereas pure aluminum exhibited a high wear rate throughout the test period. Wear rate decreased and the transition stress from high to low wear increased with increasing hardness. There was no correlation between friction coefficient and hardness. A least squares curve fit indicated a wear-rate dependence greater than the inverse first power of hardness. The lower wear rates of the alloys may be due to the composites of silicon platelets in aluminum resulting in increased hardness and thus impairing the shear of the aluminum.

Ferrante, J.↗

Vapor phase diamond growth technology

Ion beam deposition chambers used for carbon film generation were designed and constructed. Features of the developed equipment include: (1) carbon ion energies down to approx. 50 eV; (2) in suit surface monitoring with HEED; (3) provision for flooding the surface with ultraviolet radiation; (4) infrared laser heating of substrate; (5) residual gas monitoring; (6) provision for several source gases, including diborane for doping studies; and (7) growth from either hydrocarbon source gases or from carbon/argon arc sources. Various analytical techniques for characterization of from carbon/argon arc sources. Various analytical techniques for characterization of the ion deposited carbon films used to establish the nature of the chemical bonding and crystallographic structure of the films are discussed. These include: H2204/HN03 etch; resistance measurements; hardness tests; Fourier transform infrared spectroscopy; scanning auger microscopy; electron spectroscopy for chemical analysis; electron diffraction and energy dispersive X-ray analysis; electron energy loss spectroscopy; density measurements; secondary ion mass spectroscopy; high energy electron diffraction; and electron spin resonance. Results of the tests are summarized.

Angus, J. C.↗

Deep-sea spherules from Pacific clay - Mass distribution and influx rate

From 411 kg of Pacific clay, 22 mg of stony spherules and 50 mg of iron spherules larger than 150 microns were concentrated. The extraterrestrial origin of these particles was evaluated with the aid of optical and electron microscopy and atomic absorption elemental analysis. An expression for the integral number of stony particles from this sediment in the mass range 20-300 micrograms was derived. The world-wide influx rate of stony particles in the mass range which survive atmospheric heating and ocean sediment storage is calculated to be 90 tons/yr. The relative contributions of ablation debris vs fused interplanetary dust to the influx of stony spherules is discussed, but no conclusions could be made.

Murrell, M. T.↗

Metallic minerals, thermal histories and parent bodies of some xenolithic, ordinary chondrite meteorites

The metal grains were investigated in the hosts and lithic fragments of various petrologic types in four xenolithic chondrites using reflected-light microscopy and electron-probe analysis. The kamacite, taenite, tetrataenite, and troilite in Weston and Fayetteville have many textures; on a Wood plot of the central Ni content vs dimensions, the taenite content shows scatter if metal grains had cooled at rates of 10-1000 and 1-100 K/Myr through 700 K. In contrast, metallic minerals in Bhola and Mezo-Madaras have uniform textures and plot coherently, indicating cooling rates of 0.1 and 1 K/Myr, respectively, in the 700-600 K range. It is concluded that the host and xenoliths in these chondrites were cooled slowly after compaction; their clasts underwent peak metamorphic temperatures and slow cooling through 700 K in different environments.

Scott, E. R. D.↗

Chemical and morphological characteristics of lithium electrode surfaces

Lithium electrode surfaces were analyzed for chemical and morphological characteristics, using electron spectroscopy chemical analysis (ESCA) and scanning electron microscopy (SEM). Samples included lithium metal and lithium electrodes which were cycled in a 1.5 M lithium arsenic hexafluoride/two-methyl tetrahydrofuran electrolyte. Results show that the surface of the as-received lithium metal was already covered by a film composed of LiO2 and an Li2O/CO2 adduct with a thickness of approximately 100-200 A. No evidence of Ni3 was found. Upon exposure of the lithium electrode to a 1.5 M LiAsF6/2-Me-THF electrochemical environment, a second film was observed to form on the surface, consisting primarily of As, Si, and F, possibly in the form of lithium arsenic oxyfluorides or lithium fluorosilicates. It is suggested that the film formation may be attributed to salt degradation.

Yen, S. P. S.↗

The effects of electron and gamma radiation on epoxy-based materials

Specimens of graphite/epoxy composites and epoxy resins were exposed to electron and gamma radiation, followed by mechanical property and fundamental measurements. Measurement techniques included: scanning electron microscopy, X-ray diffraction analysis, and electron spin resonance spectroscopic analysis. Results indicate little or no change in flexural properties of miniature specimens of a graphite/epoxy composite and no change in failure mode at the fiber-resin interface and in the crystallinity of the fiber and the resin. Some doubt in the observation of stable flexural properties is cast by electron paramagnetic resonance spectra of a relatively large number of radiation-generated radicals. These generally lead to a change in cross-linking and in chain-scissioning which should alter mechanical properties.

Fornes, R. E.↗

Radiative properties of advanced spacecraft heat shield materials

Experimental results are presented to show the effects of simulated reentry exposure by convective heating and by radiant heating on spectral and total emittance of statically oxidized Inconel 617 and Haynes HS188 superalloys to 1260 K and a silicide coatea (R512E) columbium 752 alloy to 1590 K. Convective heating exposures were conducted in a supersonic arc plasma wind tunnel using a wedge-shaped specimen configuration. Radiant tests were conducted at a pressure of .003 atmospheres of dry air at a flow velocity of several meters per second. Convective heating specimens were subjected to 8, 20, and 38 15-min heating cycles, and radiant heating specimens were tested for 10, 20, 50, and 100 30-min heating cycles. Changes in radiative properties are explained in terms of changes in composition resulting from simulated reentry tests. The methods used to evaluate morphological, compositional and crystallographic changes include: Auger electron spectroscopy; scanning electron microscopy; X-ray diffraction analysis; and electron microprobe analysis.

Cunnington, G. R.↗

A three-dimensional study of metal grains in equilibrated, ordinary chondrites

Metal particles in Guarena (H6), Colby (L6) and St. Severin (LL6) were studied by optical microscopy and by electron microprobe analysis. Observations from successive polished sections through the metal particles show that kamacite and taenite grains, which often appear to be isolated particles, are connected directly or by intervening sulfides. Also tetrataenite rims are widest when adjacent to sulfide or kamacite. These observations indicate that transfer of Ni during cooling when kamacite-taenite phase growth takes place does not occur through the silicate phases but proceeds through metal and sulfide phases or along grain boundaries. By utilizing the central Ni content of taenite grains from successive sections, metallographic cooling rates were determined more precisely than by using one arbitrary section. Cooling rates determined in this manner for Guarena, Colby, and St. Severin are 4.3 K, 4.0 K, and 1.0 K per million years, respectively.

Willis, J.↗

Melting, ablation, and vapor phase condensation during atmospheric passage of the Bjurbole meteorite

A detailed study of the Bjurbole fusion crust using scanning electron microscopy (SEM) and energy dispersive analysis (EDS) shows that filamentary crystals and ablation spheres may form on the meteoroid surface. Filamentary crystals, hollow spheres, and porous regions of the surface point to a period of intense vapor phase activity during atmospheric passage. Filamentary crystals can be divided into three categories on the basis of bulk composition and morphology. Two types of filamentary crystals are vapor phase condensation products formed during atmospheric entry of the meteoroid. The other type forms by the interaction of seawater with the fusion surface. The density and composition of ablation spheres varies with the flight orientation of the meteorite. The size range and composition of iron-nickel spheres on the surface of Bjurbole are similar to spheres collected in the stratosphere. A comparison of stratospheric dust collections with meteorite surfaces may provide further insight into the mechanisms of meteoroid entry into planetary atmospheres.

Rietmeijer, F. J. M.↗