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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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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.↗

Surface Chemistry, Friction, and Wear Properties of Untreated and Laser-Annealed Surfaces of Pulsed-Laser-Deposited WS(sub 2) Coatings

An investigation was conducted to examine the surface chemistry, friction, and wear behavior of untreated and annealed tungsten disulfide (WS2) coatings in sliding contact with a 6-mm-diameter 440C stainless-steel ball. The WS2 coatings and annealing were performed using the pulsed-laser-deposition technique. All sliding friction experiments were conducted with a load of 0.98 N (100 g), an average Hertzian contact pressure of 0.44 GPa, and a constant rotating speed of 120 rpm. The sliding velocity ranged from 31 to 107 mm/s because of the range of wear track radii involved in the experiments. The experiment was performed at room temperature in three environments: ultrahigh vacuum (vacuum pressure, 7X(exp -10) Pa), dry nitrogen (relative humidity, less than 1 percent), and humid air (relative humidity, 15 to 40 percent). Analytical techniques, including scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDX), x-ray photo electron spectroscopy (XPS), surface profilometry, and Vickers hardness testing, were used to characterize the tribological surfaces of WS2 coatings. The results of the investigation indicate that the laser annealing decreased the wear of a WS2 coating in an ultrahigh vacuum. The wear rate was reduced by a factor of 30. Thus, the laser annealing increased the wear life and resistance of the WS2 coating. The annealed WS 2 coating had a low coefficient of friction (less than O.1) and a low wear rate ((10(exp -7) mm(exp 3)/N-m)) both of which are favorable in an ultrahigh vacuum.

Miyoshi, Kazuhisa↗

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.↗

Synthesis and characterization of high-T(sub c) screen-printed Y-Ba-Cu-O films on alumina

Thick films of YBa2Cu3O(sub 7-x) have been deposited on highly polished alumina substrates by the screen printing technique. To optimize the post-printing heat treatment, the films were baked at various temperatures for different lengths of time and oxygen-annealed at a lower temperature. The resulting films were characterized by electrical resistivity measurements, x-ray diffraction, and optical and scanning electron microscopy. Properties of the films were found to be highly sensitive to the post-printing thermal treatment. Films baked for 15 min at 1000 C in oxygen were hard, adherent, near single phase, and superconducting with T(sub c)(onset) approx 96 K, T(sub c)(zero) approx 66 K and Delta T sub c (10 to 90 percent) approx 10 K.

Bansal, Narottam P.↗

Synthesis and characterization of high-T(c) screen-printed Y-Ba-Cu-O films on alumina

Thick films of YBa2Cu3O(sub 7-x) have been deposited on highly polished alumina substrates by the screen printing technique. To optimize the post-printing heat treatment, the films were baked at various temperatures for different lengths of time and oxygen-annealed at a lower temperature. The resulting films were characterized by electrical resistivity measurements, X-ray diffraction, and optical and scanning electron microscopy. Properties of the films were found to be highly sensitive to the post-printing thermal treatment. Films baked for 15 min at 1000 C in oxygen were hard, adherent, near single phase, and superconducting with T(sub c) (onset) approx 96 KK, T(sub c) (zero) approx 66 K and Delta T sub c (10 to 90 percent) approx 10 K.

Bansal, Narottam P.↗

NASA Work Experience

I have had the opportunity to support the analytical laboratories in chemical analysis of unknown samples, using Optical Microscopy (OM), Polarizing Light Microscopy (PLM), Fourier-Transform Infrared Spectroscopy (FT-IR), Scanning Electron Microscopy with Energy Dispersive Spectroscopy (SEMEDS), and X-ray Powder Diffraction (XPD). I have assisted in characterizing fibers pulled from a spacecraft, a white fibrous residue discovered in a jet refueler truck, brown residue from a plant habitat slated for delivery to the ISS (International Space Station), corrosion on a pipe from a sprinkler, and air filtration material brought back from the ISS. I also conducted my own fiber study in order to practice techniques and further my understanding of background concepts. Furthermore, I had the opportunity to participate in diverse work assignments, where I was assigned to work with other branches of the engineering department for 1-2 days each. The first was in the Materials Science branch where I participated in the construction of the plant habitat intended for use in research aboard the ISS. The second was in the Testing Design branch where I assisted with tensile and hardness testing of over 40 samples. In addition, I have had the privilege to attend multiple tours of the NASA KSC campus, including to the Astronaut Crew Quarters, the VAB (the main area, the Columbia room, and the catwalk), the Visitor Center housing the shuttle Atlantis, the Saturn-V exhibit, the Prototype laboratory, SWAMP WORKS, the Shuttle Landing Facility, the Crawler, and the Booster Fabrication Facility (BFF). Lastly, much of my coursework prepared me for this experience, including numerous laboratory courses with topics diverse as chemistry, physics, and biology.

Florida Tech↗

Methodology for Producing a Uniform Distribution of UO2 in a Tungsten Matrix

Current work at NASA's Marshall Space Flight Center (MSFC) is focused on the development CERMET fuel materials for Nuclear Thermal Propulsion (NTP). The CERMETs consist of uranium dioxide (UO2) fuel particles embedded in a tungsten (W) metal matrix. Initial testing of W-UO2 samples fabricated from fine angular powders performed reasonably well, but suffered from significant fuel loss during repeated thermal cycling due to agglomeration of the UO2 (1). The blended powder mixtures resulted in a non-uniform dispersion of the UO2 particles in the tungsten matrix, which allows rapid vaporization of the interconnected UO2 from the sample edges into the bulk material. Also, the angular powders create areas of stress concentrations due to thermal expansion mismatch, which eventually cracks the tungsten matrix. Evenly coating spherical UO2 particles with chemical vapor deposited (CVD) tungsten prior to consolidation was previously demonstrated to provide improved performance. However, the CVD processing technology is expensive and not currently available. In order to reduce cost and enhance performance, a powder coating process has been developed at MSFC to produce a uniform distribution of the spherical UO2 particles in a tungsten matrix. The method involves utilization of a polyethylene binder during mixing which leads to fine tungsten powders clinging to the larger UO2 spherical particles. This process was developed using HfO2 as a surrogate for UO2. Enough powder was mixed to make 8 discs (2cm diameter x 8mm thickness) using spark plasma sintering. A uniaxial pressure of 50 MPa was used at four different temperatures (2 samples at each temperature). The first two samples were heated to 1400C and 1500C respectively for 5 minutes. Densities for these samples were less than 85% of theoretical, so the time at temperature was increased to 20 minutes for the remaining samples. The highest densities were achieved for the two samples sintered at 1700C (approx. 92% of theoretical). Scanning electron microscopy (SEM) of the mixed powders and the sintered samples along with energy dispersive x-ray analysis was obtained. The SEM of the powders clearly show the fine W powder adhered to the larger HfO2 particles and a uniform distribution of HfO2 particles in a tungsten matrix upon densification. Vicker's Microhardness testing was also performed on all samples using 0.5, 1.0 and 2.0 kg loads. Five indents were made at each load level. All indents were placed in the tungsten matrix to assist as a proxy in measuring densification. The highest hardness value was obtained for the 1700C specimens. The hardness average for these samples was 312.14 MPa. This powder processing method has been applied to W/UO2 powders with the SEM of the powders appearing similar to the W/HfO2 powder images.

Tucker, Dennis S.↗

Metallographic Preparation of Space Shuttle Reaction Control System Thruster Electron Beam Welds for Electron Backscatter Diffraction

A Space Shuttle Reaction Control System (RCS) thruster failed during a firing test at the NASA White Sands Test Facility (WSTF), Las Cruces, New Mexico. The firing test was being conducted to investigate a previous electrical malfunction. A number of cracks were found associated with the fuel closure plate/injector assembly (Fig 1). The firing test failure generated a flight constraint to the launch of STS-133. A team comprised of several NASA centers and other research institutes was assembled to investigate and determine the root cause of the failure. The JSC Materials Evaluation Laboratory was asked to compare and characterize the outboard circumferential electron beam (EB) weld between the fuel closure plate (Titanium 6Al-4V) and the injector (Niobium C-103 alloy) of four different RCS thrusters, including the failed RCS thruster. Several metallographic challenges in grinding/polishing, and particularly in etching were encountered because of the differences in hardness, ductility, and chemical resistance between the two alloys and the bimetallic weld. Segments from each thruster were sectioned from the outboard weld. The segments were hot-compression mounted using a conductive, carbon-filled epoxy. A grinding/polishing procedure for titanium alloys was used [1]. This procedure worked well on the titanium; but a thin, disturbed layer was visible on the niobium surface by means of polarized light. Once polished, each sample was micrographed using bright field, differential interference contrast optical microscopy, and scanning electron microscopy (SEM) using a backscatter electron (BSE) detector. No typical weld anomalies were observed in any of the cross sections. However, areas of large atomic contrast were clearly visible in the weld nugget, particularly along fusion line interfaces between the titanium and the niobium. This prompted the need to better understand the chemistry and microstructure of the weld (Fig 2). Energy Dispersive X-Ray Spectroscopy (EDS) was used to confirm the chemical composition of the variations in contrast in these areas. Niobium alloys generally require exposure to more aggressive chemical reagents than titanium alloys for etching because of niobium s chemical resistance; therefore, the titanium portion of the sample was etched first. A five second immersion in Kroll s reagent revealed a general microstructure on the titanium portion of the sample; however, the titanium heat affected zone closest to the weld, was over-etched due to higher concentrations of refined grains and an increase in eta-phase. The Kroll s etchant also revealed some microstructure in the weld nugget itself; the niobium portion of the sample remained unetched.

Martinez, James↗

A Novel Microcharacterization Technique in the Measurement of Strain and Orientation Gradient in Advanced Materials

Representation of morphology and evolution of the microstructure during processing and their relation to properties requires proper experimental techniques. Residual strains, lattice distortion, and texture (micro-texture) at the interface and the matrix of a layered structure or a functionally gradient material and their variation are among parameters important in materials characterization but hard to measure with present experimental techniques. Current techniques available to measure changes in interred material parameters (residual stress, micro-texture, microplasticity) produce results which are either qualitative or unreliable. This problem becomes even more complicated in the case of a temperature variation. These parameters affect many of the mechanical properties of advanced materials including stress-strain relation, ductility, creep, and fatigue. A review of some novel experimental techniques using recent advances in electron microscopy is presented here to measure internal stress, (micro)texture, interracial strength and (sub)grain formation and realignment. Two of these techniques are combined in the chamber of an Environmental Scanning Electron Microscope to measure strain and orientation gradients in advanced materials. These techniques which include Backscattered Kikuchi Diffractometry (BKD) and Microscopic Strain Field Analysis are used to characterize metallic and intermetallic matrix composites and superplastic materials. These techniques are compared with the more conventional x-ray diffraction and indentation techniques.

Garmestai, H.↗

Stardust Interstellar Preliminary Examination IV: Scanning Transmission X-Ray Microscopy Analyses of Impact Features in the Stardust Interstellar Dust Collector

We report the quantitative characterization by synchrotron soft X-ray spectroscopy of 31 potential impact features in the aerogel capture medium of the Stardust Interstellar Dust Collector. Samples were analyzed in aerogel by acquiring high spatial resolution maps and high energy-resolution spectra of major rock-forming elements Mg, Al, Si, Fe, and others. We developed diagnostic screening tests to reject spacecraft secondary ejecta and terrestrial contaminants from further consideration as interstellar dust candidates. The results support an extraterrestrial origin for three interstellar candidates: I1043,1,30 (Orion) is a 3 pg particle with Mg-spinel, forsterite, and an iron-bearing phase. I1047,1,34 (Hylabrook) is a 4 pg particle comprising an olivine core surrounded by low-density, amorphous Mg-silicate and amorphous Fe, Cr, and Mn phases. I1003,1,40 (Sorok) has the track morphology of a high-speed impact, but contains no detectable residue that is convincingly distinguishable from the background aerogel. Twenty-two samples with an anthropogenic origin were rejected, including four secondary ejecta from impacts on the Stardust spacecraft aft solar panels, nine ejecta from secondary impacts on the Stardust Sample Return Capsule, and nine contaminants lacking evidence of an impact. Other samples in the collection included I1029,1,6, which contained surviving solar system impactor material. Four samples remained ambiguous: I1006,2,18, I1044,2,32, and I1092,2,38 were too dense for analysis, and we did not detect an intact projectile in I1044,3,33. We detected no radiation effects from the synchrotron soft X-ray analyses; however, we recorded the effects of synchrotron hard X-ray radiation on I1043,1,30 and I1047,1,34.

Dust↗