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At least 37 records · Page 2

Phase analysis of plasma-sprayed zirconia-yttria coatings

Phase analysis of plasma-sprayed 8 wt pct-yttria-stabilized zirconia (YSZ) thermal barrier coatings and powders was carried out by X-ray diffraction. Step scanning was used for increased peak resolution. Plasma spraying of the YSZ powder into water or onto a steel substrate to form a coating reduced the cubic and monoclinic phases with a simultaneous increase in the tetragonal phase. Heat treatment of the coating at 1150 C for 10 h in an Ar atmosphere increased the amount of cubic and monoclinic phases. The implications of these transformations on coating performance and integrity are discussed.

Shankar, N. R.↗

Neutron and X-ray diffraction of plasma-sprayed zirconia-yttria thermal barrier coatings

ZrO2-7.8mol. pct. YO1.5, a fused powder, and ZrO2-8.7mol. pct. YO1.5, a prereacted powder, were plasma-sprayed onto steel substrates. Neutron diffraction and X-ray diffraction of the as-received powder, the powder plasma sprayed into water, as-sprayed coatings, and coatings heat-treated for 10 and 100 h were carried out to study phase transformations and ordering of the oxygen ions on the oxygen sublattice. The as-received fused powder has a much lower monoclinic percentage than does the pre-reacted powder, this resulting in a much lower monoclinic percentage in the coating. Heat treatment increases the percentages of the cubic and monoclinic phases, while decreasing the tetragonal content. An ordered tetragonal phase is detected by the presence of extra neutron diffraction peaks. These phase transformations and ordering will result in volume changes. The implications of these transformations on the performance of partially stabilized zirconia thermal barrier coatings is discussed.

Shankar, N. R.↗

Effect of starting powder characteristics on density, microstructure and low temperature oxidation behavior of a Si3N48w/o Y2O3 ceramic

The densification and oxidation behavior of Si3N4 - 8w/oY2O3 prepared from three commercial starting powders were studied. Bars of SN 402, SN 502, and CP 85/15 were sintered for 3 to 4.5 hours at 1750 C. A second set was hot pressed for 2 hours at 1750 C. The microstructures were studied by transmission electron microscopy and scanning electron microscopy, densities were determined, and the phase compositions were determined by X-ray diffraction. Densification and microstructure were greatly influenced by the starting powder morphology and impurity content. Although SN 402 exhibited the maximum weight lose, the highest sintered and hot pressed densities were obtained with this powder. All powders had both equiaxed and elongated grains. Sintered bars were composed of beta silicon nitride and n-melelite. In contrast, hot pressed bars contained beta silicon nitride, H-phase, and J-phase, but no melelite. Yttria distribution in sintered bars was related to the presence of cation impurities such as Ca, Fe, and Mg. A limited oxidation study at 750 C in air showed no instability in these Si3N4 - 8 w/oY2O3 specimens, regardless of startin powder.

Schuon, S.↗

Effect of substrate surface finish on the lubrication and failure mechanisms of molybdenum disulfide films

An optical microscope was used to study the lubrication and failure mechanisms of rubbed (burnished) MoS2 films applied to three substrate surface finishes - polished, sanded, and sandblasted - as a function of sliding distance. The lubrication mechanism was the plastic flow of thin films of MoS2 between flat plateaus on the rider and on the metallic substrate. If the substrate was rough, flat plateaus were created during 'run-in' and the MoS2 flowed across them. Wear life was extended by increasing surface roughness since valleys in the roughened substrate served as reservoirs for MoS2 and a deposit site for wear debris. In moist air, the failure mechanism was the transformation of metallic-colored MoS2 films to a black, powdery material that was found by X-ray diffraction to consist primarily of alpha-iron and MoO3 powders. In dry argon, the failure mechanism was the gradual depletion of the MoS2 film from the contact region by transverse flow. Analysis of the wear debris on the wear track at failure showed it consisted mainly of alpha-iron and some residual MoS2. No molybdenum oxides were found.

Fusaro, R. L.↗

X-ray investigations related to the shock history of the Shergotty achondrite

The shock stress suffered by naturally shocked materials from the Shergotty achondrite was studied using X-ray diffraction techniques and experimentally shocked augite and enstatite as standards. The Shergotty pyroxenes revealed the formation of continuous diffraction rings, line broadening, preferred orientation of small scale diffraction domains, and other evidence of substantial lattice disorders. As disclosed by the application of Debye-Scherrer techniques, they are hybrids between single crystals and fine-grained random powders. The pyroxene lattice is very resistant to shock damage on smaller scales. While measurable lattice disaggregation and progressive fragmentation occur below 25 GPa, little additional damage is suffered from application of pressures between 30 to 60 GPa, making pressure calibration of naturally shocked pyroxenes via X-ray methods difficult. Powder diffractometer scans on pure maskelynite fractions of Shergotty revealed small amounts of still coherently diffracting plagioclase, which may contribute to the high refractive indices of the diaplectic feldspar glasses of Shergotty.

Horz, F.↗

Silicon nitride-aluminum oxide solid solution (SiAION) formation and densification by pressure sintering

Stirred-ball-mill-blended Si3N4 and Al2O3 powders were pressure sintered in order to investigate the mechanism of solid solution formation and densification in the Si3N4-Al2O3 system. Powder blends with Si3N4:Al2O3 mole ratios of 4:1, 3:2, and 2:3 were pressure sintered at 27.6-MN/sq m pressure at temperatures to 17000 C (3090 F). The compaction behavior of the powder blends during pressure sintering was determined by observing the density of the powder compact as a function of temperature and time starting from room temperature. This information, combined with the results of X-ray diffraction and metallographic analyses regarding solutioning and phase transformation phenomena in the Si3N4-Al2O3 system, was used to describe the densification behavior.

Yeh, H. C.↗

Comparison of the tribological properties of fluorinated cokes and graphites

The friction, wear, endurance life, and surface morphology of rubbed (burnished) fluorinated graphite and fluorinated coke materials were studied. Two different coke powders, a graphitic carbon powder, and a graphite powder were fluorinated and then tribologically investigated. In addition, one of the coke powders was reduced in size before fluorinating to evaluate the effect of a finer particle size on the tribological properties. For comparison, graphite and coke powders which were not fluorinated were also tribologically evaluated. Elemental analysis by emission spectroscopy was performed on each sample to determine the impurity content and X-ray diffraction analysis was performed to determine the crystallinity. Coke was found to have very little lubricating ability, but fluorinated coke did possess good lubricating properties. However, the fluorinated graphite and fluorinated graphitic carbon (which gave equivalent results) gave superior results to those obtained with the fluorinated cokes. No tribological benefit was found for using small versus a larger particle size of coke, at least when evaluated as a rubbed film.

Fusaro, Robert L.↗

Utilization of Space Shuttle External Tank materials by melting and powder metallurgy

The Crucible Melt Extraction Process was demonstrated to convert scraps of aluminum alloy 2219, used in the Space Shuttle External Tank, into fibers. The cast fibers were then consolidated by cold welding. The X-ray diffraction test of the cast fibers was done to examine the crystallinity and oxide content of the fibers. The compressive stress-strain behavior of the consolidated materials was also examined. Two conceptual schemes which would adapt the as-developed Crucible Melt Extraction Process to the microgravity condition in space were finally proposed.

Chern, T. S.↗

Effect of reduced cobalt contents on hot isostatically pressed powder metallurgy U-700 alloys

The effect of reducing the cobalt content of prealloyed powders of UDIMET 700 (U-700) alloys to 12.7, 8.6, 4.3, and 0% was examined. The powders were hot isostatically pressed into billets, which were given heat treatments appropriate for turbine disks, namely partial solutioning at temperatures below the gamma prime solvus and four step aging treatments. Chemical analyses, metallographic examinations, and X-ray diffraction measurements were performed on the materials. Minor effects on gamma prime content and on room temperature and 650 C tensile properties were observed. Creep rupture lives at 650 C reached a maximum at the 8.4% concentration, while at 760 C a maximum in life was reached at the 4.3% cobalt level. Minimum creep rates increased with decreasing cobalt content at both test temperatures. Extended exposures at 760 and 815 C resulted in decreased tensile strengths and rupture lives for all alloys. Evidence of sigma phase formation was also found.

Harf, F. H.↗

X-ray diffraction studies of shocked lunar analogs

The X-ray diffraction experiments on shocked rock and mineral analogs of particular significance to lunar geology are described. Materials naturally shocked by meteorite impact, nuclear-shocked, or artificially shocked in a flat plate accelerator were utilized. Four areas were outlined for investigation: powder diffractometer studies of shocked single crystal silicate minerals (quartz, orthoclase, oligoclase, pyroxene), powder diffractometer studies of shocked polycrystalline monomineralic samples (dunite), Debye-Scherrer studies of single grains of shocked granodiorite, and powder diffractometer studies of shocked whole rock samples. Quantitative interpretation of peak shock pressures experienced by materials found in lunar or terrestrial impact structures is presented.

Hanss, R. E.↗

Effect of W and WC on the oxidation resistance of yttria-doped silicon nitride

The effect of tungsten and tungsten carbide contamination on the oxidation and cracking in air of yttria-doped silicon nitride ceramics is investigated. Silicon nitride powder containing 8 wt % Y2O3 was doped with 2 wt % W, 4 wt % W, 2 wt % WC or left undoped, and sintered in order to simulate contamination during milling, and specimens were exposed in air to 500, 750 and 1350 C for various lengths of time. Scanning electron and optical microscopy and X-ray diffraction of the specimens in the as-sintered state reveals that the addition of W or WC does not affect the phase relationships in the system, composed of alpha and beta Si3N4, melilite and an amorphous phase. Catastrophic oxidation is observed at 750 C in specimens containing 2 and 4 wt % W, accompanied by the disappearance of alpha Si3N4 and melilite from the structure. At 1350 C, the formation of a protective glassy oxide layer was observed on all specimens without catastrophic oxidation, and it is found that pre-oxidation at 1350 C also improved the oxidation resistance at 750 C of bars doped with 4 wt % W. It is suggested that tungsten contamination from WC grinding balls may be the major cause of the intermediate-temperature cracking and instability frequently observed in Si3N4-8Y2O3.

Schuon, S.↗

Study of a columnar grain structure produced in a superalloy by gradient-annealing prealloyed powder extrusions

Annealing in a temperature gradient was used to produce a structure of continuous columnar grains in alloy 713 C made by extrusion of prealloyed powder. The columnar-grained specimens had tensile strengths within plus or minus 5 percent of those of the as-cast alloy at 760 C and 980 C but were significantly stronger at room temperature. Stress-rupture tests at 760 C and 980 C showed lives scattered from 17 to 376 percent of those of as-cast 713 C tested under the same conditions. X-ray diffraction studies showed the large grains formed upon annealing to have a well-defined texture, although the as-extruded material had none.

Miner, R. V., 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↗

Remote analysis of planetary soils: X-ray diffractometer development

A system is described suitable for remote low power mineralogical analysis of lunar, planetary, or asteroid soils. It includes an X-ray diffractometer, fluorescence spectrometer, and sample preparation system. A one Curie Fe-55 source provides a monochromatic X-ray beam of 5.9 keV. Seeman-Bohlin or focusing geometry is employed in the camera, allowing peak detection to proceed simultaneously at all angles and obviating the need for moving parts. The detector system is an array of 500-600 proportional counters with a wire-spacing of 1 mm. An electronics unit comprising preamplifier, postamplifier, window discriminators, and storage flipflops requiring only 3.5 milliwatts was designed and tested. Total instrument power is less than 5 watts. Powder diffraction patterns using a flat breadboard multiwire counter were recorded.

Gregory, J. C.↗

Pressure sintering of Si3N4-Al2O3 /Sialon/

Essentially pore-free Sialon bodies were obtained by pressure sintering for three blends (mol ratios of 4:1, 2:3, and 3:2) of Si3N4 and Al2O3 powders under the conditions of 27.6 MN/sq m and a temperature of 1700 C for 2 h. These dense bodies consist mainly of a Sialon solid solution with a minor amount of a particular second phase. The higher the Al2O3 content (20 to 60 mol% range) in Sialon, the higher the densification rate. Fully dense bodies can be obtained at temperatures as low as 1500 C at 27.6 MN/sq m for 2 h with no second phase detectable by X-ray diffraction. A 100% dense body can be obtained by heating at 1700 C at 27.6 MN/sq m without a holding time.

Yeh, H. C.↗

Phosphate Textural Diversity in CI Chondrites and C-Type Asteroids

Introduction: Apatite, Ca 5 (PO 4 ) 3 (CL/F/OH-), is a ubiquitous phosphate found throughout the solar system, including the most primitive solids, CI-chondrites [1,2] and related samples of carbonaceous asteroids Ryugu [3] and Bennu [4], returned by JAXA’s Hayabusa2 and NASA’s OSIRIS-REx missions, respectively. Apatite in these primitive solids is found as individual grains or mineral clusters and has been inferred to form from the hydrothermal sequence during cooling of their respective parent body or bodies. To better understand the formation history and reworking of these early phosphates we have undertaken a highly coordinated study of phosphate microstructures, geochemistry and U/Pb geochronology from a suite of CI meteorites and carbonaceous asteroid samples. These data have identified novel phosphate microstructures and complex relationships across a suite of apatite grains from the early solar system, indicating multiple episodes of growth and modification on the CI parent body(ies). Methods: Samples of CI chondrites, Alais, Ivuna, Orgueil, Oued Chebeika 002, Yamato (Y) 82162, Y980115, Y980134, and two chips of Hayabusa2 Ryugu particles (A0262 and C0263) have been acquired for analysis. The bulk texture of the samples were first scanned by X-ray Computed Tomography (XCT) using the Nikon XT H 320 within the XFACT facility at NASA JSC or the Xradia 620 Versa at the UTCT facility. Based on the identification of petrofabrics or features of interest from the XCT data, samples were chipped, oriented, potted in epoxy and thick sections were prepared. After anhydrously polishing the samples with silicon carbide and dry diamond powder down to 1 µm, the samples were ion polished using a Hitachi ArBlade. Energy dispersive Xray spectrometry (EDS) maps were collected to ID phosphates of interest using a JEOL 7900F SEM. The internal microstructures of identified phosphates were then mapped by electron backscatter diffraction (EBSD) using the JEOL 7900F. Based on the EDS and EBSD data, domains of interest were targeted for quantitative chemical analyses using a JEOL 8530 EPMA. Subsequently, in situ U-Pb and 207 Pb/ 206 Pb ages will be collected using a Cameca ims1290 secondary ion mass spectrometer at UCLA across a range of microstructures. Results: Apatite grains are ubiquitous throughout the CI chondrites and carbonaceous asteroid materials, found as individual grains, disseminated clusters or grain aggregates. Apatite grains are associated with serpentine, magnet-ite, and/or carbonate. Of particular interest, we have identified individual and aggregate polycrystalline grains ex-hibiting an internal ‘honeycomb’ texture (Fig. 1). Some of these grains appear overprinted by subsequent alteration while others remain unaltered. Apatite halogen sites are dominated by the missing component, assumed to be OH, and F, comparable to published values from Bennu, Ryugu and CM-chondrites [3-5]. However, the Yamato CI-like meteorites show a broader range of Cl values, and one grain from Alais is dominated by CL. Summary: Apatite growth features indicate a protracted and complex growth history, consistent with precipitation from an evolving fluid system. The ‘honeycomb’ texture identified in some CI meteorites is, to the best of our knowledge, the first report of such a microstructure in meteoritic phosphate. The microtextures and zoning will guide subsequent age analyses, to better constrain the formation and reworking of phosphate in CI(-like) materials. Acknowledgments: We thank the National Institute of Polar Research, Japan for samples of Y82162, 980115 and 980134 meteorites, ASU’s Buseck Center for Meteorite Studies for samples of Ivuna and Alais meteorites, and JAXA curation for chips of Ryugu material. This work was funded by NASA ROSES LARS grant 24-LARS24-0014. References: [1] Morlok et al., 2016, GCA 70:5371-5394. [2] Alfin g et al., 2019, Geochemistry 79:125532. [3] Nakamura et al. (2022) Science 379:1-15. [4] Seifert et al. (2026) MAPS 61:504-521. [5] Piralla et al. (2021) MAPS 56:809-828.

CI chondrites↗

Impact-induced water loss from serpentine, nontronite and kernite

Preliminary experiments have been conducted to study shock-release of volatiles from minerals. Impact-induced loss of bound water from hydrous minerals has been observed, using infrared absorption and X-ray powder diffractometer techniques. Serpentine (Mg3Si2O5(OH)4) and nontronite (.5Ca(0.7)Fe4/(Si(7.3)Al(0.7))O20/(OH)4.nH2O) were shocked and recovered from pressures of up to 38 GPa, using one-dimensional shock reverberation techniques. Kernite (Na2B4O7.4H2O) was impacted by a spherical pyrex projectile traveling at 4.89 km/sec, which produced a peak pressure of approximately 33 GPa. The infrared absorption spectra indicate that some of the bound water from these three minerals was released as a result of shock compression and subsequent rarefaction. This evidence is supported by the recovery of small amounts of vapor from the serpentine shocked to 23.5 GPa and the nontronite shocked to 18 GPa. The recovered vapor is inferred to be water from the shocked minerals. X-ray diffraction spectra indicate no major changes in the unit cell dimensions of the two silicates, except for a decrease in the lattice constant in the c-direction of the nontronite, consistent with the loss of interlayer water.

Boslough, M. B.↗

Specimen Holder Design Improves Accuracy of X-Ray Powder Analysis

Specimen holder for X ray diffraction analysis presents the specimen to the incident X rays in a curvature. This permits the use of an X ray beam having a larger divergence angle, the beam intensity is increased, and the statistical accuracy of analysis is improved.

Mack, M.↗