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At least 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
NASA NTRS2018

Investigation of Alpha Silicon Carbide / Carbon Fiber Proposed (2H & 6H-SiC) / C

A commercially available alpha silicon carbide coated carbon 12k fiber tow was subjected to rigorous inspection and testing. The pyrolized polyacrylonitrile (PAN) fiber had gone through a conversion process that resulted in a thin layer of SiC forming on the exterior of the fiber. The fibers? surface was characterized by x-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES) and scanning electron microscopy (SEM). Powdered x-ray diffraction (XRD) examined the bulk material properties. Transmission electron microscopy (TEM) coupled with energy-dispersive X-ray spectroscopy (EDS) examined the crystallinity of the SiC. A number of pristine samples were used to determine elongation rate and tensile strength.

Trunek, Andrew↗
NASA NTRS2020

Thermal Analysis, Compressibility, and Decomposition of Synthetic Bastnäsite-(La) to Lanthanum Oxyfluoride

Understanding basic material properties of rare earth element (REE) bearing minerals such as their phase stability and equations of state can assist in understanding how economically viable deposits might form. Bastnäsite is the most commonly mined REE bearing mineral. We synthesized the lanthanum-fluoride end member, bastnäsite-(La) (LaCO3F), and investigated its thermal behavior and decomposition products from 298 K to 1173 K under ambient pressure conditions through thermogravimetric analysis, differential scanning calorimetry, evolved gas analysis, and high temperature powder X-ray diffraction. We also investigated the compressibility of bastnäsite-(La) via single crystal X-ray diffraction in diamond anvil cells at an ambient temperature up to 11.3 GPa and from 4.9 GPa to 7.7 GPa up to 673 K. At ambient pressure, bastnäsite-(La) was stable up to 598 K in air, where it decomposed into CO2 and tetragonal γ-LaOF. Above 948 K, cubic α-LaOF is stable. High temperature X-ray diffraction data were used to fit the Fei thermal equation of state and the thermal expansion coefficient α(sub 298) for all three materials. Bastnäsite-(La) was fit from 298 K to 723 K with V(sub 0) = 439.82 Å(exp 3), α(sub 298) = 4.32 × 10(exp -5) K(exp -1), a(sub 0) = −1.68 × 10(exp -5) K(exp -1), a(sub 1) = 8.34 × 10(exp -8) K(exp -1), and a(sub 2) = 3.126 K(exp -1). Tetragonal γ-LaOF was fit from 723 K to 948 K with V(sub 0) = 96.51 Å(exp 3), α(sub 298) = 2.95×10(exp -4) K(exp -1), a(sub 0) = −2.41×10(exp -5) K(exp -1), a(sub 1) = 2.42×10(exp -7) K(exp -1), and a(sub 2) = 41.147 K(exp -1). Cubic α-LaOF was fit from 973 K to 1123 K with V(sub 0) = 190.71 Å(exp 3), α(sub 298) = −1.12×10(exp -5) K(exp -1), a(sub 0) = 2.36×10(exp -4) K(exp -1), a(sub 1) = −1.73 × 10(exp -7) K(exp -1), and a(sub 2) = −17.362 K(exp -1). An ambient temperature third order Birch–Murnaghan equation of state was fit with V(sub 0) = 439.82 Å(exp 3), K(sub 0) = 105 GPa, and K’ = 5.58.

Bastnäsite↗
NASA NTRSDate not supplied

TEM and XRD Investigation of Impact Glass Alteration Products: Amorphous Materials, Phyllosilicates and Everything in Between

Impact cratering is one of the most ubiquitous geologic processes shaping the surface of all solid bodies in our solar system. Impacts are also a major source of clay minerals and poorly crystalline, clay-like materials on Earth and Mars[1,2].These phyllosilicates and related clay-like phases comprise an incredibly complex group of materials, and their characterization, even in controlled laboratory settings, remains a challenging endeavor. The nature and origin of clay minerals and amorphous materials on Mars, which form a major component (~20-70 wt %) of rock and soil samples in Gale Crater as determined by the CheMin instrument on Curiosity, have remained ambiguous[3]. These amorphous phases likely fall on a spectrum between pristine volcanic and/or impact-produced primary materials and clay minerals and related phases formed from aqueous alteration. Amorphous materials are common weathering products in terrestrial sediments, soils, and paleosols [e.g., 4,5].Primary impact materials (glass, melt rocks)are comparable in some ways to those generated volcanically [6], and so it may be possible that an amorphous component is preserved within altered impactites. There are hundreds of thousands of impact craters on Mars, and Curiosity and Perseverance are currently exploring ancient impact craters. We hypothesize that the sediments and lithologies in Gale and Jezero Craters and elsewhere contain altered impact products; it is therefore important to better understand the composition and structure of these materials. Here we present the first results from a study characterizing materials produced from impact glass alteration–clay minerals, poorly crystalline/amorphous materials–in terrestrial craters using Transmission Electron Microscopy (TEM), powder X-ray diffraction (pXRD)and chemical (EDS) analysis.

Impact crater↗
NASA NTRS2022

Effect of Ni2+, Zn2+, and Co2+ on green rust transformation to magnetite

In this study, we investigated Ni2+, Zn2+, and Co2+ mineralogical incorporation and its effect on green rust transformation to magnetite. Mineral transformation experiments were conducted by heating green rust suspensions at 85 °C in the presence of Ni2+, Zn2+, or Co2+ under strict anoxic conditions. Transmission electron microscopy and powder X-ray diffraction showed the conversion of hexagonal green rust platelets to fine grained cubic magnetite crystals. The addition of Ni2+, Zn2+, and Co2+ resulted in faster rates of mineral transformation. The conversion of green rust to magnetite was concurrent to significant increases in metal uptake, demonstrating a strong affinity for metal sorption/ co-precipitation by magnetite. Dissolution ratio curves showed that Ni2+, Zn2+, and Co2+ cations were incorporated into the mineral structure during magnetite crystal growth. The results indicate that the transformation of green rust to magnetite is accelerated by metal impurities, and that magnetite is a highly effective scavenger of trace metals during mineral transformation. The implications for using diagenetic magnetite from green rust precursors as paleoproxies of Precambrian ocean chemistry are discussed.

Hydrosulfate green rust↗
NASA NTRS1984

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.↗
NASA NTRS1966

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.↗
NASA NTRS1990

Lead-ruthenium pyrochlores as oxygen electrocatalysts

An investigation of lead-ruthenium pyrochlores of the structure Pb2(Ru/2-x/Pb/x/) O7-y for use as oxygen electrocatalysts in alkaline media is discussed. Lead-ruthenium pyrochlore mixed metal oxides were prepared and characterized by X-ray diffraction, BET surface area, dry powder conductivity, and chemical stability. Gas diffusion electrodes were developed specifically for the lead-ruthenium pyrochlore materials. Also investigated were the effects of varying electrode fabrication parameters on the oxygen reduction performance of the lead-ruthenium pyrochlore electrocatalyst. Long-term stability performance was also evaluated. The oxygen reduction performance of the pyrochlore electrocatalyst is considerably higher than that of the state-of-the-art gold-platinum alloy electrocatalyst currently used by NASA. Furthermore, the pyrochlore electrocatalysts are attractive candidates for high-performance pressurized alkaline fuel cells.

Anderson, E. B.↗
NASA NTRS1995

Hematite, pyroxene, and phyllosilicates on Mars: Implications from oxidized impact melt rocks from Manicouagan Crater, Quebec, Canada

Visible and near-IR refectivity, Moessbauer, and X ray diffraction data were obtained on powders of impact melt rock from the Manicouagan Impact Crater located in Quebec, Canada. The iron mineralogy is dominated by pyroxene for the least oxidized samples and by hematite for the most oxidized samples. Phyllosilicate (smectite) contents up to approximately 15 wt % were found in some heavily oxidized samples. Nanophase hematite and/or paramagnetic ferric iron is observed in all samples. No hydrous ferric oxides (e.g., goethite, lepidocrocite, and ferrihydrite) were detected, which implies the alteration occurred above 250 C. Oxidative alteration is thought to have occurred predominantly during late-stage crystallization and subsolidus cooling of the impact melt by invasion of oxidizing vapors and/or solutions while the impact melt rocks were still hot. The near-IR band minimum correlated with the extent of aleration Fe(3+)/Fe(sub tot) and ranged from approximately 1000 nm (high-Ca pyroxene) to approximately 850 nm (bulk, well-crystalline hematite) for least and most oxidized samples, respectively. Intermediate band positions (900-920 nm) are attributed to low-Ca pyroxene and/or a composite band from hematite-pyroxene assemblages. Manicouagan data are consistent with previous assignments of hematite and pyroxene to the approximately 850 and approximately 1000nm bands observed in Martian reflectivity spectra. Manicouagan data also show that possible assignments for intermediate band positions (900-920 nm) in Martian spectra are pyroxene and/or hematite-pyroxene assemblages. By analogy with impact melt sheets and in agreement with observables for Mars, oxidative alteration of Martian impact melt sheets above 250 C and subsequent erosion could produce rocks and soils with variable proportions of hematite (both bulk and nanophase), pyroxene, and phyllosilicates as iron-bearing mineralogies. If this process is dominant, these phases on Mars were formed rapidly at relativly high temperatures on a sporadic basis throughout the history of the planet. The Manicouagan samples also show that this mineralogical diversity can be accomplished at constant chemical composition, which is also indicated for Mars from the analyses of soil at the two Viking landing sites.

Morris, Richard V.↗
NASA NTRS1995

Hematite, pyroxene, and phyllosilicates on Mars: Implications from oxidized impact melt rocks from Manicouagan Crater, Quebec, Canada

Visible and near-IR reflectivity, Mossbauer, and X ray diffraction data were obtained on powders of impact melt rock from the Manicouagan Impact Crater located in Quebec, Canada. The iron mineralogy is dominated by pyroxene for the least oxidized samples and by hematite for the most oxidized samples. Phyllosilicate (smectite) contents up to 15 wt % were found in some heavily oxidized samples. Nanophase hematite and/or paramagnetic ferric iron is observed in all samples. No hydrous ferric oxides (e.g., goethite, lepidocrocite, and ferrihydrite) were detected, which implies the alteration occurred above 250 C. Oxidative alteration is thought to have occurred predominantly during late-stage crystallization and subsolidus cooling of the impact melt by invasion of oxidizing vapors and/or solutions while the impact melt rocks were still hot. The near-IR band minimum correlated with the extent of aleration (Fe(3+)/Fe(sub tot)) and ranged from approx. 1000 nm (high-Ca pyroxene) to approx. 850 nm (bulk, well-crystalline hematite) for least and most oxidized samples, respectively. Intermediate band positions (900-920 nm) are attributed to low-Ca pyroxene and/or a composite band from hematite-pyroxene assemblages. Manicouagan data are consistent with previous assignments of hematite and pyroxene to the 850 and 1000 nm bands observed in Martian reflectivity spectra. Manicouagan data also show that possible assignments for intermediate band positions (900-920 nm) in Martian spectra are pyroxene and/or hematite-pyroxene assemblages. By analogy with impact melt sheets and in agreement with observables for Mars, oxidative alteration of Martian impact melt sheets above 250 C and subsequent erosion could produce rocks and soils with variable proportions of hematite (both bulk and nanophase), pyroxene, and phyllosilicates as iron-bearing mineralogies. If this process is dominant, these phases on Mars were formed rapidly at relatively high temperatures on a sporadic basis throughout the history of the planet. The Manicouagan samples also show that this mineralogical diversity can be accomplished at constant chemical composition, which is also indicated for Mars from analyses of soil at the two Viking landing sites.

Morris, Richard V.↗
NASA NTRS1983

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.↗
NASA NTRS1984

Comparative measurements using different particle size instruments

This paper discusses the measurement and comparison of particle size and velocity measurements in sprays. The general nature of sprays and the development of standard, consistent research sprays are described. The instruments considered in this paper are: pulsed laser photography, holography, television, and cinematography; laser anemometry and interferometry using visibility, peak amplitude, and intensity ratioing; and laser diffraction. Calibration is by graticule, reticle, powders with known size distributions in liquid cells, monosize sprays, and, eventually, standard sprays. Statistical analyses including spatial and temporal long-time averaging as well as high-frequency response time histories with conditional sampling are examined. Previous attempts at comparing instruments, the making of simultaneous or consecutive measurements with similar types and different types of imaging, interferometric, and diffraction instruments are reviewed. A program of calibration and experiments for comparing and assessing different instruments is presented.

Chigier, N.↗
NASA NTRS2004

Ultrasonic Apparatus for Pulverizing Brittle Material

The figure depicts an apparatus that pulverizes brittle material by means of a combination of ultrasonic and sonic vibration, hammering, and abrasion. The basic design of the apparatus could be specialized to be a portable version for use by a geologist in collecting powdered rock samples for analysis in the field or in a laboratory. Alternatively, a larger benchtop version could be designed for milling and mixing of precursor powders for such purposes as synthesis of ceramic and other polycrystalline materials or preparing powder samples for x-ray diffraction or x-ray fluorescence measurements to determine crystalline structures and compositions. Among the most attractive characteristics of this apparatus are its light weight and the ability to function without need for a large preload or a large power supply: It has been estimated that a portable version could have a mass <0.5 kg, would consume less than 1 W h of energy in milling a 1-cm3 volume of rock, and could operate at a preload <10 N. The basic design and principle of operation of this apparatus are similar to those of other apparatuses described in a series of prior NASA Tech Briefs articles, the two most relevant being Ultrasonic/ Sonic Drill/Corers With Integrated Sensors (NPO-20856), Vol. 25, No. 1 (January 2001), page 38 and Ultrasonic/ Sonic Mechanisms for Deep Drilling and Coring (NPO-30291), Vol. 27, No. 9 (September 2003), page 65. As before, vibrations are excited by means of a piezoelectric actuator, an ultrasonic horn, and a mass that is free to move axially over a limited range. As before, the ultrasonic harmonic motion of the horn drives the free-mass in a combination of ultrasonic harmonic and lower-frequency hammering motion. In this case, the free-mass is confined within a hollow cylinder that serves as a crushing chamber, and the free-mass serves as a crushing or milling tool. The hammering of the free-mass against a material sample at the lower end of the chamber grinds the sample into powder in a relatively short time. The restriction of the free-mass to axial motion only makes the grinding very efficient. The free-mass can be fabricated to have teeth on its lower face to enhance the grinding effect. Optionally, there can be a hole at the bottom of the chamber covered with a sieve to tailor the size distribution of the powder leaving the crushing chamber.

Sherrit, Stewart↗
NASA NTRS1996

Gas-Phase Combustion Synthesis of Aluminum Nitride Powder

Due to its combined properties of high electrical resistivity and high thermal conductivity aluminum nitride (AlN) is a highly desirable material for electronics applications. Methods are being sought for synthesis of unagglomerated, nanometer-sized powders of this material, prepared in such a way that they can be consolidated into solid compacts having minimal oxygen content. A procedure for synthesizing these powders through gas-phase combustion is described. This novel approach involves reacting AlCl3, NH3, and Na vapors. Equilibrium thermodynamic calculations show that 100% yields can be obtained for these reactants with the products being AlN, NaCl, and H2. The NaCl by-product is used to coat the AlN particles in situ. The coating allows for control of AlN agglomeration and protects the powders from hydrolysis during post-flame handling. On the basis of thermodynamic and kinetic considerations, two different approaches were employed to produce the powder, in co-flow diffusion flame configurations. In the first approach, the three reactants were supplied in separate streams. In the second, the AlCl3 and NH3 were premixed with HCl and then reacted with Na vapor. X-ray diffraction (XRD) spectra of as-produced powders show only NaCl for the first case and NaCl and AlN for the second. After annealing at 775 C tinder dynamic vacuum, the salt was removed and XRD spectra of powders from both approaches show only AlN. Aluminum metal was also produced in the co-flow flame by reacting AlCl3 with Na. XRD spectra of as-produced powders show the products to be only NaCl and elemental aluminum.

Axelbaum, R. L.↗
NASA NTRS1973

A method for determining the preferred orientation of crystallites normal to a surface

Techniques representing the angular distribution of a particular direction in a crystallographic reference frame or analytical methods were developed. The data required by these techniques for displaying preferred orientation is obtained by measuring the orientation of a large number of crystallites. This may be done visually using etch-pit or Laue techniques which, experimentally, are both tedious and difficult. The intensities of X ray diffraction maxima are proportional to the number of crystallites whose crystallographic plane normals bisect the incident and diffracted beams. Parameters used in calculating powder patterns are also presented.

Snyder, R. L.↗
NASA NTRS2005

Capture of Hydrogen Using ZrNi

Water, as ice, is thought to reside in craters at the lunar poles along with CH4 and H2 . A proposed robotic mission for 2012 will utilize metal/metal hydrides for H2 recovery. Specifications are 99% capture of H2 initially at 5 bar and 100C (or greater), and degassing completely at 300C. Of 47-systems examined using the van't Hoff equation, 4 systems, Mg/MgH2, Mg2Ni/Mg2NiH4, ZrNi/ZrNiH2.8, and Pd/PdH0.77, were considered likely candidates for further examination. It is essential, when selecting a system, to also examine questions regarding activation, kinetics, cyclic stability, and gas impurity effects. After considering those issues, ZrN1 was selected as the most promising candidate, as it is easily activated and rapidly forms ZrNiH 2.8 . In addition, it resists oxide poisoning by CO2, and H2O, while some oxidation by O2 is recommended for improved activation . The presence of hydrogen in the as received Zr-Ni alloy from Alfa Aesar posed additional technical problems. X-ray diffraction of the Zr-Ni powder (-325 mesh), with a Zr:Ni wt% ratio of 70:30, was found to consist of ZrH2, ZrNiH2.8, and ZrNi. ZrH2 in the alloy presented the risk that after degassing that both Zr and ZrNi would be present, and thus lead to erroneous results regarding the reactivity of ZrNi with H2 . Fortunately, ZrH2 is a highly stable hydride that does not degas H2 to any significant extent at temperatures below 300C. Based on equilibrium calculations for the decomposition of ZrH2, only 1 millionth of the hydride decomposed at 300C under a N2 atmosphere flowing at 25 ccm for 64 hours, the longest time for pretreatment employed in the investigation. It was possible, from the X-ray results and knowledge of the Zr:Ni ratio, to compute the composition of a pretreated specimen as being 76 wt% ZrNi and the balance ZrH2.

Patton, Lisa↗
NASA NTRS2022

(Preliminary) Effects of Ball Milling Zeolite Powders for Use in Additively Manufactured Solid Sorbents

Zeolite 13X is favorable to be used as an adsorbent in carbon dioxide (CO2) removal from the spacecraft cabin air. Reducing the size of the zeolite particles and particle size distribution is thought to increase the capacity of CO2 adsorption of the zeolite 13X powder, and potentially increase its manufacturability as a paste for additive manufacturing or slip casting. This paper will go into detail on the process of using ball milling in order to reduce particle size and particle size distribution of commercial zeolite 13X powder, as well as to characterize CO2 adsorption and manufacturability of the milled powder. Both dry and wet ball milling was analyzed during the experiment. Studies were also ran on the amount of time the powder was milled, rotational speed of the milling machine, ball to powder ratio, ball to jar ratio, and ethanol to powder ratio. The processed powder was then characterized through laser diffraction, SEM, and surface measurement techniques to show that particle size and particle size distribution could be reduced, and to show the effect of the reduced particle size and particle size distribution on CO2 adsorption and manufacturability.

zeolite↗
NASA NTRS2002

Effect of the Chemical State of the Surface on the Relaxation of the Surface Shell Atoms in SiC and GaN Nanocrystals

The effect of the chemical state of the surface of nanoparticles on the relaxation in the near-surface layer was examined using the concept of the apparent lattice parameter (alp) determined for different diffraction vectors Q. The apparent lattice parameter is a lattice parameter determined either from an individual Bragg reflection, or from a selected region of the diffraction pattern. At low diffraction vectors the Bragg peak positions are affected mainly by the structure of the near-surface layer, while at high Q-values only the interior of the nano-grain contributes to the diffraction pattern. Following the measurements on raw (as prepared) powders we investigated powders cleaned by annealing at 400C under vacuum, and the same powders wetted with water. Theoretical alp-Q plots showed that the structure of the surface layer depends on the sample treatment. Semi-quantitative analysis based on the comparison of the experimental and theoretical alp-Q plots was performed. Theoretical alp-Q relations were obtained from the diffraction patterns calculated for models of nanocrystals with a strained surface layer using the Debye functions.

Palosz, B.↗
NASA NTRS2008

Compact, Non-Pneumatic Rock-Powder Samplers

Tool bits that automatically collect powdered rock, permafrost, or other hard material generated in repeated hammering action have been invented. The present invention pertains to the special case in which it is desired to collect samples in powder form for analysis by x-ray diffraction and possibly other techniques. The present invention eliminates the need for both the mechanical collection equipment and the crushing chamber and the pneumatic collection equipment of prior approaches, so that it becomes possible to make the overall sample-acquisition apparatus more compact.

Sherrit, Stewart↗