Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “Powder diffraction”

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 163 records · Page 9

Advantages of barium peroxide in the powder synthesis of perovskite superconductors

This paper compares reaction chemistry, material processing, and material characteristics for the solid state reaction using BaCO3 or BaO2 in the synthesis of perovskite superconductors. Results are presented for weight loss and X-ray diffraction, sample morphology and homogeneity as monitored by SEM and EDS, and the superconductivity critical temperature and ac susceptibility. Greater mass density, increased sample homogeneity, lower resistance, and improved reproducibility for material are found when BaO32 is used.

Hepp, A. F.↗

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.↗

Processing Bi-Pb-Sr-Ca-Cu-O superconductors from amorphous state

Researchers produced superconducting ceramics of the Bi-Pb-Sr-Ca-Cu-O system started from a glass. To form the glass, the mixed oxide powder was melted at 1200 C in air. The liquid was quenched rapidly by pouring it onto an aluminum plate and rapidly pressing with another plate. The quenched compound was in the form of black amorphous solid, whose x-ray powder pattern has no crystalline peaks. After heat treatment at high temperatures, the glass crystallized into a superconductor. The crystalline phases in the superconductor identified using x-ray diffraction patterns. These phases were that associated with the superconducting phases of T(sub c) = 80 K (Bi2Ca1Sr2Cu2Ox) and of T(sub c) = 110 K (Bi2Ca2Sr2Cu3Ox). The dc resistivity and the ac susceptibility of these superconductors were studied.

Chiang, C. K.↗

Tribological performance of Al2O3-B2O3 composites: Role of CuOand CaO constituents

Al2O3-B2O3 based composites for wear resistant applications (e.g., seal rings and bearings) were manufactured using powder metallurgy route. Four different compositions were considered to control amount of in situ phases, mainly aluminum borate, formed during sintering. The fabricated composites were characterized using X-ray diffraction to identify the phases. Hardness was measured in terms of micro-hardness. The tribological performance of the composites were evaluated by conducting dry sliding tests against alumina balls at different humidity levels (10 – 95% relative humidity). The X-ray spectrum revealed that increase in B2O3 content in the composites increased the amount of aluminum borate phase that enhanced the micro-hardness. Results revealed that aluminum borate enhanced the wear resistance of the composites, whereas the humidity-sensitive alumina phase reduced friction at higher humidity levels. Furthermore, CuO and CaO (2-5 wt.%) were added separately to the composite, resulting in increased density by 22-48 %. Athough the addition of CuO and CaO led to increase in hardness and wear resistance of the composites, the coefficient of friction was negatively affected. The friction and wear performance along with wear mechanism are discussed with respect to observed phases in the composites.

Ashish K. Kasar↗

The oxidation state of the surface of Venus

We present experimental results showing that basalt is oxidized in CO-CO2 gas mixtures having CO number densities close to those (approximately 2 times higher) at the surface of Venus. The results suggest that the red color observed by Pieters et al at the Venera 9 and 10 landing sites is due to subaerial oxidation of Fe(2+)-bearing basalt on the surface of Venus, and that hematite, instead of magnetite, is present on the surface of Venus. Well-characterized basalt powder was iosthermally heated in 1000 ppm CO-CO2 gas mixtures at atmospheric pressure for several days. The starting material and reacted samples were analyzed by Mossbauer spectroscopy to determine the amount of Fe(2+) and Fe(3+) in the samples. X-ray diffraction and optical microscopy were also used to characterize samples. The basalt oxidation occurs because the CO and CO2 do not equilibrate in the gas mixture at the low temperatures used. Thus, the basalt reacts with the more abundant CO2 and is oxidized. We propose that the red color of the surface of Venus is due to failure of CO and CO2 to equilibrate with one another in the near-surface atmosphere of Venus, leading to subaerial oxidation of erupted Fe(2+)-bearing basalts. Our interpretation is supported by our studies of magnetite oxidation, which show that synthetic magnetite powders are oxidized to hematite in CO-CO2 gas mixtures inside the magnetite stability field, by our studies of pyrite decomposition, and by independent work on CO-CO2 equilibration in furnace gases.

Fegley, B., Jr.↗

Progress in development of tapes and magnets made from Bi-2223 superconductors

Long lengths of (Bi,Pb)2Sr2Ca2Cu3O(x) tapes made by powder-in-tube processing have been wound into coils. Performance of the coils has been measured at temperatures of 4.2 to 77 K, and microstructures have been examined by x-ray diffraction and electron microscopy and then related to superconducting properties. A summary of recent results and an overview of future goals are presented.

Balachandran, U.↗

Chemical and Thermal Analysis

Work during the past three years has included significant research in several areas aimed at further clarification of the aging and chemical failure mechanism of thermoplastics (PVDF or Tefzel) for pipes. Among the areas investigated were the crystallinity changes associated with both the Coflon and Tefzel after various simulated environmental exposures using X-Ray diffraction analysis. We have found that significant changes in polymer crystallinity levels occur as a function of the exposures. These crystallinity changes may have important consequences on the fracture, fatigue, tensile, and chemical resistance of the materials. We have also noted changes in the molecular weight distribution and the increased crosslinking of the Coflon material using Gel Permeation Chromatographic Analysis. Again these changes may result in variations in the mechanical and chemical properties in the material. We conducted numerous analytical studies with methods including X-ray Diffraction, Gel Permeation Chromatography, Fourier Transform Infrared Spectroscopy, and Differential Scanning Calorimetry. We investigated a plethora of aged samples of both Tefzel and Coflon that were forwarded from MERL. Pressurized tests were performed on powdered PVDF in a modified Fluid A, which we will call A-2. In this case the ethylene diamine concentration was increased to 3 percent in methanol. Coflon pipe sections and powdered Coflon were exposed in pressure cells at 1700 psi at three separate test temperatures.

Bulluck, J. W.↗

Thermoelectric Properties of Self Assemble TiO2/SnO2 Nanocomposites

Recent advances in improving efficiency of thermoelectric materials are linked to nanotechnology. Thermodynamically driven spinodal decomposition was utilized to synthesize bulk nanocomposites. TiO2/SnO2 system exhibits a large spinodal region, ranging from 15 to 85 mole % TiO2. The phase separated microstructures are stable up to 1400 C. Semiconducting TiO2/SnO2 powders were synthesized by solid state reaction between TiO2 and SnO2. High density samples were fabricated by pressureless sintering. Self assemble nanocomposites were achieved by annealing at 1000 to 1350 C. X-ray diffraction reveal phase separation of (Ti(x)Sn(1-x))O2 type phases. The TiO2/SnO2 nanocomposites exhibit n-type behavior; a power factor of 70 (mu)W/m sq K at 1000 C has been achieved with penta-valent doping. Seebeck, thermal conductivity, electrical resistivity and microstructure will be discussed in relation to composition and doping.

Dynys, Fred↗

Thermoelectric Properties of Self Assembled TiO2/SnO2 Nanocomposites

Recent advances in improving efficiency of thermoelectric materials are linked to nanotechnology. Thermodynamically driven spinodal decomposition was utilized to synthesize bulk nanocomposites. TiO2/SnO2 system exhibits a large spinodal region, ranging from 15 to 85 mole % TiO2. The phase separated microstructures are stable up to 1400 C. Semiconducting TiO2/SnO2 powders were synthesized by solid state reaction between TiO2 and SnO2. High density samples were fabricated by pressureless sintering. Self assemble nanocomposites were achieved by annealing at 1000 to 1350 C. X-ray diffraction reveal phase separation of (Ti(x)Sn(1-x))O2 type phases. The TiO2/SnO2 nanocomposites exhibit n-type behavior; a power factor of 70 W/mK2 at 1000 C has been achieved with penta-valent doping. Seebeck, thermal conductivity, electrical resistivity and microstructure will be discussed in relation to composition and doping.

Dynys, Fred↗

Stability of Ceramics in Hydrogen between 4000 and 4500 F

The various reactions that are possible between hydrogen and certain ceramic materials are discussed as well as the means of measuring the extent of such reactions. Powdered carbides, nitrides, borides, and oxides were tested. These materials were heated inductively in a tungsten cup between 4000 and 4500 F for two 1-hour periods under a static hydrogen atmosphere. Weight, pressure, and diffraction pattern changes were observed, and these served to indicate the extent of reaction. Most of the ceramics, HfC, ZrC, TiC, TaC, NbC, WC, MO2C, HfN, ZrN, NbN, ZrB2, NbB2, and WB, showed less reaction than the minimum detectable value. However, the ceramics, TiN, TaN, HfB2, TiB2, ZrO2, and Cr2O3, apparently reacted to a measurable extent with hydrogen. Reactions of SiC, VC, and TaB2 with hydrogen were not determinable because of their incompatibility with the tungsten container.

May, Charles E.↗

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.↗

Field-induced orientation of nonlevitated microcrystals of superconducting YBa2Cu3O(7-x)

X-ray diffraction patterns of superconducting YBa2Cu3O(7-x) particles which have typical dimensions D of less than 5 microns and do not levitate in an inhomogeneous magnetic field at T less than Tc show marked evidence of particle alignment when powder specimens are subjected to a 0.5-T field at T less than Tc, but reveal random orientation for T greater than Tc. A majority of the particles align preferentially with their antiphase twin boundary planes and a-b planes along the applied field, but a minority align with their b axes along the field.

Solin, S. A.↗

Surveying Clay Mineral Diversity in the Murray Formation, Gale Crater, Mars

One of the primary science goals of Mars Science Laboratory (MSL) is to investigate layered clay mineral-bearing deposits outcropping in the lower NW slopes of Aeolis Mons (Mt. Sharp) detected from orbit. Martian clay mineral-bearing layered rocks are of particular interest because they are potential markers of sedimentary deposits formed in habitable aqueous environments. The CheMin X-ray diffraction (XRD) instrument aboard MSL has documented clay minerals in various drill samples during its traverse of Gale Crater's floor and ascent of Mt. Sharp. Previously, the high concentrations of clay minerals (approximately 20 wt.%) detected in drill powders of mudstone (Sheepbed member) at Yellowknife Bay (YKB) allowed their detailed characterization. Drill powders recovered from lacustrine mudstones of the Sheepbed member at YKB contain smectite clay minerals. Based on the position of 02l reflections in XRD patterns, which serve as an indicator of octahedral occupancy, the smectites are Fe-bearing, trioctahedral species analogous to ferrian saponites from terrestrial deposits. The smectites are thought to have been formed through a process of isochemical aqueous alteration of detrital olivine close to the time of sediment deposition under anoxic to poorly oxidizing conditions. The clay minerals are key indicators that the lake waters were benign and habitable at the time. Clay minerals were detected at other locations during MSL's traverse, including samples from the Pahrump Hills, but lower abundances and overlapping peaks from crystalline phases in XRD patterns hamper in-depth analysis.

Bristow, T. F.↗

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.↗

Powder Handling Device for Analytical Instruments

Method and system for causing a powder sample in a sample holder to undergo at least one of three motions (vibration, rotation and translation) at a selected motion frequency in order to present several views of an individual grain of the sample. One or more measurements of diffraction, fluorescence, spectroscopic interaction, transmission, absorption and/or reflection can be made on the sample, using light in a selected wavelength region.

Sarrazin, Philippe C.↗

Effects of Kapton Sample Cell Windows on the Detection Limit of Smectite: Implications for CheMin on the Mars Science Laboratory Mission

The CheMin instrument on the Mars Science Laboratory (MSL) rover Curiosity is an X-ray diffraction (XRD) and X-ray fluorescence (XRF) instrument capable of providing the mineralogical and chemical compositions of rocks and soils on the surface of Mars. CheMin uses a microfocus X-ray tube with a Co target, transmission geometry, and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D XRD patterns and energy-dispersive X-ray histograms from powdered samples. CheMin has two different window materials used for sample cells -- Mylar and Kapton. Instrument details are provided elsewhere. Fe/Mg-smectite (e.g., nontronite) has been identified in Gale Crater, the MSL future landing site, by CRISM spectra. While large quantities of phyllosilicate minerals will be easily detected by CheMin, it is important to establish detection limits of such phases to understand capabilities and limitations of the instrument. A previous study indicated that the (001) peak of smectite at 15 Ang was detectable in a mixture of 1 wt.% smectite with olivine when Mylar is the window material for the sample cell. Complications arise when Kapton is the window material because Kapton itself also has a diffraction peak near 15 Ang (6.8 deg 2 Theta). This study presents results of mineral mixtures of smectite and olivine to determine smectite detection limits for Kapton sample cells. Because the intensity and position of the smectite (001) peak depends on the hydration state, we also analyzed mixtures with "hydrated" and "dehydrated"h smectite to examine the effects of hydration state on detection limits.

Achilles, C. N.↗

Synthesis, Structure, and Characterization of Cu4S10(4-methylpyridine)4

The title compound, Cu4S10(4-methylpyridine)(sub 4) (dot) 4-methylpyridine was prepared by three different reactions: the oxidation of copper powder by sulfur and the reaction of copper (I) sulfide (or CuBr (dot) SMe2) with excess sulfur, both in the coordinating solvent, 4-methylpyridine. Red crystals of the compound obtained by layering with hexanes were subjected to single crystal X-ray diffraction. The structure was refined to R = 0.026 and R(sub w) = 0.036 in a space group P1bar (No. 2), with Z = 2, a = 13.983 (2) A, b = 15.384 (2) A, c = 9.660 (1) A, alpha = 93.87 (1)deg., beta = 93.38 (1)deg., gamma = 99.78 (1)deg., V = 2037.9 (9) A(exp 3). The compound has approximate S(sub 4) symmetry and consists of two pentasulfide chains linking four Cu(I) ions, each with a corrdinating 2-methylpyridine. The infrared spectrum was dominated by absorption due to coordinated 4-methylpyridine with several low-energy peaks attributable to S-S stretches, which were also observed by Raman spectroscopy. A featureless electronic absorption spectrum yielded a single peak in the near ultraviolet upon computer enhancement (lambda = 334 nm, epsilon = 10,000), most likely an intraligand transition. Cyclic voltammetry indicates that the polysulfide complex undergoes irrversible oxidation and reduction at +0.04 and -0.34 V vs. SCE, respectively, at 298 K in 4-methylpyridine when swept at 20 mV/sec. The electrochemical behavior was unvaried even at sweep rates as high as 100 V/sec.

Hepp, Aloysius F.↗

X-Ray Diffraction on Mars: Scientific Discoveries Made by the CheMin Instrument

The Mars Science Laboratory Curiosity landed in Gale crater in August 2012 with the goal to identify and characterize habitable environments on Mars. Curiosity has been studying a series of sedimentary rocks primarily deposited in fluviolacustrine environments approximately 3.5 Ga. Minerals in the rocks and soils on Mars can help place further constraints on these ancient aqueous environments, including pH, salinity, and relative duration of liquid water. The Chemistry and Mineralogy (CheMin) X-ray diffraction and X-ray fluorescence instrument on Curiosity uses a Co X-ray source and charge-coupled device detector in transmission geometry to collect 2D Debye-Scherrer ring patterns of the less than 150 micron size fraction of drilled rock powders or scooped sediments. With an angular range of approximately 2.52deg 20 and a 20 resolution of approximately 0.3deg, mineral abundances can be quantified with a detection limit of approximately 1-2 wt. %. CheMin has returned quantitative mineral abundances from 16 mudstone, sandstone, and aeolian sand samples so far. The mineralogy of these samples is incredibly diverse, suggesting a variety of depositional and diagenetic environments and different source regions for the sediments. Results from CheMin have been essential for reconstructing the geologic history of Gale crater and addressing the question of habitability on ancient Mars.

Rampe, E. B.↗