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At least 487 records · Page 27

The interaction of atomic oxygen with copper: An XPS, AES, XRD, optical transmission, and stylus profilometry study

The University of Alabama in Huntsville (UAH) experiment A-0114 was designed to study the reaction of material surfaces with low earth orbits (LEO) atmospheric oxygen. The experiment contained 128 one-inch circular samples; metals, polymers, carbons, and semiconductors. Half of these samples were exposed on the front of the Long Duration Exposure Facility (LDEF) and remaining on the rear. Among metal samples, copper has shown some interesting new results. There were two forms of copper samples: a thin film sputter-coated on fused silica and a solid piece of OFHC copper. They were characterized by x-ray and Auger electron spectroscopies, x-ray diffraction, and high resolution profilometry. Cu 2p core level spectra were used to demonstrate the presence of Cu2O and CuO and to determine the oxidation states.

Raikar, Ganesh N.↗

Growth of Carbon Nanostructure Materials Using Laser Vaporization

Since the potential applications of carbon nanotubes (CNT) was discovered in many fields, such as non-structure electronics, lightweight composite structure, and drug delivery, CNT has been grown by many techniques in which high yield single wall CNT has been produced by physical processes including arc vaporization and laser vaporization. In this presentation, the growth mechanism of the carbon nanostructure materials by laser vaporization is to be discussed. Carbon nanoparticles and nanotubes have been synthesized using pulsed laser vaporization on Si substrates in various temperatures and pressures. Two kinds of targets were used to grow the nanostructure materials. One was a pure graphite target and the other one contained Ni and Co catalysts. The growth temperatures were 600-1000 C and the pressures varied from several torr to 500 torr. Carbon nanoparticles were observed when a graphite target was used, although catalysts were deposited on substrates before growing carbon films. When the target contains catalysts, carbon nanotubes (CNT) are obtained. The CNT were characterized by scanning electron microscopy, x-ray diffraction, optical absorption and transmission, and Raman spectroscopy. The temperature-and pressure-dependencies of carbon nanotubes' growth rate and size were investigated.

Zhu, Shen↗

Controlling Growth Orientation of Phthalocyanine Films by Electrical Fields

Organic Phthalocyanine films have many applications ranging from data storage to various non-linear optical devices whose quality is affected by the growth orientation of Phthalocyanine films. Due to the structural and electrical properties of Phthalocyanine molecules, the film growth orientation depends strongly on the substrate surface states. In this presentation, an electrical field up to 4000 V/cm is introduced during film growth. The Phthalocyanine films are synthesized on quartz substrates using thermal evaporation. An intermediate layer is deposited on some substrates for introducing the electrical field. Scanning electron microscopy, x-ray diffraction, and Fourier transform infrared spectroscopy are used for measuring surface morphology, film structure, and optical properties, respectively. The comparison of Phthalocyanine films grown with and without the electrical field reveals different morphology, film density, and growth orientation, which eventually change optical properties of these films. These results suggest that the growth method in the electrical field can be used to synthesized Phthalocyanine films with a preferred crystal orientation as well as propose an interaction mechanism between the substrate surface and the depositing molecules. The details of growth conditions and of the growth model of how the Phthalocyanine molecules grow in the electrical field will be discussed.

Zhu, S.↗

Structure Orientation in Phthalocyanine Film Growth by Vapor Deposition in Electrical Fields

Films of phthalocyanines were grown by vapor deposition in an electric field on to quartz substrates coated with a very thin layer of gold or indium tin oxide and compared to films grown in the absence of an electric field. A comparison of morphology, nonlinear optical properties, and crystal structure was also made. The films were characterized using scanning electron microscopy, x-ray diffraction, and FTIR. Films grown in the absence of an electric field had a fiber like morphology and those grown in electric fields having a maximum strength of 4000 V/cm had a dense-columnar structure. The crystal structure of films grown in an electric field was different than those grown in the absence of a field.

Banks, C. E.↗

Pigmenting agents in Martian soils: inferences from spectral, Mossbauer, and magnetic properties of nanophase and other iron oxides in Hawaiian palagonitic soil PN-9

We have examined a Hawaiian palagonitic tephra sample (PN-9) that has spectroscopic similarities to Martian bright regions using a number of analytical techniques, including Mossbauer and reflectance spectroscopy, X-ray diffraction, instrumental neutron activation analysis, electron probe microanalysis, transmission electron microscopy, and dithionite-citrate-bicarbonate extraction. Chemically, PN-9 has a Hawaiitic composition with alkali (and presumably silica) loss resulting from leaching by meteoric water during palagonitization; no Ce anomaly is present in the REE pattern. Mineralogically, our results show that nanophase ferric oxide (np-Ox) particles (either nanophase hematite (np-Hm) or a mixture of ferrihydrite and np-Hm) are responsible for the distinctive ferric doublet and visible-wavelength ferric absorption edge observed in Mossbauer and reflectivity spectra, respectively, for this and other spectrally similar palagonitic samples. The np-Ox particles appear to be imbedded in a hydrated aluminosilicate matrix material; no evidence was found for phyllosilicates. Other iron-bearing phases observed are titanomagnetite, which accounts for the magnetic nature of the sample; olivine; pyroxene; and glass. By analogy, np-Ox is likely the primary pigmenting agent of the bright soils and dust of Mars.

Minerals/analysis↗

Low Conductive Thermal Barrier Coatings Produced by Ion Beam Assisted EB-PVD with Controlled Porosity, Microstructure Refinement and Alloying Additions for High Temperature Applications

Various advanced Hafnia-based thermal barrier coatings (TBC) were applied on nickel-based superalloy coupons by electron beam physical vapor deposition. In addition, microstructural modifications to the coating material were made in an effort to reduce the thermal conductivity of the coating materials. Various processing parameters and coating system modifications were made in order to deposit the alloyed TBC with the desired microstructure and thus coating performance, some of which include applying coatings at substrate temperatures of 1150 C on both PtAl and CoNiCrAlY bond coated samples, as well as using 8YSZ as a bond layer. In addition, various characterization techniques including thermal cyclic tests, scanning electron microscopy, x-ray diffraction, thermal conductivity, and reflectivity measurements were performed. Although the coating microstructure was never fully optimized due to funding being cut short, significant reductions in thermal conductivity were accomplished through both chemistry changes (composition) and microstructural modifications.

Wolfe, Douglas E.↗

Producing Zirconium Diboride Components with Complex, Near-Net Shape Geometries by Aqueous Room-Temperature Injection Molding

Room-temperature injection molding is proposed as a novel, low-cost and more energy efficient manufacturing process capable of forming complex-shaped zirconium diboride (ZrB2) parts. This innovative processing method utilized aqueous suspensions with high powder loading and a minimal amount (5 vol.) of water-soluble polyvinylpyrrolidone (PVP), which was used as a viscosity modifier. Rheological characterization was performed to evaluate the room-temperature flow properties of ZrB2-PVP suspensions. ZrB2 specimens were fabricated with high green body strength and were machinable prior to binder removal despite their low polymer content. After binder burnout and pressureless sintering, the bulk density and microstructure of specimens were characterized using Archimedes technique and scanning electron microscopy. X-Ray Diffraction was used to determine the phase compositions present in sintered specimens. Ultimate strength of sintered specimens will be determined using ASTM C1323-10 compressive C-ring test.

Near-Net Shape Forming↗

Chemical, Structural, and Microstructural Changes in Metallic and Silicon-Based Coating Materials Exposed to Iodine Vapor

The chemical, structural and microstructural behavior of steels (304, 316 and A36), titanium-aluminum alloy (Ti-Al, (6Al-4V)), aluminum-magnesium alloy (Al-Mg, 6061), and coatings (Silcolloy and Dursan (SilcoTek Corporation)) were probed after exposure to iodine laminar flow. Exposures were carried out in a custom-built Iodine Vapor RIG (IVR) at 300 degrees C to an iodine laminar vapor flow of 1 mg min(exp. -1), carried by 145 mL-min(exp. -1) argon gas, for 5, 15 and 30 days. Samples were characterized before and after the experiment by gravimetric analysis, X-ray diffraction (XRD) and cross section electron microscopy analysis coupled with energy dispersive X-ray spectroscopy (EDS). All steels exposed for 30 days formed scales consisting mainly of metal (Cr, Fe, Ni) oxides showing different chemistry, microstructure and crystalline phases. Elemental iodine was only detected by EDS analysis in the scales of stainless steels 304 and 316. After 30 days, the Ti-Al exhibited no detectable scale, suggesting only a very thin film was formed. A scale consisting mainly of aluminum, iodine, and oxygen formed on the Al-Mg sample exposed to 30 days. Some pockets rich in magnesium, iodine and oxygen also formed in this Al-Mg alloy. Stainless steel 316, low carbon steel A36 and Ti-Al alloy coated with Silcolloy and stainless steel 304 coated with Dursan that were exposed for 30 days exhibited no oxidation. Stainless steel 304 coated with Silcolloy exposed for 30 days did not exhibit corrosion although the sample gained weight and the coating exhibited expansion. The weight gain per area performance of the materials exposed in iodine lamina flow containing oxygen at impurity level for 10, 15 and 30 days are reported from the lowest to the highest weight gain per area as follows: Steels: Less than 316 less than 304 less than A36; Ti-Al-Mg based alloys: Al-Mg less than Ti-Al: Considering the experimental uncertainties, no weight change was observed for Stainless steel 316, low carbon steel A36 and Ti-Al alloy coated with Silcolloy and stainless steel 304 coated with Dursan. The corrosion of the alloys is catalyzed by iodine in the presence of oxygen as impurity.

Costa, Gustavo C. C.↗

Thermochemistry of Calcium-Magnesium-Aluminum-Silicate (CMAS) and Components of Advanced Thermal and Environmental Barrier Coating Systems

There is increasing interest in the degradation mechanism studies of thermal and environmental barrier coatings (TEBCs) of gas turbines by molten CaO-MgO-Al(exp. 2)O(exp. 3)-SiO(exp. 2) CMAS). CMAS minerals are usually referred as silicon-containing sand dust and volcano ash materials that are carried by the intake air into gas turbines, e.g. in aircraft engines, and their deposits often react at high temperatures (greater than 1200 degrees C) with the engine turbine coating systems and components. The high temperature reactions causes degradation and accelerated failure of the static and rotating components of the turbine engines. We discuss some results of the reactions between the CMAS and Rare-Earth (RE = Y, Yb, Dy, Gd, Nd and Sm) - oxide stabilized ZrO(exp. 2) or HfO(exp. 2) systems, and the stability of the resulting oxides and silicates. Plasma sprayed hollow tube samples (outside diameter = 4.7 mm, wall thickness = 0.76 mm and = 26 mm height) were half filled with CMAS powder, wrapped and sealed with platinum foil, and heat treated at 1310 degrees C for 5h. Samples were characterized by differential scanning calorimetry (DSC), X-ray diffraction, and cross-section electron microscopy analysis and energy dispersive X-ray spectroscopy. It was found that CMAS penetrated the samples at the grain boundaries and dissolved the TEBC materials to form silicate phases containing the rare-earth elements. Furthermore, it was found that apatite crystalline phases were formed in the samples with total rare-earth content higher than 12 mol% in the reaction zone for the ZrO(exp. 2) system. In general, samples with the nominal compositions (30YSZ), HfO(exp. 2)-7Dy(exp. 2)O(exp. 2) and ZrO(exp. 2)-9.5Y(exp. 2)O(exp. 3)-2.25Gd(exp. 2)O(exp. 3)-2.25Yb(exp. 2)O(exp. 3) exhibited lower reactivity or more resistance to CMAS than the other coating compositions of this work.

degradation↗

Basalt Weathering in a Cold and Icy Climate: Three Sisters, Oregon as an Analog for Early Mars

There is abundant evidence for liquid water on early Mars, but the debate remains whether early Mars was warm and wet or cold and icy with punctuated periods of melting. To further investigate the hypothesis of a cold and icy early Mars, we collected rocks and sediments from the Collier and Diller glacial valleys in the Three Sisters volcanic complex in Oregon. We analyzed rocks and sediments with X-ray diffraction (XRD), scanning and transmission electron microscopies with energy dispersive spectroscopy (SEM, TEM, EDS), and visible, short-wave infrared (VSWIR) and thermal-IR (TIR) spectroscopies to characterize chemical weathering and sediment transport through the valleys. Here, we focus on the composition and mineralogy of the weathering products and how they compare to those identified on the martian surface. Phyllosilicates (smectite), zeolites, and poorly crystalline phases were discovered in pro- and supra-glacial sediments, whereas Si-rich regelation films were found on hand samples and boulders in the proglacial valleys. Most phyllosilicates and zeolites are likely detrital, originating from hydrothermally altered units on North Sister. TEM-EDS analyses of the <2 um size fraction of glacial flour samples demonstrate a variety of poorly crystalline (i.e., no long-range crystallographic order) phases: iron oxides, devitrified volcanic glass, and Fe-Si-Al phases. The CheMin XRD on the Curiosity rover in Gale crater has identified significant amounts of X-ray amorphous materials in all samples measured to date. The amorphous component is likely a combination of silicates, iron oxides, and sulfates. Although we have not yet observed amorphous sulfate in the samples from Three Sisters, the variety of poorly crystalline weathering products found at this site is consistent with the variable composition of the X-ray amorphous component identified by CheMin. We suggest that these amorphous phases on Mars could have formed in a similarly cold and icy environment.

Rampe, E. B.↗

Microstructural and Mechanical Characterization of a Dispersion Strengthened Medium Entropy Alloy Produced Using Selective Laser Melting

High entropy alloys (HEAs) are an interesting new class of alloys which have been shown to exhibit both notable strength and ductility for a wide range of temperature and stresses. In addition, the remarkably small difference between the solvus and liquidus temperatures for many face centered cubic HEAs makes them an excellent candidate for selective laser melting fabrication. In this study, the microstructure and mechanical properties of a dispersion strengthened equiatomic NiCoCr alloy successfully produced using selective laser melting are explored. The effect laser speed, laser power, and powder recyclability have on final part density and microstructural segregation are analyzed through both x-ray diffraction and high resolution scanning electron microscopy. These results are further validated and compared to stable phase predictions produced using a commercially available high entropy alloy mobility database. Lastly, the tensile strengths resulting from different heat treatment pathways are detailed.

Smith, T. M.↗

Studies of mineralization in tissue culture: optimal conditions for cartilage calcification

The optimal conditions for obtaining a calcified cartilage matrix approximating that which exists in situ were established in a differentiating chick limb bud mesenchymal cell culture system. Using cells from stage 21-24 embryos in a micro-mass culture, at an optimal density of 0.5 million cells/20 microliters spot, the deposition of small crystals of hydroxyapatite on a collagenous matrix and matrix vesicles was detected by day 21 using X-ray diffraction, FT-IR microscopy, and electron microscopy. Optimal media, containing 1.1 mM Ca, 4 mM P, 25 micrograms/ml vitamin C, 0.3 mg/ml glutamine, no Hepes buffer, and 10% fetal bovine serum, produced matrix resembling the calcifying cartilage matrix of fetal chick long bones. Interestingly, higher concentrations of fetal bovine serum had an inhibitory effect on calcification. The cartilage phenotype was confirmed based on the cellular expression of cartilage collagen and proteoglycan mRNAs, the presence of type II and type X collagen, and cartilage type proteoglycan at the light microscopic level, and the presence of chondrocytes and matrix vesicles at the EM level. The system is proposed as a model for evaluating the events in cell mediated cartilage calcification.

Non-NASA Center↗

Electronic heterodyne moire deflectometry: A method for transient and three dimensional density fields measurements

Effects of diffraction and nonlinear photographic emulsion characteristics on the performance of deferred electronic heterodyne moire deflectometry are investigated. The deferred deflectometry is used for measurements of nonsteady phase objects where it is difficult to complete the analysis of the field in real time. The sensitivity, accuracy and resolution of the system are calculated and it is shown that they are weakly affected by diffraction and by nonlinear recording. The feactures of the system are significantly improved compared with the conventional deferred intensity moire technique, and are comparable with the online heterodyne moire. The system was evaluated experimentally by deferred measurements of the refractive index gradients of a weak phase object consisting of a large KD*P crystal. This was done by photographing the phase object through a Ronchi grating and analyzing the tranparency with the electronic heterodyne readout system. The results are compared with the measurements performed on the same phase object with online heterodyne moire deflectometry and with heterodyne holographic interferometry methods. Some practical considerations for system improvement are discussed.

Stricker, Josef↗

Lunar resources: Oxygen from rocks and soil

The first set of hydrogen reduction experiments to use actual lunar material was recently completed. The sample, 70035, is a coarse-grained vesicular basalt containing 18.46 wt. percent FeO and 12.97 wt. percent TiO2. The mineralogy includes pyroxene, ilmenite, plagioclase, and minor olivine. The sample was crushed to a grain size of less than 500 microns. The crushed basalt was reduced with hydrogen in seven tests at temperatures of 900-1050 C and pressures of 1-10 atm for 30-60 minutes. A capacitance probe, measuring the dew point of the gas stream, was used to follow reaction progress. Experiments were also conducted using a terrestrial basalt similar to some lunar mare samples. Minnesota Lunar Simulant (MLS-1) contains 13.29 wt. percent FeO, 2.96 wt. percent Fe2O3, and 6.56 wt. percent TiO2. The major minerals include plagioclase, pyroxene, olivine, ilmenite, and magnetite. The rock was ground and seived, and experiments were run on the less than 74- and 500-1168-micron fractions. Experiments were also conducted on less than 74-micron powders of olivine, pyroxene, synthetic ilmenite, and TiO2. The terrestrial rock and mineral samples were reduced with flowing hydrogen at 1100 C in a microbalance furnace, with reaction progress monitored by weight loss. Experiments were run at atmospheric pressure for durations of 3-4 hr. Solid samples from both sets of experiments were analyzed by Mossbauer spectroscopy, petrographic microscopy, scanning electron microscopy, tunneling electron microscopy, and x-ray diffraction. Apollo 17 soil 78221 was examined for evidence of natural reduction in the lunar environment. This sample was chosen based on its high maturity level (I sub s/FeO = 93.0). The FeO content is 11.68 wt. percent and the TiO2 content is 3.84 wt. percent. A polished thin section of the 90-150 micron size fraction was analyzed by petrographic microscopy and scanning electron microscopy.

Allen, C. C.↗

Preliminary Examination of Returned Samples From Bennu Using Quantitative Particle Analysis in the Scanning Electron Microscope

The sample of regolith collected from asteroid Bennu by NASA’s OSIRIS-REx spacecraft will land in Utah on September 24, 2023. A 100-mg aliquot of fine Bennu dust adhering to the internal surfaces of the sample return capsule and associated hardware will be collected by curation staff during disassembly and analyzed immediately by members of the sample analysis team in a “Quick-Look” (Q-L) procedure. The Q-L objectives are (1) to provide images for release to the public to inform on the nature of the returned sample, and (2) to perform a reconnaissance investigation of the mineralogic characteristics of the returned material for science purposes. We will determine the minerals that occur in the dust, assess their diversity, and determine relative abundances at the >5% level using a combination of optical microscopy, Fourier-transform infrared spectroscopy, X-ray powder diffraction, and field-emission scanning electron microscopy (SEM). Here we describe the procedures and techniques developed for the Q-L analyses using analog samples analyzed by SEM equipped with energy dispersive X-ray spectroscopy (EDX). To test these techniques, we have applied them to several samples, including powders of the Murchison (Fig. 1) and Orgueil meteorites, as well as simulant samples prepared by the mission.

OSIRIS-REx↗

Dynamical diffraction imaging (topography) with X-ray synchrotron radiation

By contrast to electron microscopy, which yields information on the location of features in small regions of materials, X-ray diffraction imaging can portray minute deviations from perfect crystalline order over larger areas. Synchrotron radiation-based X-ray optics technology uses a highly parallel incident beam to eliminate ambiguities in the interpretation of image details; scattering phenomena previously unobserved are now readily detected. Synchrotron diffraction imaging renders high-resolution, real-time, in situ observations of materials under pertinent environmental conditions possible.

Kuriyama, M.↗

Microwave diagnostic for the determination of the electron temperature of a low density shock-heated argon plasma

The diffraction, defocusing and beam bending effects of microwaves transmitted through a bounded shock-heated argon plasma with low electron density are investigated with the purpose of developing an accurate method for electron temperature (Te) determination. This report describes the evaluation technique and presents results for an argon plasma with pressure between 3 and 10 torr, and T2 between 5500 and 9500 K. The electron temperature values obtained have a range of uncertainty between -20% and +10% only. The electron temperature is equal or lower by approximately 1000 K in comparison to the heavy particle temperature (T2).

Schneider, C. P.↗

Space radiation effects on poly(aryl-ether-ketone) thin films and composites

The purpose of this study was to assess the space durability of poly(aryl-ether-ketone) (PEEK) in the forms of films and graphite fiber reinforced composites. The influence of the film's crystallinity on electron radiation stability was evaluated using X-ray diffraction, DSC, FTIR, and mechanical property tests. The mechanical properties of the composites material were evaluated after electron radiation and after electron radiation followed by thermal cycling simulating 30 years in geosynchronous orbit.

Funk, Joan G.↗