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At least 181 records · Page 10
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Universal mechanical exfoliation of large-area 2D crystals

Two-dimensional materials provide extraordinary opportunities for exploring phenomena arising in atomically thin crystals. Beginning with the first isolation of graphene, mechanical exfoliation has been a key to provide high-quality two-dimensional materials, but despite improvements it is still limited in yield, lateral size and contamination. Here we introduce a contamination-free, one-step and universal Au-assisted mechanical exfoliation method and demonstrate its effectiveness by isolating 40 types of single-crystalline monolayers, including elemental two-dimensional crystals, metal-dichalcogenides, magnets and superconductors. Most of them are of millimeter-size and high-quality, as shown by transfer-free measurements of electron microscopy, photo spectroscopies and electrical transport. Large suspended two-dimensional crystals and heterojunctions were also prepared with high-yield. Enhanced adhesion between the crystals and the substrates enables such efficient exfoliation, for which we identify a gold-assisted exfoliation method that underpins a universal route for producing large-area monolayers and thus supports studies of fundamental properties and potential application of two-dimensional materials.

36 MATERIALS SCIENCE↗
NASA NTRS2002

Distributed I/O Control System Implementation for the 1238 Optical Witness Sample Thermoelectric Quartz Crystal Microbalance Thermal Vacuum Bakeout Chamber

The 1238 Thermal Vacuum Bakeout Chamber is used to test materials to determine if they meet space program contamination requirements. The system was previously manual in its operation, in that there was no supervisory control system and therefore, no means for automated operation. Marshall Space Flight Center (MSFC) requested that its operation be automated. The subsequent process implemented involved a hybrid scenario that included existing hardware, a distributed input and output (I/O) system and a graphical user interface (GUI).

Randy K. Buchanan↗
DOE OSTI2021

Oxygen isotope ratios in zircon and garnet: A record of assimilation and fractional crystallization in the Dinkey Dome peraluminous granite, Sierra Nevada, California

Abstract The 119 Ma Dinkey Dome pluton in the central Sierra Nevada Batholith is a peraluminous granite and contains magmatic garnet and zircon that are complexly zoned with respect to oxygen isotope ratios. Intracrystalline SIMS analysis tests the relative importance of magmatic differentiation processes vs. partial melting of metasedimentary rocks. Whereas δ18O values of bulk zircon concentrates are uniform across the entire pluton (7.7‰ VSMOW), zircon crystals are zoned in δ18O by up to 1.8‰, and when compared to late garnet, show evidence of changing magma chemistry during multiple interactions of the magma with wall rock during crustal transit. The evolution from an early high-δ18O magma [δ18O(WR) = 9.8‰] toward lower values is shown by high-δ18O zircon cores (7.8‰) and lower δ 18O rims (6.8‰). Garnets from the northwest side of the pluton show a final increase in δ18O with rims reaching 8.1‰. In situ REE measurements show zircon is magmatic and grew before garnets. Additionally, δ18O in garnets from the western side of the pluton are consistently higher (avg = 7.3‰) relative to the west (avg = 5.9‰). These δ18O variations in zircon and garnet record different stages of assimilation and fractional crystallization whereby an initially high-δ18O magma partially melted low-δ18O wallrock and was subsequently contaminated near the current level of emplacement by higher δ18O melts. Collectively, the comparison of δ18O zoning in garnet and zircon shows how a peraluminous pluton can be constructed from multiple batches of variably contaminated melts, especially in early stages of arc magmatism where magmas encounter significant heterogeneity of wall-rock assemblages. Collectively, peraluminous magmas in the Sierran arc are limited to small <100 km2 plutons that are intimately associated with metasedimentary wall rocks and often surrounded by later and larger metaluminous tonalite and granodiorite plutons. The general associations suggest that early-stage arc magmas sample crustal heterogeneities in small melt batches, but that with progressive invigoration of the arc, such compositions are more effectively blended with mantle melts in source regions. Thus, peraluminous magmas provide important details of the nascent Sierran arc and pre-batholithic crustal structure.

Geochemistry & Geophysics↗
NASA NTRS2005

Thruster Plume Plasma Diagnostics: A Ground Chamber Experiment for a 2-Kilowatt Arcjet

Although detailed near field (0 to 3 cm) information regarding the exhaust plume of a two kilowatt arc jet is available (refs. 1 to 6), there is virtually little or no information (outside of theoretical extrapolations) available concerning the far field (2.6 to 6.1 m). Furthermore real information about the plasma at distances between (3 to 6 m) is of critical importance to high technology satellite companies in understanding the effect of arc jet plume exhausts on space based power systems. It is therefore of utmost importance that one understands the exact nature of the interaction between the arc jet plume, the spacecraft power system and the surrounding electrical plasma environment. A good first step in understanding the nature of the interactions lies in making the needed plume parameter measurements in the far field. All diagnostic measurements are performed inside a large vacuum system (12 m diameter by 18 m high) with a full scale arc jet and solar array panel in the required flight configuration geometry. Thus, necessary information regarding the plume plasma parameters in the far field is obtained. Measurements of the floating potential, the plasma potential, the electron temperature, number density, density distribution, debye length, and plasma frequency are obtained at various locations about the array (at vertical distances from the arc jet nozzle: 2.6, 2.7, 2.8, 3.2, 3.6, 4.0, 4.9, 5.0, 5.4, 5.75, and 6.14 m). Plasma diagnostic parameters are measured for both the floating and grounded configurations of the arc jet anode and array. Spectroscopic optical measurements are then acquired in close proximity to the nozzle, and contamination measurements are made in the vicinity of the array utilizing a mass spectrometer and two Quartz Crystal Microbalances (QCM's).

Galofaro, Joel T.↗
NASA NTRS1998

Effects of Convective Solute and Impurity Transport in Protein Crystal Growth

High-resolution optical interferometry was used to investigate the effects of forced solution convection on the crystal growth kinetics of the model protein lysozyme. Most experiments were conducted with 99.99% pure protein solutions. To study impurity effects, approx. 1% of lysozyme dimer (covalently bound) was added in some cases. We show that the unsteady kinetics, corresponding to bunching of growth steps, can be characterized by the Fourier components of time traces of the growth rate. Specific Fourier spectra are uniquely determined by the solution conditions (composition, temperature, and flow rate) and the growth layer source activity. We found that the average step velocity and growth rate increase by approx. I0% with increasing flow rate, as a result of the enhanced solute supply to the interface. More importantly, faster convective transport results in lower fluctuation amplitudes. This observation supports our rationale for system-dependent effects of transport on the structural perfection of protein crystals. We also found that solution flow rates greater than 500 microns/s result in stronger fluctuations while the average growth rate is decreased. This can lead to growth cessation at low supersaturations. With the intentionally contaminated solutions, these undesirable phenomena occurred at about half the flow rates required in pure solutions. Thus, we conclude that they are due to enhanced convective supply of impurities that are incorporated into the crystal during growth. Furthermore, we found that the impurity effects are reduced at higher crystal growth rates. Since the exposure time of terraces is inversely proportional to the growth rate, this observation suggests that the increased kinetics instability results from impurity adsorption on the interface. Finally, we provide evidence relating earlier observations of "slow protein crystal growth kinetics" to step bunch formation in response to nonsteady step generation.

Vekilov, Peter G.↗
NASA NTRS1993

Extrapolation of space weathering processes to other small solar system bodies

A diverse range of processes were invoked as the dominant factor or as important contributory factors in the modification of the optical surface and regolith of the moon. These include impact vitrification by large and small projectiles, solar wind implantation and the reduction of oxidized iron during energetic events, sputtering and crystal lattice damage by energetic cosmic rays, shock metamorphism of minerals, mixing of diverse lithologies by impacts, and contamination by external materials. These processes are also potentially important on the rocky surfaces of other small solar system bodies. For icy bodies, several additional processes are also possible, including formation of complex organic compounds from methane and ammonia-bearing ices by ultraviolet irradiation and the condensation of vapor species to form frost layers in the polar or cooler regions of objects at appropriate heliocentric distances. The lunar case, even when completely understood, will not extend in a simple linear fashion to other small rocky objects, nor will the optical surfaces of those objects all be affected to the same degree by each process. The major factors that will control the relative efficacy of a possible mechanism include the efficiency of ejecta retention and the degree to which the regolith materials experience multiple events (primarily a function of body size, escape velocity, and impactor velocities); the mean duration of typical regolith particle exposure at the optical surface and within reach of the micrometeorite, cosmic ray, solar wind, or UV fluxes (a function of the rate and scale of regolith mixing, production, and removal processes); the incident flux of solar (low energy) cosmic rays, solar wind, or UV radiation (inverse square of heliocentric distance) or of galactic (high energy) cosmic rays (slowly increasing flux with heliocentric distance); and the compositional and mineralogical nature of the surface being affected. In general, those processes that depend upon either the retention of impact ejecta or on the presence of multigenerational regoliths should be substantially less effective on smaller bodies with lower escape velocities. However, there are important exceptions to this generalization. For example, a process that involves the hypervelocity impact of small particles into a fine-grained regolith may be able to effectively retain highly shocked or melted material due to the nature of shock wave propagation in such a heterogeneous material.

Gaffey, M. J.↗
NASA NTRS1978

A precision measurement of the X-ray polarization of the Crab Nebula without pulsar contamination

The linear X-ray polarization of the Crab Nebula has been precisely measured at 2.6 keV and 5.2 keV with the OSO 8 graphite crystal polarimeters. The 1.4 ms time resolution of these instruments permitted the removal of any contribution to the polarization from the pulsar. The nebular polarization is 19.2% plus or minus 1.0% at a position angle of 156.4 plus or minus 1.4 deg at 2.6 keV. At 5.2 keV the corresponding results are 19.5% plus or minus 2.8% at 152.6 plus or minus 4.0 deg.

Weisskopf, M. C.↗
NASA NTRSDate not supplied

Removing Contamination from Genesis Sapphire Collectors by Polishing

The Genesis Solar Wind Sample Re-turn Mission used a variety of materials as solar wind (SW) collectors. “Sapphire”, which is single crystal corundum, was ~6.7% of the collector material flown. But, a much higher percentage of Genesis sapphire collectors (SAP) survived the crash of the sample-return capsule as SAP is chemically inert, physically tough, and hard (MOHS 9, by definition). In fact, 39 sapphire fragments of bulk SW collector having areas ≥60 sq mm are available in JSC’s Genesis online catalog, whereas only 1 similarly sized silicon fragment is available (accessed 1/1/2020). In spite of the ease of accessing larger fragments, sapphire has not been popular among Genesis re-searchers because it is an electrical insulator (making SIMS more difficult) and its chemical inertness, high melting point and high hardness precludes the use of many mass-spectroscopic techniques. Recently, as alternative techniques for measuring Genesis samples are developed (e.g., synchrotron TXRF, INAA, laser ablation mass spectroscopy), more researchers are choosing to analyze sapphire. Thus, a number of researchers are actively studying how to best remove contamination from the Genesis sapphire surfaces. This report extends the task in Schmeling et al. that used polishing compounds to remove contamination from Genesis sapphire and focuses on contaminants (welded silicon, aluminum) that current chemical methods find recalcitrant.

M. Schmeling↗
NASA NTRS2001

Satellite Contamination and Materials Outgassing Knowledge base

Satellite contamination continues to be a design problem that engineers must take into account when developing new satellites. To help with this issue, NASA's Space Environments and Effects (SEE) Program funded the development of the Satellite Contamination and Materials Outgassing Knowledge base. This engineering tool brings together in one location information about the outgassing properties of aerospace materials based upon ground-testing data, the effects of outgassing that has been observed during flight and measurements of the contamination environment by on-orbit instruments. The knowledge base contains information using the ASTM Standard E- 1559 and also consolidates data from missions using quartz-crystal microbalances (QCM's). The data contained in the knowledge base was shared with NASA by government agencies and industry in the US and international space agencies as well. The term 'knowledgebase' was used because so much information and capability was brought together in one comprehensive engineering design tool. It is the SEE Program's intent to continually add additional material contamination data as it becomes available - creating a dynamic tool whose value to the user is ever increasing. The SEE Program firmly believes that NASA, and ultimately the entire contamination user community, will greatly benefit from this new engineering tool and highly encourages the community to not only use the tool but add data to it as well.

Minor, Jody L.↗
NASA NTRS1977

Small monopropellant thruster contamination measurement in a high-vacuum low-temperature facility

The contamination that results from the exhaust plume of small thrusters used for attitude control maneuvers can pose severe problems for long-life satellite systems. In order to assess this type of contamination problem, analytical and experimental techniques must be developed. Mass deposition rate measurements of a representative 0.44-N thrust hydrazine thruster were made in a space simulation chamber using five appropriately placed variable-temperature quartz crystal microbalances. The mass deposition rates within the thruster plume were measured while operating the thruster over a wide range of operating parameters, including duty cycles, catalyst bed start temperatures, propellant water variation, as well as thruster aging effects. The contamination measurements were made over a temperature range of 144 to 256 K for all duty cycles. In addition, the nominal duty cycle of 100 msec on and 10 sec off was run at a temperature of 106 K. These data will make possible better prediction of deposition rates of contaminants from thrusters used in satellite systems.

Passamaneck, R. S.↗
NASA NTRS1973

Exhaust plume and contamination characteristics of a bipropellant (MMH/N2O4) RCS thruster

Results are presented for three recent tests in a series of thruster contamination experiments made in liquid helium-cooled environmental facility. The contaminating effects encountered on various materials, surfaces, and components, due to the exhaust products from a 5-pound thrust, bipropellant (MMH/N2O4) thruster are investigated. The angular distribution of plume effects around the periphery of the thruster established by transmittance changes of quartz samples over the wavelength range from 0.2 to 2.0 micrometer is studied, along with mass deposition rates at a specific location measured with a quartz crystal microbalance for three different experiments. Quadrupole mass spectrometer measurements of the exhaust products over the mass number range from 12 to 75; infrared transmittance measurements of contaminated samples for the wavelength range from 2.5 to 15 microns; and infrared transmittance measurements of residue from the thruster nozzle are also considered.

Spisz, E. W.↗
NASA NTRS2001

Vapor Growth of Binary and Ternary Chalcogenides in Preparation for Microgravity Experiments

In the bulk crystal growth of some technologically important semiconducting chalcopyrites, such as ZnTe, CdS, ZnSe and ZnS, vapor growth techniques have significant advantages over melt growth techniques due to the high melting points of these materials. The realization of routine production of high-quality single crystals of these semiconductors requires a fundamental, systematic and in-depth study on the PVT growth process and crystal growth by vapor transport in low gravity offers a set of unique conditions for this study. Previously, two reasons have been put forward to account for this. The first is weight-related reductions in crystal strain and defects. These are thought to be caused by the weight of the crystals during processing at elevated temperatures and retained on cooling, particularly for materials with a low yield strength. The second, and more general, reason is related to the reduction in density-gradient driven convection. The PVT crystal growth process consists of essentially three processes: sublimation of the source material, transport of the vapor species and condensation of the vapor species to form the crystal. The latter two processes can be affected by the convection caused by gravitational accelerations on Earth. Reductions in such convection in low gravity is expected to yield a nearly diffusion-limited growth condition which results in more uniform growth rates (on the microscopic scale) and hence greater crystalline perfection and compositional homogeneity. The reduction of convective contamination by performing flight experiments in a reduced gravity environment will help to understand the relation between fluid phase processes (growth parameters) and defect and impurity incorporation in grown crystals.

Su, C.↗
NASA NTRS2001

Vapor Growth of Binary and Ternary Chalcogenides in Preparation for Microgravity Experiments

In the bulk crystal growth of some technologically important semiconducting chalcopyrites, such as ZnTe, CdS, ZnSe and ZnS, vapor growth techniques have significant advantages over melt growth techniques due to the high melting points of these materials. The realization of routine production of high-quality single crystals of these semiconductors requires a fundamental, systematic and in-depth study on the PVT growth process and crystal growth by vapor transport in low gravity offers a set of unique conditions for this study. Previously, two reasons have been put forward to account for this. The first is weight-related reductions in crystal strain and defects. These are thought to be caused by the weight of the crystals during processing at elevated temperatures and retained on cooling, particularly for materials with a low yield strength. The second, and more general, reason is related to the reduction in density-gradient driven convection. The PVT crystal growth process consists of essentially three processes: sublimation of the source material, transport of the vapor species and condensation of the vapor species to form the crystal. The latter two processes can be affected by the convection caused by gravitational accelerations on Earth. Reductions in such convection in low gravity is expected to yield a nearly diffusion-limited growth condition which results in more uniform growth rates (on the microscopic scale) and hence greater crystalline perfection and compositional homogeneity. The reduction of convective contamination by performing flight experiments in a reduced gravity environment will help to understand the relation between fluid phase processes (growth parameters) and defect and impurity incorporation in grown crystals.

Su, Ching-Hua↗
DOE OSTI2022

Deciphering the Distribution and Crystal-Chemical Environment of Arsenic, Lead, Silica, Phosphorus, Tin, and Zinc in a Porous Ferrihydrite Grain Using Transmission Electron Microscopy and Atom Probe Tomography

Here the interaction of contaminants and nutrients with soil constituents is controlled by processes in intergranular and intragranular pore spaces of organic matter or/and common secondary minerals such as ferrihydrite, ~Fe 3+ 10 O 14 (OH) 2 . This contribution shows that distribution and clustering of the contaminants As, P, Pb, Si, Sn, and Zn in a porous ferrihydrite grain is greatly affected by the heterogeneous size distribution and chemical composition of the pores as well as the ability of their polyhedra to polymerize with the same type of polyhedron. Transmission electron microscopy (TEM) and atom probe tomography (APT) studies are conducted on focused ion beam (FIB) sections extracted from a porous ferrihydrite grain from the smelter-impacted topsoil in Sudbury, Ontario, Canada. The ferrihydrite grain has pore spaces ranging in diameter from tens to hundreds of nanometers. TEM and scanning-TEM studies indicate that the surfaces of the pore walls are enriched in Si. APT data in conjunction with First Near Neighbor (1NN) analyses indicate different degrees of clustering of Pb, As, Sn, Zn, Si, and P within the sample and selected domains. Careful evaluations of 3D atomic plots and 1NN distances indicates the occurrence of polymerized arsenite-, silica-, Sn-, and Zn-polyhedra within pore spaces of the ferrihydrite. Deciphering adsorption, polymerization, and nucleation processes in porous Fe-(hydr)oxides and other soil constituents requires multianalytical approaches and, in this regard, we discuss the advantages and disadvantages of the combination of TEM and APT for characterizing complex environmental samples at the atomic to nanometer scale.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1984

Extreme incompatibility of Pb during the crystallization of magmatic iron meteorites

The partitioning behavior of Pb in the three-phase system metal-troilite-sulfide liquid was investigated. Microscopic examination and electron microprobe analysis of a polished section showed three phases--Fe metal, troilite and an Fe-S-Pb-O metallic liquid. The Pb concentration of the metallic liquid was 1.4 wt.%; the Pb contents of both the troilite and the Fe metal were below the detection limit of the electron probe. To better define the Pb concentrations of the solid phases, the same sample was analyzed for Pb and Fe using the M.I.T., Harvard and Brown ion microprobe. Even at this level of precision, some conclusions and speculations are possible: (1) The D(Pb) (troilite/metallic liquid) is low (.01 to .001) and, contrary to expectation, troilite, like metal, excludes Pb very effectively during the crystallization of metallic liquids; (2) Pb in iron meteorites is conceivably concentrated in trace phases which are less susceptible to contamination than metal and troilite; and (3) taken at face value D(Pb)(metal/troilite) is 0.1, but given the Pb and Fe ion yields from simple endmember phases (Fe, FeS, Pb, PbS), this D is more likely to be 0.05 to 0.03.

Jones, J. H.↗
NASA NTRS1986

Mapping of carbon concentrations in the Allende meteorite with the C-12(d,p)C-13 method

Carbon concentrations in a 4.2 x 4.2 mm area of the Allende meteorite were mapped with the C-12(d,p)C-13 nuclear method. The x,y resolution perpendicular to the deuteron beam was 65 microns; the depth resolution was 0.6 micron. The matrix of the meteorite contains about 1 wt pct carbon, which is uniformly distributed at the 65-micron level of resolution. The matrix contains most, perhaps close to all, C of this meteorite. The coarse-grained constituents, such as chondrules, show a very strong enhancement of C in the depth range 2 to about 0 micron; the matrix does not show this enhancement. The enhancement may be due to contamination of the coarse-grained areas or else to migration of C in solid solution from the interiors of comparatively large crystals to their freshly polished surfaces.

Van Der Stap, C. A. H.↗
DOE OSTI2023

Investigations towards incorporation of Eu 3+ and Cm 3+ during ZrO 2 crystallization in aqueous solution

Nuclear energy provides a widely applied carbon-reduced energy source. Following operation, the spent nuclear fuel (SNF), containing a mixture of radiotoxic elements such as transuranics, needs to be safely disposed of. Safe storage of SNF in a deep geological repository (DGR) relies on multiple engineered and natural retention barriers to prevent environmental contamination. In this context, zirconia (ZrO 2 ) formed on the SNF rod cladding, could be employed as an engineered barrier for immobilization of radionuclides via structural incorporation. This study investigates the incorporation of Eu 3+ and Cm 3+ , representatives for trivalent transuranics, into zirconia by co-precipitation and crystallization in aqueous solution at 80 °C. Complementary structural and microstructural characterization has been carried out by powder X-ray diffraction (PXRD), spectrum imaging analysis based on energy-dispersive X-ray spectroscopy in scanning transmission electron microscopy mode (STEM-EDXS), and luminescence spectroscopy. The results reveal the association of the dopants with the zirconia particles and elucidate the presence of distinct bulk and superficially incorporated species. Hydrothermal aging for up to 460 days in alkaline media points to great stability of these incorporated species after initial crystallization, with no indication of phase segregation or release of Eu 3+ and Cm 3+ over time. These results suggest that zirconia would be a suitable technical retention barrier for mobilized trivalent actinides in a DGR.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRSDate not supplied

Obtaining cryogenic molecular transport data for analysis

The James Webb Space Telescope (JWST) has a primary mirror, made of 18 segments, and a secondary mirror (SM) that are used to direct the light of desired targets. While on orbit, the secondary mirror assembly (SMA) was stowed for approximately 10 days and was subject to molecular contamination outgassing from the cavity of the secondary mirror support structure (SMSS) in-board hinge (IBH) which contains cables, motors, resolvers, and coatings. The main concern during this period before SMA deployment is the accumulation of ice due to the lack of a heater on the SMA. The temperature differentials between the IBH surfaces and SMA could cause redistribution of contaminants. To address this concern, single layer insulation (SLI) was used to create adequate venting and path redirection of outgassing from the IBH. Two separate thermal vacuum tests were performed to quantify this contamination: one Z307 ASTM E 1559 materials test of the radiator paint used on the motor of the IBH and a separate test on a primary mirror backplane assembly (PMBA) qualification engineering test unit (ETU) of the IBH. These tests approximately followed the predicted SMA pre-deployment thermal environment. To quantify source rates in case of a leak, the motor and resolver sides were separated and quartz crystal microbalances (QCM) were used to measure the deposition of water. The SLI redesign and implementation and outgassing measurements to understand leak effects from the IBH were essential to mitigate the deposition of contamination on the SMA.

James Webb Space Telescope, contamination, cleanro↗