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At least 1,477 records · Page 82
All sourcesNASA NTRSDOE OSTI
NASA NTRS1988

Liquid encapsulated float zone process and apparatus

The process and apparatus for growing crystals using float zone techniques are described. A rod of crystalline materials is disposed in a cylindrical container, leaving a space between the rod and container walls. This space is filled with an encapsulant, selected to have a slightly lower melting point than the crystalline material. The rod is secured to a container end cap at one end and to a shaft at its other end. A piston slides over the rod and provides pressure to prevent loss of volatile components upon melting of the rod. Prior to melting the rod the container is first heated to melt the encapsulant, with any off-gas from this step being vented to a cavity behind the piston. The piston moves slightly forward owing to volume change upon melting of the encapsulant, and the vent passageway is closed. The container is then moved longitudinally through a heated zone to progressively melt sections of the rod as in conventional float zone processes. The float zone technique may be used in the microgravity environment of space.

Naumann, Robert J.↗
NASA NTRS1980

On the barrier to crystal nucleation in lunar glasses

The paper describes an analytical method for calculating in detail the size distributions of small crystallites and nuclei in supercooled liquids as they are being quenched to form a glass and subsequently reheated above the glass transition to produce crystallization. This method is applied to experiments performed using differential thermal analysis (DTA) to estimate the barriers to crystal nucleation and the cooling rates required to form glasses or bodies with various degrees of crystallinity. DTA data and derived nucleation barriers are reported for anorthite and for the following lunar compositions: 15498, 15418, matrix and intrusion compositions of breccia 15286, Apollo 15 green glass, Luna 24 highland basalt, and 65016.

Yinnon, H.↗
NASA NTRS1991

Comparative study of flux pinning, creep and critical currents between YBaCuO crystals with and without Y2BaCuO5 inclusions

In the Y-Ba-Cu-O system, YBa2Cu3O(x) phase is produced by the following peritectic reaction: Y2BaCuO5 + liquid yields 2YBa2Cu3O(x). Through the control of processing conditions and starting compositions, it becomes possible to fabricate large crystals containing fine Y2BaCuO5(211) inclusions. Such crystals exhibit Jc values exceeding 10000 A/sq cm at 77 K and 1T. Recently, researchers developed a novel process which can control the volume fraction of 211 inclusions. Elimination of 211 inclusions is also possible. In this study, researchers prepared YBaCuO crystals with and without 211 inclusions using the novel process, and compared flux pinning, flux creep and critical currents. Magnetic field dependence of Jc for YBaCuO crystals with and with 211 inclusions is shown. It is clear that fine 211 inclusions can contribute to flux pinning. It was also found that flux creep rate could be reduced by increasing flux pinning force. Critical current density estimates based on the conventional flux pinning theory were in good agreement with experimental results.

Murakami, Masato↗
NASA NTRS1971

Photoemf in cadmium sulfide

Theoretical and experimental investigations on CdS single crystals and CuxS:CdS photovoltaic cells prepared from CdS single crystals by a chemical-dip procedure are described. The studies are aimed at clarifying cell mechanisms which affect key cell properties (efficiency, reliability, and lifetime) by examining the properties of intrinsic and extrinsic defects in the junction and surface regions and their effects on carrier transport through these regions. The experimental research described includes studies of thermal, infrared, and field quenching of acceptor-doped CdS crystals; investigation of optical and electrical properties of CuxS:CdS photovoltaic cells (current-voltage characteristics, spectral distribution of photocurrent and photovoltage) and the dependence of these properties on temperature and light intensity; measurement of changes, as a result of heat treatment in ultrahigh vacuum, in the spectral distribution of photoconductivity at room temperature and liquid nitrogen temperature, the luminescence spectrum at liquid nitrogen temperature, and the thermally stimulated current curves of CdS crystals; determination of the effect of irradiation with 150 keV (maximum) X-rays on the spectral distribution of photoconductivity and thermally-stimulated current of CdS crystals; and studies of the effect of growth conditions on the photoconductive properties of CdS crystals.

Boeer, K. W.↗
DOE OSTI2024

Synthesis, disorder and Ising anisotropy in a new spin liquid candidate PrMgAl 11 O 19

Here we report the successful synthesis of large single crystals of triangular frustrated PrMgAl 11 O 19 using the optical floating zone technique. Single crystal x-ray diffraction (XRD) measurements unveiled the presence of quenched disorder within the mirror plane, specifically ~7% of Pr ions deviating from the ideal 2d site towards the 6h site. Magnetic susceptibility measurements revealed an Ising anisotropy with the c-axis being the easy axis. Despite a large spin–spin interaction that develops below ~10 K and considerable site disorder, the spins do not order or freeze down to at least 50 mK. The availability of large single crystals offers a distinct opportunity to investigate the exotic magnetic state on a triangular lattice with an easy axis out of the plane.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Iron isotope fractionation between solid and liquid metal in the Fe-P±Ni system: Experimental constraints and implications for meteorites

Iron meteorites record a range of Fe isotope compositions that hold valuable information regarding the evolution of their parent bodies. Interpreting this isotopic variability, however, requires experimental constraints on the equilibrium isotope fractionation between phases. It is thought that the cores of many iron meteorite parent bodies experienced fractional crystallization, during which crystallization of solid iron-nickel occurs from an increasingly non-metal-rich liquid alloy. Phosphorus is one component of this alloy, and this study provides the first constraints on Fe-isotope fractionation between solid and liquid alloys in the Fe-Ni-P system. Experiments comprising Fe and P show a clear enrichment in the light isotopes of Fe in the liquid phase, which increases with the amount of phosphorus. Nickel-bearing samples are offset from the trend defined by Ni-free experiments, which is accounted for by the change in the solid alloy phase from a body-centered cubic to face-centered cubic structure upon the addition of Ni. The increasing light isotope enrichment of the liquid with increasing P content suggests interstitial solution of P, which is known to lengthen Fe-Fe bonds in Fe-P liquids (Waseda and Shiraishi 1977). Results suggest a negligible effect of P on Fe isotope fractionation during planetesimal core crystallization. Iron isotopes may, however, prove useful for identifying the petrogenesis of schreibersite in pallasites and iron meteorites.

58 GEOSCIENCES↗
NASA NTRSDate not supplied

Icing Physics Studies Using the 3D SIDRM Test Article: Aerodynamic and Supercooled Liquid Icing Analysis

In-flight icing is an important safety issue and is a factor that affects aircraft design and performance. Newer regulations are driving a need for improvements in airframe and engine icing simulation capability. Experimental data is required for development of icing physics models and simulation validation. To that end, this paper discusses analyzed data from icing tests conducted with a 3D test article in 2022 at the NASA Icing Research Tunnel. The test article, whose geometry is representative of an inter-compressor duct and strut region of a turbofan engine, has been designed and constructed to study the physics of supercooled water icing and ice crystal icing. The surfaces of the Simulated Inter-compressor Duct Research Model (SIDRM) can be heated to simulate the warm surfaces of the turbofan inter-compressor duct. The test article is instrumented with pressure taps, heaters, heat flux gauges, and thermocouples, while a 3D laser scanner, cameras, and a scale to measure ice mass were utilized to characterize the icing behavior. The aim of these tests was to generate ice accretions on the SIDRM test article under well-characterized supercooled liquid icing and ice crystal icing conditions. This paper discusses measurements related to aerodynamic tests and supercooled liquid icing tests that were conducted. Aerodynamic measurements were analyzed and compared to computational simulations and were found to be in good agreement for the range of airspeeds (50 to 230 knots) and angles of attack (0 to 4°) tested. Various parametric sweeps were conducted during the supercooled liquid icing portion of the test entry (cloud median volumetric diameter ranged from 15 to 90 µm, total air temperature from -3 to -17 °C, angle of attack from 0 to 4°, and accretion time from 5 to 20 min). These sweeps were performed to measure that parameter’s impact on ice accretion size, location, characteristics (such as glaze/rime ice and shedding behavior), and test article surface temperature. Analysis of the test data showed that clouds composed of larger drops, colder air temperatures, smaller angles of attack, and longer spray times were the primary parameters that resulted in accretions with greater ice mass. Test article angle of attack and cloud droplet size influenced the location of ice accretion as these two parameters directly impact collection efficiency. With respect to icing characteristics, total air temperature dictated icing type, and smaller cloud drop size along with warmer air temperatures resulted in greater amounts of ice shedding. Surface temperature increased during ice accretion from the release of latent (fusion) heat, where total air temperature and cloud drop size impacted the amount of surface temperature change. The icing measurements collected during the SIDRM tests will be used to develop and validate 3D computational engine icing tools, such as GlennICE, that predictively assesses the onset and growth of ice. One of the goals of the sponsoring NASA project is to develop simulation models and tools that can assist in the design and certification of engines for flight in icing conditions in a cost‑effective way.

supercooled liquid icing↗
NASA NTRS1994

The Divnoe meteorite: Petrology, chemistry, oxygen isotopes and origin

The Divnoe meteorite is an olivine-rich primitive achondrite with subchondritic chemistry and mineralogy. It has a granoblastic, coarse-grained, olivine groundmass (CGL: coarse-grained lithology) with relatively large pyroxene-plagioclase poiklitic patches (PP) and small fine-grained domains of an opaque-rich lithology (ORL). Both PP and ORL are inhomogeneously distributed and display reaction boundaries with the groundmass. Major silicates, olivine Fa(20-28) and orthopyroxyene Fs(20-28 Wo(0.5-2.5), display systematic differences in composition between CGL and ORL as well as a complicated pattern of variations within CGL. Accessory plagioclase has low K content and displays regular igneous zoning with core compositions An(40-45) and rims An(32-37). The bulk chemical composition of Divnoe is similar to that of olivine-rich primitive achondrites, except for a depletion of incompatible elements and minor enrichment of refractory siderophiles. Oxygen isotope compositions for whole-rock and separated minerals from Divnoe fall in a narrow range, with mean delta O-18 = +4.91, delta O-17 = +2.24, and Delta O-17 = -0.26 +/- 0.11. The isotopic composition is not within the range of any previously recognized group but is very close to that of the brachinites. To understand the origin of Divnoe lithologies, partial melting and crystallization were modelled using starting compositions equal to that of Divnoe and some chondritic meteorites. It was found that the Divnoe composition could be derived from a chondritic source region by approximately 20 wt% partial melting at Ta approximately 1300 C and log(fO2) = IW-1.8, followed by approximtely 60 wt% crystallization of the partial melt formed, and removal of the still-liquid portion of the partial melt. Removal of the last partial melt resulted in depletion of the Divnoe plagioclase in Na and K. In this scenario, CGL represents the residue of partial melting, and PP is a portion of the partial melt that crystallized in situ. The ORL was formed during the final stages of partial melting by reaction between gaseous sulfur and residual olivine in the source region. A prominent feature of Divnoe is fine micron-scale chemical variations within olivine grains, related to lamellar structures the olivines display. The origin of these structures is not known.

Petaev, M. I.↗
NASA NTRS1972

Experimental petrology and origin of Fra Mauro rocks and soil

Melting experiments over the pressure range 0 to 20 kilobars were conducted on Apollo 14 igneous rocks 14310 and 14072 and on comprehensive fines 14259. The mineralogy and textures of rocks 14310 and 14072 are presumed to be the result of near-surface crystallization. The chemical compositions of the samples show special relationships to multiply-saturated liquids in the system: anorthite-forsterite-fayalite-silica at low pressure. Partial melting of a lunar crust consisting largely of plagioclase, low calcium pyroxene, and olivine, followed by crystal fractionation at the lunar surface is proposed as a mechanism for the production of the igneous rocks and soil glasses sampled by Apollo 14.

Walker, D.↗
DOE OSTI2020

Interface velocity dependent solute trapping and phase selection during rapid solidification of laser melted hypo-eutectic Al-11at.%Cu alloy

Microstructure formation of a hypo-eutectic Al-11Cu (atom percent) alloy during solidification after laser melting has been studied by transmission electron microscopy (TEM). The evolution of the solid-liquid-interface velocity, V SL , during the solidification process has been determined from direct observation by in-situ TEM. This enabled correlating V SL with development of four distinct microstructure zones. Crystal growth mode transitions from planar to cellular, cellular to dendritic, dendritic to cellular, and cellular to planar, have been observed for the accelerating solid-liquid-interface. The transition from coupled two-phase growth to the single-phase growth occurred for V SL = V a = (0.80±0.05) m/s, where V a is the velocity of absolute stability, at the onset of banded morphology grain formation. The in-situ and post-mortem TEM uniquely permitted determination of the non-equilibrium solidus for the rapidly solidifying Al-11Cu alloy. Experimental evidence for solute clustering and chemical ordering tendencies at length scales on the order of ≤ 5nm has been detected in the single-phase regions of the banded grains. The structural features of the single-phase bands have been interpreted as signatures of ‘frozen in’ configurations present in the liquid boundary layer adjacent to the growing crystal, which has a width of about 3nm. Finally, the nano-scale spatiotemporal resolution experimental TEM studies performed here provided quantitative metrics, e.g. the solidification interface velocity dependent solute concentration of the α-Al phase and the near-atomic scale structure in the single-phase bands, that are uniquely suitable for comparison with theory and model predictions for solidification microstructure development in multicomponent alloys after laser melting.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Improved liquid lithium surfaces in the Lithium Tokamak Experiment-β

Advances in vacuum, surface, and lithium conditioning techniques throughout five years of continuous operations in LTX-β have produced mirror-like liquid lithium surfaces and demonstrated the feasibility of high-performance tokamak discharges fully surrounded by liquid metal without significant operational problems. Improvements in conditioning techniques and procedures, including many weeks of baking and accumulation of 70 g of Li, led to reduced residual gasses and clean Li surfaces - all while still maintaining enough operational flexibility for multiple in-vacuum diagnostic upgrades and calibrations. Coatings had a visibly clean appearance, with reflective liquid metal demonstrating good wetting and surface adhesion with films that were now macroscopically thick. Solidified Li showed large crystal grains, while surface science measurements observed reduced impurities in the lithium. Steadily improved plasma performance was achieved with liquid lithium, with discharges able to match solid Li in terms of evolution of I p and n e , including rapid density pumping indicating low recycling. There were indications of moderately increased Li impurity influx, though few significant disturbances by the large liquid surfaces on tokamak operations over hundreds of discharges. Liquid metal plasma facing components are a potential solution to the extreme heat and particle fluxes that could cause unacceptable damage to solid materials, while liquid lithium also has the potential for greatly increased confinement in the low-recycling regime. While many liquid metal approaches are possible, and numerous experiments have been conducted in test stands and small modules in fusion devices, LTX-β is the only tokamak operated while fully surrounded by liquid metal.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2022

Molecular Reaction Imaging of a Surface Recombination Process Explains Performance Variation Among Smooth MoS 2 Photoelectrodes

Transition metal dichalcogenides (TMD) such as WSe 2 and MoS 2 are highly efficient and stable light absorbers in TMD∣I − ,I 3 − ∣Pt liquid junction solar cells. It is generally accepted that TMD crystals with a large fraction of exposed edge sites exhibit lower power conversion efficiencies (PCEs) than apparently smooth crystals. However, one open question is why does the PCE vary significantly from one crystal to another? Answering this critical question could lead to robust syntheses for high quality and uniform TMD samples. In this work, we apply nanoscale photoelectrochemical microscopy techniques to study n-type TMD nanoflake∣I − ,I 3 − ∣Pt cells. Using a combination of near-diffraction-limited photocurrent mapping and molecular reaction imaging techniques, we reveal a previously hidden surface recombination process: photogenerated holes in hidden p-type domains travel micron-scale distances parallel to the solid/liquid interface and preferentially react with iodide at step-edges. The overall efficiency of the nanoflake, as evidenced from whole nanoflake-level photoelectrochemical measurements, is dictated by the size, efficiency, and location of n- and p-type domains. Furthermore, these results provide a unifying view of efficiency losses in smooth TMD photoelectrodes and open the possibility to design electrode architectures that leverage the long-range lateral charge transport property for photoelectrocatalysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1996

The Structural Properties of Vapor Deposited Water Ice and Astrophysical Implications

Films of vapor deposited water ice at low temperature (T<30 K) show a number of interesting structural changes during a gradual warmup. We would like to talk about the structure of the low temperature high density amorphous form of water ice, the process of crystallization, and some recent work on the morphological changes of water ice films at high temperature. The studies of the high density amorphous form are from in-situ electron microscopy as well as numerical simulations of molecular dynamics and have lead to new insights into the physical distinction between this high density amorphous form and the low density amorphous form. For the process of crystallization, we propose a model that describes the crystallization of water ice from the amorphous phase to cubic ice in terms of the nucleation of small domains in the ice. This model agrees well with the behavior of water ice in our electron microscopy studies and finds that pure water above the glass transition is a strong liquid. In more recent work, we have concentrated on temperatures above the crystallization temperature and we find interesting morphological changes related to the decrease in viscosity of the amorphous component in the cubic crystalline regime. Given enough time, we would like to put these results in an astrophysical context and discuss some observed features of the frost on interstellar grains and the bulk ice in comets.

Jenniskens, P.↗
NASA NTRS1998

Semiconductor apparatus utilizing gradient freeze and liquid-solid techniques

Transition metals of Group VIII (Co, Rh and Ir) have been prepared as semiconductor compounds with the general formula TSb.sub.3. The skutterudite-type crystal lattice structure of these semiconductor compounds and their enhanced thermoelectric properties results in semiconductor materials which may be used in the fabrication of thermoelectric elements to substantially improve the efficiency of the resulting thermoelectric device. Semiconductor materials having the desired skutterudite-type crystal lattice structure may be prepared in accordance with the present invention by using vertical gradient freezing techniques and/or liquid phase sintering techniques. Measurements of electrical and thermal transport properties of selected semiconductor materials prepared in accordance with the present invention, demonstrated high Hall mobilities (up to 1200 cm.sup.2.V.sup.-1.s.sup.-1) and good Seebeck coefficients (up to 150 .mu.VK.sup.-1 between 300.degree. C. and 700.degree. C.). Optimizing the transport properties of semiconductor materials prepared from elemental mixtures Co, Rh, Ir and Sb resulted in a substantial increase in the thermoelectric figure of merit (ZT) at temperatures as high as 400.degree. C. for thermoelectric elements fabricated from such semiconductor materials.

Fleurial, Jean-Pierre↗
DOE OSTI2024

In Situ Alloying Enabled by Active Liquid Metal Filler for Self‐Healing Composite Polymer Electrolytes

Abstract Solid inorganics, known for kinetically inhibiting polymer crystallization and enhancing ionic conductivity, have attracted significant attention in solid polymer electrolytes. However, current composite polymer electrolytes (CPEs) are still facing challenges in Li metal batteries, falling short of inhibiting severe dendritic growth and resulting in very limited cycling life. This study introduces Ga 62.5 In 21.5 Sn 16 (Galinstan) liquid metal (LM) as an active liquid alternative to conventional passive solid fillers, aiming at realizing self‐healing protection against dendrite problems. Compared to solid inorganics, for example silica, LM droplets could more significantly reduce polymer crystallinity and enhance Li‐ion conductivity due to their liquid nature, especially at temperatures below the polymer melting point. More importantly, LMs are unraveled as dynamic chemical traps, which are capable of blocking and consuming lithium dendrites upon contact via in situ alloying during battery operation and further inhibiting dendritic growth due to the lower deposition energy barrier of the formed Li‐LM alloy. As a proof of concept, by strategically designing an asymmetric CPE with the active LM filling, a solid‐state Li/LiFePO 4 battery achieves promising full‐cell functionality with notable rate performance and stable cycle life. This active filler‐mediated self‐healing approach could bring new insights into the battery design in versatile solid‐state systems.

Wu, Kai↗
NASA NTRS2005

Synthesizing Diamond from Liquid Feedstock

A relatively economical method of chemical vapor deposition (CVD) has been developed for synthesizing diamond crystals and films. Unlike prior CVD methods for synthesizing diamond, this method does not require precisely proportioned flows of compressed gas feedstocks or the use of electrical discharges to decompose the feedstocks to obtain free radicals needed for deposition chemical reactions. Instead, the feedstocks used in this method are mixtures of common organic liquids that can be prepared in advance, and decomposition of feedstock vapors is effected simply by heating. The feedstock used in this method is a solution comprising between 90 and 99 weight percent of methanol and the balance of one or more other oxyhydrocarbons that could include ethanol, isopropanol, and/or acetone. This mixture of compounds is chosen so that dissociation of molecules results in the desired proportions of carbon-containing radicals (principally, CH3) and of OH, H, and O radicals. Undesirably, the CVD temperature and pressure conditions thermodynamically favor the growth of graphite over the growth of diamond. The H radicals are desirable because they help to stabilize the growing surface of diamond by shifting the thermodynamic balance toward favoring the growth of diamond. The OH and O radicals are desirable because they preferentially etch graphite and other non-diamond carbon, thereby helping to ensure the net deposition of pure diamond. The non-methanol compounds are included in the solution because (1) methanol contains equal numbers of C and O atoms; (2) an excess of C over O is needed to obtain net deposition of diamond; and (3) the non-methanol molecules contain multiple carbon atoms for each oxygen atom and thus supply the needed excess carbon A typical apparatus used in this method includes a reservoir containing the feedstock liquid and a partially evacuated stainless-steel reaction chamber. The reservoir is connected to the chamber via tubing and a needle valve or other suitable flow controller. When the liquid enters the low-pressure environment inside the chamber, it evaporates to form a vapor mixture of the same chemical composition. In addition to the inlet for the feedstock liquid, the chamber is fitted with an outlet connected to a vacuum pump (not shown) through a throttle valve (also not shown) that is automatically controlled to keep the pressure at or near the required value throughout the deposition process. Inside the chamber, a spiral filament made of tungsten, tantalum, graphite, or other high-melting-temperature material is electrically heated to a temperature >2,000 C high enough to cause dissociation of vapor molecules into the aforementioned radicals. A deposition substrate typically, a diamond-polished silicon wafer about 2.5 cm square is positioned about 2 cm away from the filament. The exact location of the substrate is chosen so that the substrate becomes heated by the filament to a deposition temperature in the approximate range of 800 to 1,000 C.

Tzeng, Yonhua↗
NASA NTRS1980

Structure and optical properties of evaporated films of the Cr- and V-group metals

Thin films of Cr, Mo, and W rapidly evaporated in high vacuum (5 x 10 to the -7th torr) onto room-temperature substrates show anomalously low reflectance (compared to bulk samples). From electron and X-ray diffraction and electron microscopy, the normal bcc crystal structure is found, but with very fine grains. Columnar grains about 100 A in diameter were separated by a less dense grain-boundary network about 10-A wide. The measured optical conductivity agrees with an inhomogeneous-medium model that assumes the normal crystalline conductivity for the grain interiors, with model parameters that correlate to the observed columnar grain size. In contrast, V and Nb films rapidly evaporated onto room-temperature substrates have the reflectance of bulk crystalline material. On liquid-nitrogen temperature substrates, however, V and Nb have normal bcc crystal structure but with small flat-plate grains, and the same model, with appropriate parameters, accounts for the optical conductivity. The difference between these two groups apparently depends on residual gases segregated at the grain boundaries in the Cr-group films.

Nestell, J. E., Jr.↗