Evaluation of hydraulic fluids for use in advanced supersonic aircraft First semiannual report
Polyphenyl ether, fluorocarbon, mineral oil, silicone, and halogenated polyaryl evaluation as hydraulic fluids for supersonic aircraft
HYDRAULIC FLUID↗
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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.
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Durable, Low-Surface-Energy Treatments
Chemical treatment for creation of durable, low-surface-energy coatings for glass, ceramics and other protonated surfaces easily applied, and creates very thin semipermanent film with extremely low surface tension. Exhibits excellent stability; surfaces retreated if coating becomes damaged or eroded. Uses include water-repellent surfaces, oil-repellent surfaces, antimigration barriers, corrosion barriers, mold-release agents, and self-cleaning surfaces. Film resists wetting by water, alcohols, hydrocarbon solvents, and silicone oil. Has moderate resistance to abrasion, such as rubbing with cloths, and compression molding to polymers and composite materials.
Willis, Paul B.↗
Effect of environment on fracture toughness of 96 wt pct alumina
An effort is made to deepen understanding of environmental effects on the fracture toughness of an alumina composition that contains a residual glassy phase, by ascertaining the fracture toughness under atmospheric conditions in such varied environments as air distilled water, silicone oil, and liquid nitrogen. Fracture toughness was determined via the single-edge-precracked beam technique. Weibull strength parameters are compared for polished specimens tested both in air and silicone environments.
Choi, Sung R.↗
Interfacial Assembly and Jamming of Polyelectrolyte Surfactants: A Simple Route To Print Liquids in Low-Viscosity Solution
Nanoparticle surfactants (NPSs) assembled at the oil-water interface can significantly lower the interfacial tension and be used to structure liquids. However, to realize the three-dimensional printing of one liquid in another, high-viscosity liquids, for example, silicone oil, have been generally used. In this work, we present a simple, low-cost approach to print water in low-viscosity toluene by using a new type of polyelectrolyte surfactant, sodium carboxymethyl cellulose surfactant (CMCS), that forms and assembles at the oil-water interface. The interfacial activity of CMCSs can be enhanced by tuning parameters, such as pH and concentration, and the incorporation of a rigid ligand affords excellent mechanical strength to the resultant assemblies. With CMCS jammed at the interface, liquids can be easily printed or molded to the desired shapes, with biocompatible walls that can be used to encapsulate and adsorb active materials. This study opens a new pathway to generate complex, all-liquid devices with a myriad of potential applications in biology, catalysis, and chemical separation.
36 MATERIALS SCIENCE↗
Utilizing Controlled Vibrations in a Microgravity Environment to Understand and Promote Microstructural Homogeneity During Floating-Zone Crystal Growth
It has been demonstrated in floating-zone configurations utilizing silicone oil and nitrate salts that mechanically induced vibration effectively minimizes detrimental, gravity independent, thermocapillary flow. The processing parameters leading to crystal improvement and aspects of the on-going modeling effort are discussed. Plans for applying the crystal growth technique to commercially relevant materials, e.g., silicon, as well as the value of processing in a microgravity environment are presented.
Grugel, Richard N.↗
Bond Testing for Effects of Silicone Contamination
In 2003 ATK Thiokol discovered that the smocks and coveralls worn by its operations personnel for safety and contamination control were themselves contaminated with a silicone defoamer and a silicone oil. As a growing list of items have been identified as having this form of contamination, it was desirable to devise a test method to determine if the contamination level detected could cause subsequent processing concerns. The smocks and coveralls could potentially contact bonding surfaces during processing so the test method focused on dry transfer of the silicone from the clothing to the bonding surface.
Plaia, James↗
Space simulation ultimate pressure lowered two decades by removal of diffusion pump oil contaminants during operation
The complex problem why large space simulation chambers do not realize the true ultimate vacuum was investigated. Some contaminating factors affecting diffusion pump performance have been identified and some advances in vacuum/distillation/fractionation technology have been achieved which resulted in a two decade or more lower ultimate pressure. Data are presented to show the overall or individual contaminating effect of commonly used phthalate ester plasticizers of 390 to 530 molecular weight on diffusion pump performance. Methods for removing contaminants from diffusion pump silicone oil during operation and reclaiming contaminated oil by high vacuum molecular distillation are described.
Buggele, A. E.↗
Better vacuum by removal of diffusion-pump-oil contaminants
The complex problem of why large space simulation chambers do not realize true ultimate vacuum was investigated. Some contaminating factors affecting diffusion pump performance were identified, and some advances in vacuum distillation-fractionation technology were achieved which resulted in a two-decade-or-more lower ultimate pressure. Data are presented to show the overall or individual contaminating effects of commonly used phthalate ester plasticizers of 390 to 530 molecular weight on diffusion pump performance. Methods for removing contaminants from diffusion pump silicone oil during operation and for reclaiming contaminated oil by high-vacuum molecular distillation are described. Conceptual self-cleansing designs and operating procedures are proposed for modifying large diffusion pumps into high-efficiency distillation devices. The potential exists for application of these technological advancements to other disciplines, such as medicine, biomedical materials, metallurgy, refining, and chemical (diffusion-enrichment) processing.
Buggele, A. E.↗
Emittance Measurements for a Thin Liquid Sheet Flow
The Liquid Sheet Radiator (LSR) is an external flow radiator that uses a triangular-shaped flowing liquid sheet as the radiating surface. It has potentially much lower mass than solid wall radiators such as pumped loop and heat pipe radiators, along with being nearly immune to micrometeoroid penetration. The LSR has an added advantage of simplicity. Surface tension causes a thin (100-300 microns) liquid sheet to coalesce to a point, causing the sheet flow to have a triangular shape. Such a triangular sheet is desirable since it allows for simple collection of the flow at a single point. A major problem for all external flow radiators is the requirement that the working fluid be of very low (approx. 10(sup -8) torr) vapor pressure to keep evaporative losses low. As a result, working fluids are limited to certain oils (such as used in diffusion pumps) for low temperatures (300-400 K) and liquid metals for higher temperatures. Previous research on the LSR has been directed at understanding the fluid mechanics of thin sheet flows and assessing the stability of such flows, especially with regard to the formation of holes in the sheet. Taylor studied extensively the stability of thin liquid sheets both theoretically and experimentally. He showed that thin sheets in a vacuum are stable. The latest research has been directed at determining the emittance of thin sheet flows. The emittance was calculated from spectral transmittance data for the Dow Corning 705 silicone oil. By experimentally setting up a sheet flow, the emittance was also determined as a function of measurable quantities, most importantly, the temperature drop between the top of the sheet and the temperature at the coalescence point of the sheet. Temperature fluctuations upstream of the liquid sheet were a potential problem in the analysis and were investigated.
Englehart, Amy N.↗
Relative permeabilities for two-phase flow through wellbore cement fractures
Multiple fluids are likely to exist in fractures and flow paths associated with leaky wellbores, including liquids (e.g., crude oil) and gases (e.g., gas exsolved from liquid). These fluids occupy and move through different portions of the pore spaces within the fractures depending on many factors, including fluid properties, fracture size, and the amount of the different fluids. Upward leakage of any phase, through the fracture, can contaminate water-bearing formations, create hazardous surface conditions, and compromise the functionality of the wellbore. Early signs of wellbore leaks may be expressed by anomalous pressure behavior at surface monitoring points on cavern storage wells. These pressure anomalies are difficult to interpret, necessitating knowledge of the factors that affect the multiphase flow in fractures and porous media. These parameters are critical to modeling multiphase flow in fractures. This insight can guide further diagnosis and maximize leak remediation. Here, our study focuses on the relationship of the liquid–gas relative permeabilities for representative variable-aperture wellbore cement fracture. To obtain the relative permeability of each phase, two-phase flow tests were conducted where both fluids were flowing simultaneously through a fractured wellbore cement specimen under a range of factors, namely (1) aperture size, (2) capillary numbers, and (3) viscosity ratio. The flow experiments were conducted under a range of confining stresses and flow velocities, using nitrogen gas and silicone oils (of different viscosities) in a specially designed pressure vessel. The sum of gas and oil relative permeabilities were found to be less than one under all conditions, which indicates that the presence of one phase affects the permeability of the other phase, and vice versa. Since the gas phase flow conditions include a significant inertial flow component in addition to viscous flow, the inertial flow coefficients at different saturation states are presented. The factors affecting the relationship between the relative permeabilities are discussed in detail. A new mathematical model for estimating the relative permeability of wellbore cement fracture is presented and experimentally validated.
58 GEOSCIENCES↗
Novel Shapes of Miscible Interfaces Observed
The dynamics of miscible displacements in a cylindrical tube are being investigated experimentally and numerically, with a view to understand the complex processes that occur, for example, in enhanced oil recovery, hydrology, and filtration. We have observed complex shapes of the interface between two liquids that mix with each other when the less viscous liquid is displaced by the more viscous one in a tube. A less viscous fluid that displaces a more viscous fluid is known to propagate in the form of a "finger," and a flight experiment proposed by Maxworthy et al. to investigate the miscible-interface dynamics is currently being developed by NASA. From the current theory of miscible displacements, which was developed for a porous medium satisfying Darcy's law, it can be shown that in the absence of gravity the interface between the fluids is destabilized and thus susceptible to fingering only when a more viscous fluid is displaced by a less viscous one. Therefore, if the interface is initially flat and the more viscous fluid displaces the less viscous fluid, the interface ought to be stable and remain flat. However, numerical simulations by Chen and Meiburg for such displacement in a cylindrical tube show that the interface is unstable and a finger of the more viscous fluid is indeed formed. Preliminary experiments performed at the NASA Glenn Research Center show that not only can fingering occur when the more viscous fluid displaces a less viscous one in a cylindrical tube, but also that under certain conditions the advancing finger achieves a sinuous or snakelike shape. These experiments were performed using silicone oils in a vertical pipette of small diameter. In the initial configuration, the more viscous fluid rested on top of the less viscous one, and the interface was nominally flat. A dye was added to the upper liquid for ease of observation of the interface between the fluids. The flow was initiated by draining the lower fluid from the bottom of the pipette, at speeds less than 0.1 mm/sec.
Balasubramaniam, Ramaswamy↗
Impurity Levels in Cerium Oxide Microspheres Prepared by Internal Gelation Sol-Gel Methods
Impurity levels were measured in cerium oxide microspheres fabricated by modified internal gelation sol-gel methods. A combination of glow discharge mass spectrometry, electron impact mass spectrometry, combustion gas analysis and instrumental gas analysis were used to assess a wide range of potential elemental impurities. Low concentrations of carbon, nitrogen, and hydrogen impurities in microspheres showed a dependence on how microspheres were washed. Silicon impurities are believed to derive from silicone oil used during sol-gel processing. Spheres washed by the preferred approach had impurity levels below 100 ppm for all elements tested. For applications such as nuclear fuels, sol-gel methods could meet purity specifications as long as metal nitrate feed solutions of sufficient purity are used and microspheres are washed appropriately. In this study, cerium was used as a surrogate for plutonium-238, which is used in radioisotope power systems as a heat source, to determine whether carbon or other impurities were concentrated during internal gelation processing and remained after heat treatments. Analyses indicated low concentrations of impurities in cerium oxide microspheres after sintering steps that were well below documented limits for plutonium-238 oxide fuels. Modified washing methods, combined with a pressurized water treatment, resulted in sintered cerium oxide sol-gel microspheres with low impurity levels.
cerium oxide, sol-gel, internal gelation, microsph↗
Helium Incorporation into Scandium Fluoride, a Model Negative Thermal Expansion Material
Scandium trifluoride is a model negative thermal expansion (NTE) material. Its simple structure can be described as an A-site vacant perovskite, and it shows isotropic NTE over a very wide temperature range (up to ~1100 K), due to transverse vibrational motion of the fluoride. Like many framework NTE materials, it undergoes a phase transition at low pressures, adopting a rhombohedral (R3̅c) structure at >0.7 GPa and 300 K in commonly used nonpenetrating pressure media, such as silicone oil. High pressure X-ray diffraction data and gas uptake/release measurements indicate that, on compression in helium above ~200 K, helium is inserted into ScF 3 to form the defect perovskite He x ScF 3 . The incorporation of helium stiffens the structure and changes its phase behavior. At room temperature, complete filling of the structure with helium does not occur until >1.5 GPa. On compression, a cubic perovskite structure is maintained until ~5 GPa. As the pressure was increased to ~9.5 GPa, a further transition occurred at ~7 GPa. The first transition at ~5 GPa is likely to a tetragonal (P4/mbm) perovskite, but the detailed structure of the perovskite phase formed on compression above ~7 GPa is unclear. Cooling down from 300 to 100 K in helium at ~0.4 GPa leads to an approximate composition of He 0.1 ScF 3 . High pressure neutron diffraction measurements, in the temperature range 15–150 K show that the incorporation of helium increases the pressure at which the cubic (Pm3̅m) to rhombohedral (R3̅c) putative quantum structural phase transition occurs from close to 0 GPa to ~0.2 GPa at 0 K.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Modeling thin layers of analytes on substrates for spectral analysis: use of solid/liquid n and k values to model reflectance spectra
Since solids are only sometimes seen en masse in a pure bulk form, and for liquids other than water almost never, a capability to model reflectance spectra from analytes deposited on various substrates would be highly advantageous. If available, the real, n ( ν ) , and imaginary, k ( ν ) , components of the complex refractive index, n n + i k , can be used to simulate infrared spectra, accounting for reflection, refraction, and absorption phenomena as a function of wavelength. We focus on using the Pacific Northwest National Laboratory (PNNL) derived n / k vectors for solid and liquid analytes deposited as thin layers on different types of substrates including conductors, such as aluminum, and inorganic dielectrics, such as glass. The model is an adaptation of the Monte Carlo ray trace modeling program, TracePro, extended through the use of its macrolanguage. The model is tested using thin films of organic liquids including silicone oil and no. 2 diesel fuel, as well as organic solids such as caffeine and acetaminophen on aluminum and glass. The predicted spectra for the solid films were compared to experimental hemispherical reflectance data measured using a Fourier transform spectrometer with an integrating sphere. The thickness of the calculated layer is a parameter for predicting the (transflectance) spectra and is obtained using the areal density measured from gravimetric methods to generate the thin-layer samples. Comparison of the calculated spectra with experimental hemispherical reflectance data shows excellent agreement, indicating promise for the use of measured n / k data to synthesize reference spectral data. In particular, accounting for the inhomogeneity of the deposits greatly improved the match with experimental data. Finally, the theoretical modeling shows that for thicker layers (ca. 20 to 100 μm) of typical organics possessing moderately strong k values, the longwave infrared features are often saturated and better spectral contrast is obtained from the overtone/combination bands in the shortwave infrared.
42 ENGINEERING↗
Spectroscopic evidence for the Fe3+ spin transition in iron-bearing δ-AlOOH at high pressure
δ-AlOOH has emerged as a promising candidate for water storage in the lower mantle and could have delivered water into the bottom of the mantle. To date, it still remains unclear how the presence of iron affects its elastic, rheological, vibrational, and transport properties, especially across the spin crossover. In this study, we conducted high-pressure X-ray emission spectroscopy experiments on a δ-(Al 0.85 Fe 0.15 ) OOH sample up to 53 GPa using silicone oil as the pressure transmitting medium in a diamond-anvil cell. We also carried out laser Raman measurements on δ-(Al 0.85 Fe 0.15 )OOH and δ-(Al 0.52 Fe 0.48 )OOH up to 57 and 62 GPa, respectively, using neon as the pressure-transmitting medium. Evolution of Raman spectra of δ-(Al 0.85 Fe 0.15 )OOH with pressure shows two new bands at 226 and 632 cm –1 at 6.0 GPa, in agreement with the transition from an ordered ( P 2 1 nm ) to a disordered hydrogen bonding structure ( Pnnm ) for δ-AlOOH. Similarly, the two new Raman bands at 155 and 539 cm –1 appear in δ-(Al 0.52 Fe 0.48 )OOH between 8.5 and 15.8 GPa, indicating that the incorporation of 48 mol% FeOOH could postpone the order-disorder transition upon compression. On the other hand, the satellite peak ( K β') intensity of δ-(Al 0.85 Fe 0.15 )OOH starts to decrease at ~30 GPa and it disappears completely at 42 GPa. That is, δ-(Al 0.85 Fe 0.15 )OOH undergoes a gradual electronic spin-pairing transition at 30–42 GPa. Furthermore, the pressure dependence of Raman shifts of δ-(Al 0.85 Fe 0.15 )OOH discontinuously decreases at 32–37 GPa, suggesting that the improved hydrostaticity by the use of neon pressure medium could lead to a relatively narrow spin crossover. Notably, the pressure dependence of Raman shifts and optical color of δ-(Al 0.52 Fe 0.48 )OOH dramatically change at 41–45 GPa, suggesting that it probably undergoes a relatively sharp spin transition in the neon pressure medium. Together with literature data on the solid solutions between δ-AlOOH and ε-FeOOH, we found that the onset pressure of the spin transition in δ-(Al,Fe)OOH increases with increasing FeOOH content. These results shed new insights into the effects of iron on the structural evolution and vibrational properties of δ-AlOOH. The presence of FeOOH in δ-AlOOH can substantially influence its high-pressure behavior and stability at the deep mantle conditions and play an important role in the deep-water cycle
58 GEOSCIENCES↗
Evaluation of the Barracuda Software Package for Simulating Bubble Motion in Vibrating Liquid-Filled Containers
The commercial software package Barracuda, developed by CPFD Software for simulating particle-laden fluid flows, is evaluated as a means to simulate the motion of bubbles in vibrating liquid-filled containers. Demonstration simulations of bubbles rising due to buoyancy forces in a cylinder filled with silicone oil and angled at 0, 30, 45, and 60 degrees from the vertical were performed by CPFD Software. The results of these simulations are discussed, and the capabilities of Barracuda for simulating bubble motion are assessed. It was determined that at present Barracuda does not meet the needs of the desired application. Further developments that would enable its use for this application are highlighted.
42 ENGINEERING↗
2D IR Microscopy—Technology for Visualizing Chemical Dynamics in Heterogeneous Environments (Final Technical Report)
The primary focus of this project was the design, prototype, and demonstration of a 2D IR microscope. The start date of this project was July 15, 2016 and the project end date was July 14, 2022. In the early years of this project our team designed, prototyped, and completely integrated a homebuilt microscope head with our high-repetition rate 2D IR spectrometer. Once in place our research team focused on characterizing the 2D IR microscope and using it to investigate model systems relevant to energy technologies. As part of this process, we identified two initial chemical systems to use to further develop 2D IR imaging modalities. The first chemical system developed was a room temperature ionic liquid (RTIL) electrolyte system and the second chemical system was a mixture of carbonates and salts developed as a battery electrolyte system. The completion of this project resulted in the full characterization of chemical dynamics in a bulk RTIL system and the demonstration of 2D IR imaging across the RTIL cast as a microdroplet in silicon oil. In addition, we explored the liquid structures and dynamics of organic carbonate mixtures from the vantage point of the vibrational probe, methyl thiocyanate. By the end of the project, we had moved toward in-depth studies of the organic carbonate mixtures.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Development of a Liquid Bridge Model for Particle Agglomeration and Defluidization in Plastic Pyrolysis
Molten plastic that forms during the pyrolysis of plastic or municipal solid waste feedstock can lead to particle agglomeration. A liquid bridge model is developed in MFiX-DEM and validated against a cold flow experiment with glass beads coated with silicone oil. The liquid bridge model is then extended to support an evolving liquid layer thickness for pyrolysis applications. The extended model is used to study the sensitivity of the pyrolysis reactor to solids holdup, flow conditions, and plastic properties.
Banerjee, Subhodeep↗