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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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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Structural transitions of 4:1 methanol–ethanol mixture and silicone oil under high pressure

A 4:1 (volume ratio) methanol–ethanol (ME) mixture and silicone oil are two of the most widely used liquid pressure-transmitting media (PTM) in high-pressure studies. Their hydrostatic limits have been extensively studied using various methods; however, the evolution of the atomic structures associated with their emerging nonhydrostaticity remains unclear. Here, we monitor their structures as functions of pressure up to ∼30 GPa at room temperature using in situ high-pressure synchrotron x-ray diffraction (XRD), optical micro-Raman spectroscopy, and ruby fluorescence spectroscopy in a diamond anvil cell. No crystallization is observed for either PTM. The pressure dependence of the principal diffraction peak position and width indicates the existence of a glass transition in the 4:1 ME mixture at ∼12 GPa and in the silicone oil at ∼3 GPa, beyond which a pressure gradient emerges and grows quickly with pressure. There may be another liquid-to-liquid transition in the 4:1 ME mixture at ∼5 GPa and two more glass-to-glass transitions in the silicone oil at ∼10 GPa and ∼16 GPa. By contrast, Raman signals only show peak weakening and broadening for typical structural disordering, and Raman spectroscopy seems to be less sensitive than XRD in catching these structural transitions related to hydrostaticity variations in both PTM. These results uncover rich pressure-induced transitions in the two PTM and clarify their effects on hydrostaticity with direct structural evidence. The high-pressure XRD and Raman data on the two PTM obtained in this work could also be helpful in distinguishing between signals from samples and those from PTM in future high-pressure experiments.

Chen, Xiehang (ORCID:0000000168541506)↗
DOE OSTI2021

Trichloroethylene replacements for the cleaning of silicone oil used in the internal gelation process

Silicone oil continues to be used as a gelation medium for internal gelation process. Typically, the silicone oil has been removed from the gel spheres using trichloroethylene (TCE) washes. However, TCE is no longer a viable option for large-scale operations because of environmental issues, health concerns, and disposal costs. Furthermore, during the development of a large gelation system at the Y-12 National Security Complex, two new TCE wash replacements were identified. NuSolv SOR-C and FluoSolv WS were used in a number of uranium runs and found to effectively remove silicone oil. NuSolv SOR-C was determined to be the best option.

36 MATERIALS SCIENCE↗
DOE OSTI2021

A transmissive concentrator photovoltaic module with cells directly cooled by silicone oil for solar cogeneration systems

Hybrid concentrator photovoltaic-thermal systems can cogenerate electricity and heat by beam-splitting incoming concentrated light onto photovoltaic cells and a thermal receiver to increase total conversion efficiency and potentially reduce system cost. To demonstrate this, we have designed and prototyped a transmissive spectrum-splitting concentrator photovoltaic module that maximizes solar energy conversion by utilizing the entire solar spectrum. Visible light is collected using infrared-transmissive triple-junction photovoltaic cells to achieve an in-band module efficiency of 43.3% for light of wavelength λ < 873 nm, while 44.2% of out-of-band light with λ > 873 nm is transmitted through for collection by a thermal receiver. During testing on a dual-axis tracked parabolic concentrator dish at up to 166 suns, cell temperatures were maintained at 119 °C or below via a novel active cooling method. This cooling system strictly flows silicone oil directly across both sides of the cells, without inhibiting optical transmission, as verified through experimentation and simulation. The module was validated outdoors for 572 sun·hrs, and achieved a maximum thermal receiver temperature of 180 °C. 86.1% of incident solar power is collected at 166 suns average concentration collectively among the electrical, cooling, and thermal receiver subsystems. The remaining 13.9% is lost to mirror reflectivity, dish shadowing, receiver reflection, and thermal losses. The ability to directly cool the cells with an inert silicone oil offers the potential for reduced system cost relative to previous transmissive hybrid concentrator photovoltaic-thermal systems, including microfluidic-cooled designs. This solar cogeneration capability is valuable in a wide range of commercial and industrial applications.

14 SOLAR ENERGY↗
DOE OSTI2022

On the mechanism of marine fouling-prevention performance of oil-containing silicone elastomers

For many decades, silicone elastomers with oil incorporated have served as fouling-release coating for marine applications. In a comprehensive study involving a series of laboratory-based marine fouling assays and extensive global field studies of up to 2-year duration, we compare polydimethylsiloxane (PDMS) coatings of the same composition loaded with oil via two different methods. One method used a traditional, one-pot pre-cure oil addition approach (o-PDMS) and another method used a newer post-cure infusion approach (i-PDMS). The latter displays a substantial improvement in biofouling prevention performance that exceeds established commercial silicone-based fouling-release coating standards. We interpret the differences in performance between one-pot and infused PDMS by developing a mechanistic model based on the Flory–Rehner theory of swollen polymer networks. Using this model, we propose that the chemical potential of the incorporated oil is a key consideration for the design of future fouling-release coatings, as the improved performance is driven by the formation and stabilization of an anti-adhesion oil overlayer on the polymer surface.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Organic Vacuum Pump Fluids for the Vacuum Pumping of Fusion Power Plants

Vacuum pumps are the heart of the fusion fuel cycle, but most currently proposed pumping technologies are not capable of handling the required flow rates and vacuum pressures. Oil-containing vacuum pumps can readily meet the flow requirements, but vacuum fluids will degrade in fusion-relevant environments due to contact with tritium and exposure to high-energy radiation. Here, in this study, we describe a methodology to screen vacuum fluid candidates and purify these candidate fluids post oxidation, post exposure to deuterium, and post exposure to gamma radiation (<7.5 MGy) to simulate a process in which vacuum fluids can be recovered and regenerated during the fusion fuel cycle. A series of oils, including a highly purified mineral oil, phenyl silicone oil, and a polyphenyl ether, are shown to be suitable candidates for vacuum pumping. Additionally, we describe a simple purification methodology to remove oxidized functionalities and the associated isotopologues induced by contact with deuterium from the candidate vacuum fluids This purification methodology can also be applied to radiological damage with moderate effect. Finally, we demonstrate that the sorbents can be regenerated through electromagnetic microwave digestion.

oxidation↗
DOE OSTI2020

Regenerable non-aqueous basic immobilized amine slurries for removal of CO2 from a gaseous mixture and a method of use thereof

The disclosure provides a composition for the separation of CO2 from a gaseous mixture and a method of use thereof. The composition comprises solid Basic Immobilized Amine Sorbents (BIAS) suspended in silicone oil. The method of use comprises contacting the gaseous mixture with a sorbent slurry comprising Basic Immobilized Amine Sorbents (BIAS) and silicone oil to at least partially absorb the CO2 from the gaseous mixture, and regenerating the BIAS slurry by causing desorption of the CO2.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Strategies for control and mitigation of efflorescence in metakaolin-based geopolymers

Efflorescence can be harmful to material performance as a consequence of microstructural changes due to leaching and carbonation of alkalis. This article identifies mechanisms of efflorescence in metakaolin-based geopolymers, and approaches to reduce free/mobile alkali cations and pore network connectivity, and hence reduce efflorescence. Mechanical, mass transport and microstructural properties are assessed in metakaolin-based geopolymer cements produced using different alkali concentrations in the alkali activator and substitution/addition of blast furnace slag, silica fume, calcium aluminate cement, silicone oil and a dispersive admixture. The most effective strategy to reduce efflorescence results from increasing Si/Al in the geopolymer gel by addition of soluble silicate, silica fume or silicone oil. Addition of calcium aluminate cement or a dispersive admixture also reduce efflorescence, but are less effective. These results confirm that efflorescence may be reduced by controlling the amount of soluble silicates and reducing free alkali cations in geopolymers, providing enhanced performance and durability.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Adhesion and Contact Aging of Acrylic Pressure-Sensitive Adhesives to Swollen Elastomers

Fluid-infused (or swollen) elastomers are known for their antiadhesive properties. The presence of excess fluid at their surface is the main contributor to limiting contact formation and minimizing adhesion. Despite their potential, the mechanisms for adhesion and contact aging to fluid-infused elastomers are poorly understood beyond contact with a few materials (ice, biofilms, glass). This study reports on adhesion to a model fluid-infused elastomer, poly(dimethylsiloxane) (PDMS), swollen with silicone oil. The effects of oil saturation, contact time, and the opposing surface are investigated. Specifically, adhesion to two different adherents with comparable surface energies but drastically different mechanical properties is investigated: a glass surface and a soft viscoelastic acrylic pressure-sensitive adhesive film (PSA, modulus ~25 kPa). Adhesion between the PSA and swollen PDMS [with 23% (w/w) silicone oil] retains up to 60% of its value compared to contact with unswollen (dry) PDMS. In contrast, adhesion to glass nearly vanishes in contact with the same swollen elastomer. Adhesion to the PSA also displays stronger contact aging than adhesion to glass. Contact aging with the PSA is comparable for dry and unsaturated PDMS. Moreover, load relaxation when the PSA is in contact with the PDMS does not correlate with contact aging for contact with the dry or unsaturated elastomer, suggesting that contact aging is likely caused by chain interpenetration and polymer reorganization within the contact region. Closer to full saturation of the PDMS with oil, adhesion to the PSA decreases significantly and shows a delay in the onset of contact aging that is weakly correlated to the poroelastic relaxation of the elastomer. Additional confocal imaging suggests that the presence of a layer of fluid trapped at the interface between the two solids could explain the delayed (and limited) contact aging to the oil-saturated PDMS.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Alteration in micro-mechanical characteristics of wellbore cement fracture surfaces due to fluid exposure

The stiffness of wellbore cement fracture surfaces was measured after exposing to the advective flow of nitrogen, silicone oil, and medium sweet dead crude oil for different exposure periods. The test specimens were extracted from fractured cement cylinders, where the cement fracture surfaces were exposed to the different fluids up to 15 weeks. A nanoindenter with a Berkovich indenter tip was used to measure load-indentation depth data, which was used to extract the elastic modulus (E) and nano-hardness (H) of the cement fracture surfaces. A reduction in the elastic modulus compared with an unexposed specimen were observed in all the specimens. Both elastic modulus and nano-hardness for the specimens exposed to silicone oil were lower than specimens exposed to nitrogen gas and varied with the period of exposure. The elastic modulus and nano-hardness of the specimens exposed to crude oil were the lowest with a significant decrement with the exposure period. The frequency distribution of the nanoindentation measurements shows that the volume-fraction ratio of the two types of cement hydrated nanocomposites for both the unexposed and test specimens is about 70:30%. Phase transformation beneath the indenter is observed for all of the specimens, with more obvious plastic deformation in specimens exposed to crude oil. Analytical measurements (SEM, EDS, FT-IR, and XRD) on exposed cement fracture surfaces reveal different levels of physical and chemical alteration that are consistent with the reduction in stiffness measured by nanoindentation. Furthermore, the study suggests that cement stiffness will decrease due to crude oil exposure, and the fracture will be sensitive to stress and pore pressure with time.

42 ENGINEERING↗
DOE OSTI2025

Experimental Analysis of Advanced Turbine for Supercritical CO2 Power Cycle

An advanced first stage high pressure turbine blade for a supercritical CO2 power cycle is tested in the Big Rig for Aerothermal Stationary Turbine Analysis (BRASTA) annular cascade at the Purdue Experimental Turbine Aerothermal Laboratory (PETAL) high pressure blow down facility alongside a baseline blade for comparison of aerodynamic performance. Both geometries are tested simultaneously using a novel off-axis rig design to allow for the blade geometries to be scaled up to achieve higher Reynolds numbers. The off-axis design necessitates the use of discrete sectors of airfoils, which are designed and additively manufactured in house using an mSLA printer. Printing the blades allows for unique routing of passage for blade surface static pressure taps that contour to the blade shape instead of requiring a straight line view from surface tap to egress, allowing all instrumentation for 15%, 50%, and 85% span to exist in the same passage. A flow conditioning gauze [1] is placed upstream of the blade passages to impart pressure, Mach, and swirl profiles to mimic the rotor relative frame inlet conditions to the blade. Downstream, a sonic valve is used to alter the backpressure to achieve different pressure ratios for different blowdown setpoints. The design of the rig, sonic wheel, and instrumentation are discussed along with the manufacturing and GD&T of the blades with respect to the build-up of this novel experimental apparatus. Initial commissioning data is obtained from inlet total pressure and temperature rakes, blade static pressure taps, and exit total pressure rakes. Oil visualization is performed using a silicone oil mixture containing titanium dioxide and pigmented for contrast of the blade suction side surface with the hub and shroud endwalls. The viscosity of the oil is tuned so that the oil does not fully thin and blow away during the time of the test, and endoscopic cameras are placed in the rig for live monitoring and recording. The preliminary oil visualization and rake profiles are presented, showcasing the operability of this additively manufactured off-axis flow path design.

Tuite, Logan [Purdue University]↗
DOE OSTI2020

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↗
DOE OSTI2024

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↗
DOE OSTI2020

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↗
DOE OSTI2025

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↗
DOE OSTI2020

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↗
DOE OSTI2021

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↗
DOE OSTI2021

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↗