Solvent-free processing of lithium lanthanum zirconium oxide coated-cathodes
A dry process for coating Ni-rich cathode powder with cubic LLZO powder prepared by flame spray pyrolysis.
Durham, Jessica L.↗
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Creating and protecting magnetic nanomaterials
Coated nanofibers and methods for forming the same. A magnetic nanofiber is formed and a barrier coating is deposited on the magnetic nanofiber by atomic layer deposition (“ALD”) process. The coated nanofiber may include a reduced magnetic nanostructure and a barrier coating comprising a first oxide coating on the nanofiber, the coating being non-reactive with the magnetic polymer nanofiber, the barrier coating have a thickness of 2 nm to 12 nm.
Mane, Anil U.↗
Effects of Doping on Thermal Conductivity of Pyrochlore Oxides for Advanced Thermal Barrier Coatings
Pyrochlore oxides of general composition, A2B2O7, where A is a 3(+) cation (La to Lu) and B is a 4(+) cation (Zr, Hf, Ti, etc.) have high melting point, relatively high coefficient of thermal expansion, and low thermal conductivity which make them suitable for applications as high-temperature thermal barrier coatings. The effect of doping at the A site on the thermal conductivity of a pyrochlore oxide La2Zr2O7, has been investigated. Oxide powders of various compositions La2Zr2O7, La(1.7)Gd(0.3)Zr2O7, La(1.7)Yb(0.3)Zr2O7 and La(1.7)Gd(0.15)Yb(0.15)Zr2O7 were synthesized by the citric acid sol-gel method. These powders were hot pressed into discs and used for thermal conductivity measurements using a steady-state laser heat flux test technique. The rare earth oxide doped pyrochlores La(1.7)Gd(0.3)Zr2O7, La(1.7)Yb(0.3)Zr2O7 and La(1.7)Gd(0.15)Yb(0.15)Zr2O7 had lower thermal conductivity than the un-doped La2Zr2O7. The Gd2O3 and Yb2O3 co-doped composition showed the lowest thermal conductivity.
Bansal, Narottam P.↗
Synthesis of multicomponent oxygen evolution reaction coatings via block copolymer templating with vapor- and solution-phase precursors
Porous mixed transition metal oxide heterostructures are promising electrocatalysts due to their high surface area. However, achieving conformal multicomponent oxide coatings with controlled nanoscale architectures remains challenging. Here, we report a synthesis strategy that integrates solution-based swelling infiltration (SBI) with gas-phase sequential infiltration synthesis (SIS) in a block copolymer template to fabricate porous, high-surface-area, conformal mixed-oxide electrocatalytic coatings. In this approach, a PS75-P4VP25 block copolymer (BCP) film is first infiltrated with transition metal acetylacetonate precursors via SBI, followed by exposure to gas phase precursors of ZnO via SIS process. Thermal annealing of the infiltrated BCP films converts them into all-inorganic Fe–ZnO, Fe–Co–ZnO, and Fe–Ni–ZnO coatings. Electrochemical testing on 70 nm thick conformal coatings demonstrates promising oxygen evolution reaction (OER) activity in alkaline media, with mass-specific current densities up to 1.0 × 10 5 mA/g at an overpotential of 330 mV (vs. RHE) at ultralow loading (~0.005 g/cm 2 ). Among the compositions, Fe–Co–ZnO and amorphous Fe–Ni–ZnO show the best OER performance, delivering current densities of 2.00 and 3.04 mA/cm 2 , respectively, compared to 1.52 mA/cm 2 for Fe–ZnO.. This work establishes SBI–SIS as a versatile route for fabricating nm-thin, high-performance multicomponent oxide heterostructures on cost-efficient supports, enabling efficient catalyst utilization in electrochemical energy conversion application.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
High-throughput oxidation screening and down-selection of refractory high entropy alloys in the Al-Cr-Mo-Nb-Ta-Ti system
Rapid experimentation and characterization are ever-present needs in the discovery of high entropy alloys. High entropy alloy systems are difficult to survey with systematic composition sweeps using traditional synthesis methods. The number of distinct compositions in even a four-element system is experimentally intractable. Exploration of these, and higher-element systems, necessitates thermodynamic prediction coupled with an automated sample creation method and a rapid screening methodology to effectively down-select alloys with targeted properties. As a result, a high-throughput method for evaluating the oxidation performance of refractory high entropy alloys was developed and tested. The six-element system of aluminum, chromium, molybdenum, niobium, tantalum, and titanium was evaluated for single phase stability and short-duration oxidation resistance. Target compositions were initially determined via thermodynamic predictions of single-phase stability across a wide temperature range. A twenty-five-sample build plate was produced using directed energy deposition additive manufacturing. After fabrication, the twenty-five 1 cm 3 samples were heat treated and characterized for composition and phase identification. The build plate was exposed to a high temperature oxidizing environment at 1000 °C for three hours. After oxidation, the composition, morphology, and chemistry of the oxides formed were characterized. Of the twenty-five samples produced, nine exhibited a favorable oxidation response, from which a single-phase BCC alloy at a composition of Al 13 Cr 7 Mo 19 Nb 18 Ta 26 Ti 17 was identified as the alloy with the most protective oxidation coating with a thin, adherent oxide scale. Finally, the complete experimental down-selection—from machine setup to final alloy identification—required approximately 45 labor hours, demonstrating a rapid validation for alloy discovery.
Additive manufacturing↗
Transparent switchboard
A tin oxide coating is formed on a plate of glass and the coating is then etched away from the glass in thin lines to form separate electrical conductors which extend to one end of the plate and connect to either a vertical (column) or horizontal (row) position sensing SCR circuit. A thin transparent insulating coating is formed over the oxide layer except at selected touch points which are positioned in a matrix pattern of vertical columns and horizontal rows. Touching one of these points with a finger bridges the thin line between adjacent conductors to activate trigger circuits in the particular row and column sensing circuits associated with the point touched. The row and column sensing circuits are similar and are powered with a low frequency, ac voltage source. The source for the row circuits is 180 out of phase with the source for the column circuits so that one circuit acts as ground for the other during half of the supply voltage cycle. The signals from the sensing circuits are input to a logic circuit which determines the presence of a valid touch, stores a binary matrix number associated with the touched point, signals a computer of the presence of a stored number and prevents storage of a new number before receiving an enable signal from the computer.
Rasmussen, H. P.↗
Programmable Aperture with MEMS Microshutter Arrays
A microshutter array (MSA) has been developed for use as an aperture array for multi-object selections in James Webb Space Telescope (JWST) technology. Light shields, molybdenum nitride (MoN) coating on shutters, and aluminum/aluminum oxide coatings on interior walls are put on each shutter for light leak prevention, and to enhance optical contrast. Individual shutters are patterned with a torsion flexure that permits shutters to open 90 deg. with a minimized mechanical stress concentration. The shutters are actuated magnetically, latched, and addressed electrostatically. Also, micromechanical features are tailored onto individual shutters to prevent stiction. An individual shutter consists of a torsion hinge, a shutter blade, a front electrode that is coated on the shutter blade, a backside electrode that is coated on the interior walls, and a magnetic cobalt-iron coating. The magnetic coating is patterned into stripes on microshutters so that shutters can respond to an external magnetic field for the magnetic actuation. A set of column electrodes is placed on top of shutters, and a set of row electrodes on sidewalls is underneath the shutters so that they can be electrostatically latched open. A linear permanent magnet is aligned with the shutter rows and is positioned above a flipped upside-down array, and sweeps across the array in a direction parallel to shutter columns. As the magnet sweeps across the array, sequential rows of shutters are rotated from their natural horizontal orientation to a vertical open position, where they approach vertical electrodes on the sidewalls. When the electrodes are biased with a sufficient electrostatic force to overcome the mechanical restoring force of torsion bars, shutters remain latched to vertical electrodes in their open state. When the bias is removed, or is insufficient, the shutters return to their horizontal, closed positions. To release a shutter, both the electrode on the shutter and the one on the back wall where the shutter sits are grounded. The shutters with one or both ungrounded electrodes are held open. Sub-micron bumps underneath light shields and silicon ribs on back walls are the two features to prevent stiction. These features ensure that the microshutter array functions properly in mechanical motions. The MSA technology can be used primarily in multi-object imaging and spectroscopy, photomask generation, light switches, and in the stepper equipment used to make integrated circuits and MEMS (microelectromechanical systems) devices.
Moseley, Samuel↗
Control rods for light water reactors
A control rod for a nuclear fuel assembly is described herein that includes a neutron absorbing material having a melting point greater than 1500° C. that does not form a eutectic with a melting point less than 1500° C., and may further include a cladding material having a melting point greater than 1500° C. The cladding material is selected from the group consisting of silicon carbide, zirconium, a zirconium alloy, tungsten, and molybdenum. The absorbing material is selected from the group consisting of Gd2O3, Ir, B4C, Re, and Hf. The metal cladding or the absorbing material may be coated with an anti-oxidation coating of Cr with or without a Nb intermediate layer.
Lahoda, Edward J.↗
Static and dynamic oxidation of Ti-14Al-21Nb and coatings
The oxidation of Ti-14Al-21Nb (wt pct) was studied under static conditions at 649 to 1093 C for as long as 120 hr, and under simulated hypersonic flight (dynamic oxidation) conditions at 982 C for as many as 16 half-hour cycles. Under simulated hypersonic flight conditions heavy oxidation and spalling of the oxide was observed. It was concluded that titanium aluminides used in hypersonic applications must have oxidation-protective coatings. In this preliminary study coatings about 1 micron thick were applied by sputter deposition, from solutions, and from sol-gels. It was found that, because of cracks and porosity, the sputter-deposited coatings did not have sufficient film integrity to shield the alloy. Some of the coatings applied from sol-gels demonstrated film integrity in 1 hr exposures at 982 C.
Wiedemann, K. E.↗
Defect Clustering and Nano-Phase Structure Characterization of Multi-Component Rare Earth Oxide Doped Zirconia-Yttria Thermal Barrier Coatings
Advanced oxide thermal barrier coatings have been developed by incorporating multi- component rare earth oxide dopants into zirconia-yttria to effectively promote the creation of the thermodynamically stable, immobile oxide defect clusters and/or nano-scale phases within the coating systems. The presence of these nano-sized defect clusters has found to significantly reduce the coating intrinsic thermal conductivity, improve sintering resistance, and maintain long-term high temperature stability. In this paper, the defect clusters and nano-structured phases, which were created by the addition of multi-component rare earth dopants to the plasma- sprayed and electron-beam physical vapor deposited thermal barrier coatings, were characterized by high-resolution transmission electron microscopy (TEM). The defect cluster size, distribution, crystallographic and compositional information were investigated using high-resolution TEM lattice imaging, selected area diffraction (SAD), and energy dispersive spectroscopy (EDS) analysis techniques. The results showed that substantial defect clusters were formed in the advanced multi-component rare earth oxide doped zirconia-yttria systems. The size of the oxide defect clusters and the cluster dopant segregation was typically ranging fiom 5 to 50 nm. These multi-component dopant induced defect clusters are an important factor for the coating long-term high temperature stability and excellent performance.
Zhu, Dongming↗
Defect Clustering and Nano-Phase Structure Characterization of Multi-Component Rare Earth Oxide Doped Zirconia-Yttria Thermal Barrier Coatings
Advanced oxide thermal barrier coatings have been developed by incorporating multi-component rare earth oxide dopants into zirconia-yttria to effectively promote the creation of the thermodynamically stable, immobile oxide defect clusters and/or nano-scale phases within the coating systems. The presence of these nano-sized defect clusters has found to significantly reduce the coating intrinsic thermal conductivity, improve sintering resistance, and maintain long-term high temperature stability. In this paper, the defect clusters and nano-structured phases, which were created by the addition of multi-component rare earth dopants to the plasma-sprayed and electron-beam physical vapor deposited thermal barrier coatings, were characterized by high-resolution transmission electron microscopy (TEM). The defect cluster size, distribution, crystallographic and compositional information were investigated using high-resolution TEM lattice imaging, selected area diffraction (SAD), electron energy-loss spectroscopy (EELS) and energy dispersive spectroscopy (EDS) analysis techniques. The results showed that substantial defect clusters were formed in the advanced multi-component rare earth oxide doped zirconia- yttria systems. The size of the oxide defect clusters and the cluster dopant segregation was typically ranging from 5 to 50 nm. These multi-component dopant induced defect clusters are an important factor for the coating long-term high temperature stability and excellent performance.
Zhu, Dongming↗
Sol-gel based oxidation catalyst and coating system using same
An oxidation catalyst system is formed by particles of an oxidation catalyst dispersed in a porous sol-gel binder. The oxidation catalyst system can be applied by brush or spray painting while the sol-gel binder is in its sol state.
Watkins, Anthony N.↗
Sol-gel based oxidation catalyst and coating system using same
An oxidation catalyst system is formed by particles of an oxidation catalyst dispersed in a porous sol-gel binder. The oxidation catalyst system can be applied by brush or spray painting while the sol-gel binder is in its sol state.
Watkins, Anthony N.↗
Oxidation resistant slurry coating for carbon-based materials
An oxidation resistant coating is produced on carbon-base materials, and the same processing step effects an infiltration of the substrate with silicon containing material. The process comprises making a slurry of nickel and silicon powders in a nitrocellulose lacquer, spraying onto the graphite or carbon-carbon substrate, and sintering in vacuum to form a fused coating that wets and covers the surface as well as penetrates into the pores of the substrate. Optimum wetting and infiltration occurs in the range of Ni-60 w/o Si to Ni-90 w/o Si with deposited thicknesses of 25-100 mg/sq. cm. Sintering temperatures of about 1200 C to about 1400 C are used, depending on the melting point of the specific coating composition. The sintered coating results in Ni-Si intermetallic phases and SiC, both of which are highly oxidation resistant.
Smialek, J. L.↗
Sputtered coatings for protection of spacecraft polymers
Kapton polyimide oxidizes at significant rates (4.3x10(-24) gram/incident oxygen atom) when exposed in low Earth orbit to the ram atomic oxygen flux. Ion beam sputter deposited thin films of Al2O3 and SiO2 as well as a codeposited mixture of predominantly SiO2 with a small amount of polytetrafluoroethylene were evaluated and found to be effective in protecting Kapton from oxidation in both laboratory plasma ashing tests as well as in space on board shuttle flight STS-8. A protective film of or = 96 percent SiO2 and or = 4 percent polytetrafluoroethylene was found to be very flexible compared to the pure metal oxide coatings and resulted in mass loss rates that were 0.2 percent of that of the unprotected Kapton. The optical properties of Kapton for wavelengths investigated between 0.33 and 2.2 microns were not significantly altered by the presence of the coatings or changed by exposure of the coated Kapton to the low Earth orbital ram environment.
Banks, B. A.↗
Revision 1: Characterizing Basalt-Atmosphere Interactions on Venus: A Review of Thermodynamic and Experimental Results
The surface of Venus is in contact with a hot (~470° C), high pressure (92 bars), and caustic (CO 2 with S, but little H 2 O) atmosphere, which should cause progressive alteration of the crust in the form of sulfate and iron-oxide coatings; however, the exact rate of alteration and mineral species are not well constrained. Different experimental approaches, each with its own limitations, are currently being used to constrain mineralogy and alteration rate. One note is that no experimental approach has been able to fully replicate the necessary conditions and sustain them for a significant length of time. Further, geochemical modeling studies can also constrain surface alteration mineralogy, again with different assumptions and limitations. Here we review recent geochemical modeling and experimental studies to constrain the state of the art for alteration mineralogy, rate of alteration, open questions about the surface mineralogy of Venus, and what can be constrained before the fleet of missions arrive later this decade. Combining the new results confirm that basalt on the surface of Venus should react quickly and form coatings of sulfates and iron-oxides; however, the mineralogy and rate of alteration is dependent on physical properties of the protolith (including bulk composition, mineralogy, and crystallinity), as well as atmospheric composition, and surface temperature. Importantly, the geochemically modelling results show that the mineralogy is largely controlled by atmospheric oxygen fugacity, which is not well constrained for the near surface environment on Venus. Therefore, alteration experiments run over a range of oxygen and sulfur fugacities are needed across a wide range of Venus analog materials with varying mineralogy and crystallinity.
Justin Filiberto↗
Improved zinc oxide thermal control coatings
Ferricyanide/ferrocyanide couple prevents zinc oxide pigment degradation in thermal control coatings. Chemical couple retards physical optical property changes.
Freund, T.↗
Properties of plasma sprayed bond coats
Increasing bond coat oxidation resistance has been clearly linked to increasing durability of the ceramic layer of TBC's. However, recent studies have shown that significant differences in TBC life can be achieved for different bond coats that have little or no difference in oxidation behavior. These results suggest bond coat properties other than oxidation resistance can also influence TBC life. A determination of which properties affect TBC life and an understanding of how these properties affect TBC life could be valuable in designing new, more durable TBC's. Unfortunately, there is little existing information on the physical and mechanical properties of bond coat materials and there are fewer comparative studies that can be used to determine which properties are important to TBC life. This paper compares the properties of three bond coat compositions that have similar oxidation behavior but different TBC lives. Analysis of the properties indicates that the coefficient of thermal expansion and stress relaxation (creep) behavior of the three alloys are strongly correlated to the observed differences in TBC life.
Brindley, W. J.↗