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DOE OSTI2020

The ionic conductivity of Sm‐doped ceria

Abstract The oxygen ion conductivity of polycrystalline samples of Sm‐doped ceria and of Gd‐doped ceria is studied as a function of doping fraction and temperature using impedance spectroscopy allowing the separation of bulk and grain boundary conductivity. The introduction of a fine spacing for the Sm dopant fraction allows the clear identification of the dopant fraction leading to the largest bulk conductivity. At 267°C, the largest bulk conductivity is shown for Ce 0.93 Sm 0.07 O 1.965 . With increasing temperature, indications of an increase in the dopant fraction, which leads to the maximum in conductivity, are found. For the grain boundary conductivity, the maximum appears at larger dopant fractions compared to the bulk conductivity. The largest total conductivity for both dopants is again found for Sm‐doped ceria. In literature, different syntheses and sample preparation methods led to larger total conductivities for Gd‐doped ceria. In this work, we demonstrate that the variation of sintering conditions leads to scattering in the conductivity over one order of magnitude. Finally, we demonstrate that, in nominally pure cerium oxide, impurities dominate the ionic conductivity.

Koettgen, Julius↗

NASA NTRS1969

Miniaturization of magnetic logic circuitry

Magnetic logic circuit design features two ferrite materials, with different formulation and magnetic characteristics, which are bonded into a continuous structure by preparing the materials as a slurry and using the doctor blade method to form flexible ferrite sheets. After firing, the sintering process was continuous across the bond.

Baba, P. D.↗

NASA NTRS1990

Synthesis of Y1Ba2Cu3O(sub x) superconducting powders by intermediate phase reaction

One of the more striking problems for the synthesis of the Y1Ba2Cu3Ox compound is the high-temperature decomposition of the BaCO3. This compound is present as raw material or as an intermediate compound in chemical processes such as amorphous citrate, coprecipitation oxalate, sol-gel process, acetate pyrolisis, etc. This fact makes difficult the total formation reaction of the Y1Ba2Cu3Ox phase and leads to the presence of undesirable phases such as the BaCuO2 phase, the 'green phase', Y2BaCuO5 and others. Here, a new procedure to overcome this difficulty is studied. The barium cation is previously combined with yttrium and/or copper to form intermediate compounds which can react between them to give Y1Ba2Cu3Ox. BaY2O4 and BaCu2O3 react according to the equation BaY2O4+3BaCu2O3 yields 2Y1Ba2Cu3Ox. BaY2O4 is a stable compound of the Y2O3-BaO system; BaCu2O3 is an intimate mixture of BaCuO2 and uncombined CuO. The reaction kinetics of these phases have been established between 860 and 920 C. The phase evolution has been determined. The crystal structure of the Y1Ba2Cu3Ox obtained powder was studied. According to the results obtained from the kinetics study the Y1Ba2Cu3Ox the synthesis was performed at temperatures of 910 to 920 C for short treatment times (1 to 2 hours). Pure Y1Ba2Cu3Ox was prepared, which develops orthorombic type I structure despite of the cooling cycle. Superconducting transition took place at 91 K. The sintering behavior and the superconducting properties of sintered samples were studied. Density, microstructure and electrical conductivity were measured. Sintering densities higher than 95 percent D(sub th) were attained at temperatures below 940 C. Relatively fine grained microstructure was observed, and little or no-liquid phase was detected.

Moore, C.↗

NASA NTRS1990

Fabrication and chemical composition of RF magnetron sputtered Tl-Ca-Ba-Cu-O high Tc superconducting thin films

The preparation of TlCaBaCuO superconducting thin films on (100) SrTiO3 substrates is described, and the results of their characterization are presented. Sintering and annealing the thin films in a Tl-rich ambient yielded superconductivity with a Tc of 107 K. The results of an XPS study support two possible mechanisms for the creation of holes in the TlCaBaCuO compound: (1) partial substitution of Ca(2+) for Tl(3+), resulting in hole creation, and (2) charge transfer from Tl(3+) to the CuO layers, resulting in a Tl valence between +3 and +1.

Subramanyam, G.↗

DOE OSTI2023

A Study of a Surrogate Nuclear Thermal Propulsion Fuel Element

We report a surrogate fuel, Zirconium Carbide/Titanium Nitride has been prepared using a simple method to obtain a more uniform distribution of titanium nitride in the zirconium carbide matrix. Powders were sintered using Spark Plasma Sintering at 1750oC and 1850oC using a modified sintering profile. This resulted in a fairly uniform distribution of titanium nitride in the zirconium carbide matrix with a density of 95% of theoretical at 1850oC. Scanning electron microscopy, indentation hardness and x-ray diffraction results are given.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Thermophysical properties of high-density, sintered monoliths of yttrium dihydride in the range 373–773 K

Yttrium dihydride is a promising nuclear reactor moderator for high-temperature, thermal micro-reactors due to its ability to retain hydrogen to high temperatures while having a relatively low impact on neutron economy. However, it is difficult to fabricate yttrium dihydride in high-density, near net-shape monoliths for moderator applications due to challenges associated with the hydrogen absorption process. Here, high-density monoliths of yttrium dihydride were prepared by powder metallurgical methods. The lattice strain and thermal expansion coefficient were measured using neutron diffraction of powders of directly-hydrided yttrium, while the molar heat capacity and thermal diffusivity of sintered yttrium dihydride were measured using differential scanning calorimetry (DSC) and laser flash analysis (LFA), respectively. The molar heat capacity of yttrium dihydride was also calculated using density functional theory (DFT) for comparison. These parameters were used to then calculate the thermal conductivity and resistivity of yttrium dihydride as a function of temperature. The thermophysical properties of materials produced by both methods were observed to be consistent with the values from literature for yttrium dihydride. Due to the novelty of producing yttrium dihydride by powder metallurgical methods, this result indicated that the sintered monoliths were of high quality and that powder metallurgy is a viable method for large-scale production of yttrium dihydride monoliths for nuclear reactor moderator applications.

36 MATERIALS SCIENCE↗

NASA NTRS2003

Development of Ceramic Systems for High temperature Coatings

Professor Eslamloo-Grami will synthesize ceramic powders of various compositions based on pyrochlore, perovskite, and magnetoplumbite structures by doping with various oxides. Sol-gel and combustion synthesis routes will be used for powder syntheses. The powders will be characterized for particle size, surface area, microstructure, sintering etc. Thermal conductivity of the hot pressed specimens will also be measured at various temperatures. At the end, a project report will be prepared describing in details the experimental methods, results, discussion, and future research.

Eslamloo-Grami, Maryame↗

NASA NTRS2003

Sintering and Interface Strain Tolerance of Plasma-Sprayed Thermal and Environmental Barrier Coatings

Ceramic thermal and environmental barrier coatings will be more aggressively designed to protect gas turbine engine hot section SiC/SiC Ceramic Matrix Composite (CMC) components in order to meet future engine higher fuel efficiency and lower emission goals. A coating system consisting of a zirconia-based oxide topcoat (thermal barrier) and a mullite/BSAS silicate inner coat (environmental barrier) is often considered a model system for the CMC applications. However, the coating sintering, and thermal expansion mismatch between the zirconia oxide layer and the silicate environmental barrier/CMC substrate will be of major concern at high temperature and under thermal cycling conditions. In this study, the sintering behavior of plasma-sprayed freestanding zirconia-yttria-based thermal barrier coatings and mullite (and/or barium-strontium-aluminosilicate, i.e., BSAS) environmental barrier coatings was determined using a dilatometer in the temperature range of 1200-1500 C. The effects of test temperature on the coating sintering kinetics were systematically investigated. The plasma-sprayed zirconia-8wt.%yttria and mullite (BSAS) two-layer composite coating systems were also prepared to quantitatively evaluate the interface strain tolerance of the coating system under thermal cycling conditions based on the dilatomentry. The cyclic response of the coating strain tolerance behavior and interface degradation as a function of cycle number will also be discussed.

Zhu, Dongming↗

NASA NTRS2009

Detecting Airborne Mercury by Use of Palladium Chloride

Palladium chloride films have been found to be useful as alternatives to the gold films heretofore used to detect airborne elemental mercury at concentrations of the order of parts per billion (ppb). Somewhat more specifically, when suitably prepared palladium chloride films are exposed to parts-per-billion or larger concentrations of airborne mercury, their electrical resistances change by amounts large enough to be easily measurable. Because airborne mercury adversely affects health, it is desirable to be able to detect it with high sensitivity, especially in enclosed environments in which there is a risk of leakage of mercury from lamps or other equipment. The detection of mercury by use of gold films involves the formation of gold/mercury amalgam. Gold films offer adequate sensitivity for detection of airborne mercury and could easily be integrated into an electronic-nose system designed to operate in the temperature range of 23 to 28 C. Unfortunately, in order to regenerate a gold-film mercury sensor, one must heat it to a temperature of 200 C for several minutes in clean flowing air. In preparation for an experiment to demonstrate the present sensor concept, palladium chloride was deposited from an aqueous solution onto sets of gold electrodes and sintered in air to form a film. Then while using the gold electrodes to measure the electrical resistance of the films, the films were exposed, at a temperature of 25 C, to humidified air containing mercury at various concentrations from 0 to 35 ppb (see figure). The results of this and other experiments have been interpreted as signifying that sensors of this type can detect mercury in room-temperature air at concentrations of at least 2.5 ppb and can readily be regenerated at temperatures <40 C.

Ryan, Margaret↗

DOE OSTI2025

Unravelling Adsorbate-Metal-Oxide Interactions: Water Vapor Chemistry on the Growth and Sintering of Ni over Reducible CeO2(111) Thin Films

The role of water in the growth and sintering of Ni particles over well-ordered CeOx(111) (1.5 < x < 2) thin films was investigated through scanning tunneling microscopy (STM) and X-ray photoelectron spectroscopy (XPS) studies, considering ceria-supported Ni attracts great attention as a promising catalyst for reactions such as steam reforming of ethanol and water gas shift reaction, in which water vapor is used as a key reactant. In the study, both fully oxidized CeO2 and partially reduced CeO1.75 thin films were prepared to examine the effect of the oxygen vacancies/Ce3+ sites in ceria supports. Our STM results revealed that dosing water before or after Ni deposition over the CeOx(111) surfaces at room temperature influenced the sintering behavior of Ni nanoparticles with further heating. Exposure of water to Ni nanoparticles that were deposited over both CeO2 and CeO1.75 at 300 K causes the formation of flatter particles with significantly reduced height when heating to the same temperatures compared to Ni/ceria with no water adsorbates. The flatter Ni particles were also observed when water was first dosed over CeO2 at 300 K followed by Ni deposition at room temperature and further heating. Over a partially reduced CeO1.75 surface with predosed water at 300 K, there is an extensive decrease in the particle density upon subsequent Ni deposition at room temperature and a significant increase in the height for Ni nanoparticles with further heating to higher temperatures compared to Ni over a pristine CeO1.75 surface. This is due to the filling of oxygen vacancies caused by the dissociation of water. This creates fewer nucleation sites for Ni on ceria, weakening the metal-oxide interaction and causing significant metal sintering. Our experimental findings suggest distinct adsorbate-metal-oxide interactions are key to the tuning of sintering of Ni nanoparticles over the CeOx(111) surface caused by water exposure. Such interactions are essential for the further modification of Ni-based catalysts for improved reactivity and stability.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1980

A Conceptual Design Study of a High Temperature Solar Thermal Receiver

A conceptual design was made for a solar thermal receiver capable of operation in the 1095 to 1650 C (2000 to 3000 F) temperature range. This receiver is designed for use with a two-axis paraboloidal concentrator in the 25 to 150 kW sub t power range, and is intended for industrial process heat, Brayton engines, or chemical/fuels reactions. Three concepts were analyzed parametrically. One was selected for conceptual design. Its key feature is a helical coiled tube of sintered silicon nitride which serves as the heat exchanger between the incident solar radiation and the working fluid. A mechanical design of this concept was prepared, and both thermal and stress analysis performed. The analysis showed good performance, low potential cost in mass production, and adaptability to both Brayton cycle engines and chemical/fuels production.

Robertson, C. S.↗

NASA NTRS1996

A Two Phase HfB2-SiB4 Material

A two phase HfB2-SiB4 material which is useful as a high temperature oxidation resistant coating. This invention relates to ceramic coatings and more particularly to ceramic coatings containing metal borides. Boride materials are known to have good oxidation resistance, with HfB2 considered to be the best pure boride for oxidation applications. It has been shown that the addition of 10 to 20 percent SiC to HfB2 increases the oxidation resistance. The HfB2-SiC materials are prepared by hot pressing powder mixtures. Hot pressing powder mixtures has limited ability to produce fine grained multiphase materials due to particle coarsening during the sintering process. Additionally, the purity of the final monolithic structure is limited to the purity of the starting powders. Chemical vapor deposition (CVD) offers a method of producing highly pure multiphase ceramics, with better control of microstructure. Researchers have tried to produce HfB2-SiC coatings by CVD but without success.

SILICON COMPOUNDS↗

NASA NTRSDate not supplied

Lunar Regolith: Small Scale Robotic Site Preparation and Geotechnical Experiments with Scoops

- NASA’s Moon-To-Mars Planetary Autonomous Construction Technology (MMPACT) project seeks to research, develop, and demonstrate lunar surface construction capabilities. - Quantification of lunar regolith’s geotechnical properties allows for effective prediction of forces and displacement during excavation and construction and is critical to facilitating regolith sintering capabilities all of which benefit lunar infrastructure plans. - Knowledge of shear strength, Mohr-Coulomb cohesion, angle of internal friction, bearing strength, bulk density, etc. is needed. - The use of ground-based testing of various lunar simulants with relevant hardware (e.g., robotic arm tools) enables validation of technology choices, tool paths, and lunar surface construction activities. - In addition, the use of Taguchi methods [1] will minimize the number of needed experiments to explore critical input parameters. - The Jet Propulsion Lab is preparing to fly the COLDarm payload on a CLPS lunar mission with a geotechnical measurement scoop

Regolith↗

NASA NTRS2004

Ceramic Interconnects with Low Sintering Temperature

Ceramic interconnects for use in solid oxide he1 cells are expected to operate between 900 to approximately 1000 C, sinter below 1400 C to allow co-firing and meet a number thermal mechanical requirements. The pervoskite type (ABO3) lanthanum chromite based materials have emerged as a leading candidate that will meet these criteria by varying the composition on the A and B sites. A need therefore exists to determine this material's temperature dependent electrical and mechanical properties with respect to these site substitutions. In this investigation oxide powders were prepared by the glycine-nitrate process. Ionic substitutions were carried out on A sites with Ca or Sr, and B sites with Co and Al, respectively. Only stoichiometric compositions were considered for the sake of stability. The powders and their ability to sinter were investigated by XRD, SEM, dilatometry and density measurements. The sintered materials were further examined by SEM, thermal expansion and electric conductivity measurements in order to elucidate the resulting microstructure, electrical and mechanical properties. In addition quantum mechanical calculations were performed to obtain insight into the effects of these dopants on the materials electronic band structure and lattice parameter.

Zhong, Zhi-Min↗

NASA NTRS1991

Production of superconductor/carbon bicomponent fibers

Certain materials are unable to be drawn or spun into fiber form due to their improper melting characteristics or brittleness. However, fibrous samples of such materials are often necessary for the fabrication of intricate shapes and composites. In response to this problem, a unique process, referred to as the piggyback process, was developed to prepare fibrous samples of a variety of nonspinnable ceramics. In this technique, specially produced C shaped carbon fibers serve as micromolds to hold the desired materials prior to sintering. Depending on the sintering atmosphere used, bicomponent or single component fibers result. While much has been shown worldwide concerning the YBa2Cu3O(7-x) superconductor, fabrication into unique forms has proven quite difficult. However, a variety of intricate shapes are necessary for rapid commercialization of the superconducting materials. The potential for producing fibrous samples of the YBa2Cu3O(7-x) compound by the piggyback process is being studied. Various organic and acrylic materials were studied to determine suspending ability, reactivity with the YBa2Cu3O(7-x) compound during long term storage, and burn out characteristics. While many questions were answered with respect to the interfacial reactions between YBa2Cu3O(7-x) and carbon, much work is still necessary to improve the quality of the sintered material if the fibers produced are to be incorporated into useful composite or cables.

Wise, S. A.↗

NASA NTRS1979

Array Automated Assembly Task for the Low Cost Solar Array Project, Phase 2

Using silk screened evaporated and sputtered Al as the metal source, the formation of Al back surface fields was studied. The most satisfactory results were those obtained with the sputtered A1 and in which open circuit voltages (V sub oc) of 0.585 v (12 ohm cm FZ silicon) were achieved. The ultrasonic interconnect process is discussed. The process is shown to be satisfactory, but increased pull-strength may be obtained if some form of sintering is carried out on the metallized contacts. Plasma etching is shown to be feasible as a replacement for wet chemical cleaning prior to diffusion. Initial results on cells prepared by using electroless Pd/Ni plus either electroplated Ag or Cu show slightly poor performance than cells with the baseline evaporated Ti/Pd/Ag system. A mask designed for the 1.6 x 7.0 cm and 2.0 x 7.0 cm cells is described. This mask has a lower area coverage and total lower resistive loss than the previous mask design. It is also shown that the cell width should not exceed 2.0 - 3.0 cm for optimum efficiency.

Campbell, R. B.↗

NASA NTRS1990

Production of superconductor/carbon bicomponent fibers

Certain materials are unable to be drawn or spun into fiber form due to their improper melting characteristics or brittleness. However, fibrous samples of such materials are often necessary for the fabrication of intricate shapes and composites. In response to this problem, a unique process, referred to as the piggyback process, was developed to prepare fibrous samples of a variety of nonspinnable ceramics. In this technique, specially produced C-shaped carbon fibers serve as micromolds to hold the desired materials prior to sintering. Depending on the sintering atmosphere used, bicomponent or single component fibers result. While much has been demonstrated worldwide concerning the YBa2Cu3O(7-x) superconductor, fabrication into unique forms has proven quite difficult. However, a variety of intricate shapes are necessary for rapid commercialization of the superconducting materials. The potential for producing fibrous samples of the YBa2Cu3O(7-x) compound by the piggyback process is being investigated. Various organic and acrylic materials were investigated to determine suspending ability, reactivity with the YBa2Cu3O(7-x) compound during long term storage, and burn out characteristics. While many questions were answered with respect to the interfacial reactions between YBa2Cu3O(7-x) and carbon, much work is still necessary to improve the quality of the sintered material if the fibers produced are to be incorporated into useful composites or cables. Additional research is necessary to evaluate quality of the barrier layer during long soakings at the peak temperature; adjust the firing schedule to avoid microcracking and improve densification; and increase the solids loading in the superconductive suspension to decrease porosity.

Wise, S. A.↗

NASA NTRS1994

Preparation and Dielectric Measurements of the Rare Earth Green Phases R2BaCuO(5-x) (R = Y, Sm, Gd, Dy, Ho, Er, Yb)

It has been demonstrated that R2BaCuO(5-x) (R = Y, Sm, Gd, Dy, Ho, Er, Yb) does not undergo significant densification unless the sintering temperatures are near the incongruent melting point or the sintering times are long. Good quality powders of Y2BaCuO(5-x) have been synthesized by using oxide raw materials or precursors such as acetates and nitrates. The acetates- and the nitrates-derived yttrium green phase resulted in finer particle sizes, acceptable dielectric properties and lower melting temperatures than those processed via oxide raw materials. The hot pressing technique has been employed to produce a dense R2BaCuO(5-x) (R=Y,Gd) substrate with satisfactory dielectric properties. Reactivity to reducing conditions, i.e. graphite die, limited the optimization of the properties. A high sensitivity to the annealing atmosphere has been demonstrated in Y2BaCuO,.,,. Oxygen treatment at 950 OC has been shown to improve the dielectric properties while treatment in nitrogen, at the same temperature, degraded desirable properties. A high sensitivity to the annealing atmosphere has been demonstrated in Y2BaCuO(5-x). Oxygen treatment at 950 C has been shown to improve the dielectric properties while treatment in nitrogen, at the same temperature, degraded desirable properties. The dielectric constants of the rare earth green phases R2BaCuO(5-x) were found to be low. Relaxation peaks were detected at low temperatures (T less than 150 K) and at high temperatures (150 less than T greater than 420 K). The dielectric losses and conductivities at 77 K were measured to be in the range of 10(exp -4) and 10(exp -12) (Omega-cm)(exp -1), respectively. Many parameters were found to exhibit dependencies on the rare earth cation sizes.

Gonzalez-Titman, Carlos↗