DETERIORATION OF CALCIA-STABILIZED ZIRCONIA
Deterioration of calcia-stabilized zirconia, refractory materials
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Deterioration of calcia-stabilized zirconia, refractory materials
Apparatus for melting boron carbide inductively on water-cooled hearth, noting application to other refractory materials
Influence of stress on corrosion behavior and mass transfer effect on refractory materials for advanced space power systems
High temperature behavior and properties of refractory materials such as molybdenum, tungsten, silicides, aluminides and carbides
Emittance measurement for refractory materials to 5000 deg f - temperature & structure dependence
Advances in neutron flux, neutron instrumentation, and sample environments over the past years allowed the development of unique techniques to characterize material synthesis and processing. The available infrastructure at LANL allows to apply these techniques to radioactive materials or materials containing actinides. Here, we present capabilities and results to characterize materials in situ at temperatures above 2000 Celsius degrees such as in loss-of-coolant accidents. Temperatures in excess of 2000 C. degrees are not readily achieved and neutrons are one of a few probes to characterize materials under these conditions. Research in refractory materials, phase diagram studies or accident scenarios for nuclear materials are research areas where such extreme conditions are required. As an example, we present the formation of UC{sub x} from UO{sub 2+x} and graphite in situ using high temperature neutron diffraction with particular focus on resolving the conflicting reports on the crystal structure of non-quenchable cubic UC{sub 2}. The ability to follow the reaction UO{sub 2}+C → UC{sub x}+CO{sub y} in situ with neutron diffraction allows us to conclude that the reaction occurs within minutes over a temperature range of 60 Celsius degrees. The initiation of the reaction is far below the reaction temperature of 2000 C. degrees reported for this reaction in standard text books on actinide chemistry. This may be due to the unusually small ∼100 nm grain size of our UO{sub 2} initial powder. Furthermore, the holding time of several hours reported in the literature would be unnecessary. The neutron diffraction data collected for the cubic high temperature UC{sub 2} phase unambiguously confirmed the disordered C-C dumbbells and excluded structures previously determined by X-ray diffraction.
Millimeter continuum and spectral line observations with 10 sec, 30 sec, and 60 sec resolution are used to characterize the structure and chemistry of the gas around the young, embedded star, IRAS 05338-0624. On arcminute scales, emission from dense gas tracers outline an isolated condensation centered on the IRAS source position. The condensation is characterized by a size of approximately 60 sec, a density of 2 x 10(exp 5)/cc, and a virial mass of 40 solar mass. Interferometric CS J = 2-1 observations show two peaks, one toward the continuum peak and the other toward a position 14 sec west and 8 sec south. Single-dish maps of SO, CH3OH, and SiO show pronounced wing emission to the west of the IRAS source, which interferometer observations reveal to be a compact region of outflow activity. CS emission at redshifted and blueshifted velocities reveals a bipolar outflow oriented with a position angle of 45 deg, while SiO emission appears to be tracing a fast shock interaction region at the CS red-lobe peak, 14 sec west and 8 sec south of the IRAS source. Finally, H(13)CO(+) emission traces clumps of quiescent gas toward the IRAS source and adjacent to the blue lobe of the outflow. Column densities and molecular fractional abundances are derived to explore the interaction between the surrounding condensation and the young stellar object. We find evidence for gas phase depletions within the overall condensation in several gas tracers (CO, CS, HCN, SO) but not in the region immediately around the young stellar object. Enhanced abundances of SO, CH3OH, and SiO (by factors of 4, greater than 100, greater than 1000, respectively) are observed in the shocked gas; these enhancements may be explained in terms of a nondissociative shock liberating mantle materials that contain some amount of refractory materials, a moderate velocity dissociative shock in which only minor sputtering of Si occurs, or a shock that impacts surrounding material with a range of speeds.
Dust is formed in stellar environments, and destroyed by sputtering, shattering and vaporization in shock waves due to cloud-cloud collisions and supernova blast waves. Dust is also destroyed during star formation. We review the dust formation and destruction balance. The calculated destruction time-scale is less than or equal to one billion years and the star dust injection time-scale is approx. 2.5 billion years. Hence, the fractions of elemental carbon and silicon locked up in stardust are less than 0.3 and less than 0.15, respectively. An efficient ISM dust formation route is therefore implied. In particular, in dense clouds dust grows; through the processes of coagulation and the accretion of gas phase molecules e.g. H20, CO, CH4. These icy materials may then be photoprocessed to refractory materials in more diffuse regions. The resulting carbonaceous grain mantle may actually be the glue that holds the coagulated grains together.
Refractory material irradiation, sensor studies, and sheath applications for development of ultrasonic temperature measuring device
Vugraphs are presented to show the use of refractory materials for the skin of the High speed Civil Transport (HSCT). Examples are given of skin temperature ranges, failure mode weight distribution, tensile properties as a function of temperature, and components to be constructed from composite materials. The responsibilities of various aircraft companies for specific aircraft components are defined.
Northstar Medical Radioisotopes is developing an accelerator-based method to produce 99 Mo, which is a parent isotope of the commonly used 99m Tc medical isotope. The Mo targets being designed for the accelerator will be produced from enriched 100 Mo, also known as aMo . Pressed and sintered powder feedstock is used to fabricate aMo targets, producing 29 mm disk-shaped targets. The targets are subjected to 1–6 days in line of an electron beam with subsequent dissolution of the disk to retain the 99 Mo, which decays to 99m Tc at radio-pharmacies. The press and sinter method is advantageous because the inherent porosity produced by this method enables increased surface area and therefore increased flow of dissolution media, decreasing the dissolution time and reducing the need for a highly acidic media. Although porosity aids in dissolution, it reduces the mechanical strength and ductility. Targets require good mechanical integrity when subjected to the conditions in the accelerator. Therefore, Northstar is seeking methods to rapidly test disk samples after fabrication to assure mechanical performance metrics are achieved. This report details the design and testing of a small punch test (SPT) that accommodates the 29 mm disk. Initial data were used to relate the SPT data to tensile properties, such as the yield strength (YS), ultimate tensile strength (UTS), and total elongation to failure. Although the SPT has been established as a somewhat reliable method for testing metallic materials, few studies have applied the SPT to refractory materials such as Mo. Based on tensile testing performed at Oak Ridge National Laboratory on different Mo samples, correlation between the Mo tensile and SPT properties could be performed, establishing a standard calibration that could be applied to other Mo samples. To test the efficacy of the SPT with Mo, multiple different disk batches were fabricated under different conditions (e.g., pressure, lubricant) with commercially available pure Mo powder. Generally, only a UTS could be well defined because the press and sinter disks failed under brittle fracture, making it difficult to determine the YS and elongation. Compared with disks fabricated with aMo powder, the aMo samples underperformed their pure nat Mo counterparts. This report summarizes the current status of the SPT, but further evaluation is needed before it can be applied as a reliable quality assurance tool.
A noncontact measurement technique for the density and the thermal expansion refractory materials in their molten as well as solid phases is presented. This technique is based on the video image processing of a levitated sample. Experiments were performed using the high-temperature electrostatic levitator (HTESL) at the Jet Propulsion Laboratory in which 2-3 mm diameter samples can be levitated, melted, and radiatively cooled in a vacuum. Due to the axisymmetric nature of the molten samples when levitated in the HTESL, a rather simple digital image analysis can be employed to accurately measure the volumetric change as a function of temperature. Density and the thermal expansion coefficient measurements were made on a pure nickel sample to test the accuracy of the technique in the temperature range of 1045-1565 C. The result for the liquid phase density can be expressed by p = 8.848 + (6.730 x 10(exp -4)) x T (degC) g/cu cm within 0.8% accuracy, and the corresponding thermal expansion coefficient can be expressed by Beta=(9.419 x 10(exp -5)) - (7.165 x 10(exp -9) x T (degC)/K within 0.2% accuracy.
High temperature refractory metals are required for a number of high temperature propulsion applications. Refractory metals are expensive, difficult to manufacture with high buy-to-fly ratios, and few vendors. Additive manufacture (AM) is used to produce C103, Molybdenum (Mo), and Tungsten (W) reaction chamber and thrust stand-off as well as Iridium ultra-fine lattice catalysts for integration into 1 N green propulsion thrusters. Refractory AM is in development and like traditional AM alloys requires substantial post-processing to include powder heat treatment, surface finish enhancement, inspection, and machining before placed in service. The combination of limited feedstock sources, high temperature processing, oxygen sensitivity, fracture prone nature, and need for elevated temperature mechanical testing limit the number of qualified facilities capable of post-processing AM refractory materials, which add to cost and schedule constraints. However, properly implemented refractory metal AM can overcome existing manufacture limitations by greatly increasing design flexibility, new material options, reduced price, decreased lead-time, and leverage the ever growing AM commercial supply base.
High temperature refractory metals are required for a number of high temperature propulsion applications. Refractory metals are expensive, difficult to manufacture with high buy-to-fly ratios, and few vendors. Additive manufacture (AM) is used to produce C103, Molybdenum (Mo), and Tungsten (W) reaction chamber and thrust stand-off as well as Iridium ultra-fine lattice catalysts for integration into 1 N green propulsion thrusters. Refractory AM is in development and like traditional AM alloys requires substantial post-processing to include powder heat treatment, surface finish enhancement, inspection, and machining before placed in service. The combination of limited feedstock sources, high temperature processing, oxygen sensitivity, fracture prone nature, and need for elevated temperature mechanical testing limit the number of qualified facilities capable of post-processing AM refractory materials, which add to cost and schedule constraints. However, properly implemented refractory metal AM can overcome existing manufacture limitations by greatly increasing design flexibility, new material options, reduced price, decreased lead-time, and leverage the ever growing AM commercial supply base.
Refractory metals and alloys are of major interest for nuclear fusion systems, space nuclear power and propulsion, and hypersonic applications due to their desirable properties at elevated temperatures (>1500°C). Limitations of refractory materials include their low ductility, poor oxidation resistance, and high manufacture cost using traditional techniques. Additive manufacturing (AM) can reduce material waste associated with manufacture, but AM fabrication is impacted by the brittleness of these refractory metals, resulting in excessive cracking during printing. Cracking reduces the effectiveness of hot isostatic pressing (HIP) which is commonly used to improve density and mechanical properties of AM components. The goal of this work is to improve refractory metal printability without majorly affecting the material properties which are the main reason these materials are used. Ceramic nanoparticles have been shown to help improve material properties after heat treatment. Results will be shown that demonstrate the effectiveness of adding nanoparticles to refractory metals. Additionally, there will be discussion regarding how these nanoparticles change the effect of heat treatments such as HIP compared with the AM pure metal samples.
A chloride-based molten-salt system that uses a ternary blend of MgCl2/KCl/NaCl is investigated to provide higher temperature thermal energy storage capability. Despite higher thermal stability, molten chlorides present several unique challenges, including the design of internal refractory-ceramic liners to prevent the corrosion and thermal stress of alloy tank shells. This work discusses issues and potential solutions related to containment of molten chloride salt, specifically the optimization of the refractory material at the molten salt interface (hot face). The down-selected hot face candidate limits permeation of salt through the material and forms a highly stable secondary surface phase in equilibrium with the molten salt. A mortar is created using the corrosion resistant hot face brick. Brick and mortar composite are subjected to mechanical stress/strain analysis, in order to calculate composite material properties and better inform thermomechanical models. The U.S. Department of Energy Generation 3 (DOE Gen3) program seeks to develop higher efficiency CSP plants that can provide cost-competitive, flexible power in the U.S. electric grid. The proposed Gen3 Liquid Pathway CSP plant closely resembles the configuration of current nitrate salt power towers with two-tank storage (Gen2). The differences between Gen2 and Gen3 include the types of compatible materials used in salt storage tank construction. Stainless steel loses strength at Gen3 temperatures, and although nickel superalloys would be capable of withstanding sustained high temperatures, these materials are prohibitively expensive at scale. Uninsulated tank shells also pose a significant risk as common steels are highly susceptible to chemical attack from molten chloride salt. To address these concerns, refractory-ceramic based containment materials are proposed to line the inside of the hot and cold storage tanks. In doing so, stainless or carbon steel shells may be used in construction depending on the level of insulation provided. The composition of the internal liner requires careful consideration to maximize the efficacy of multiple parameters including corrosion resistance, strength at operating temperature, durability, and cost. This is particularly true for the material at the interface with the salt, known as the "hot face", which is responsible for protecting the insulating layers between the tank shell and the hot face brick layer. The molten salt in this system is superheated over 300 °C above its freeze temperature. Therefore, unlike other industrial processes which use refractory-lined vessels, it is not expected that a freeze plane will develop in the hot face. Therefore, the hot face must be designed to withstand chemical corrosion and inhibit permeation of molten salt into the insulating layers. A down selection was performed to identify a hot face candidate best equipped to maintain thermal, mechanical, and chemical integrity when exposed to molten salt over extended periods of time. Long-duration chemical capability experiments were conducted with the down selected hot face refractory fully immersed in molten chloride salt for up to 3000 hours. The average salt penetration does not exceed 100 microns. When extrapolated to 20 and 30 years of continuous exposure, the expected salt penetration depth is approximately 2.0 mm and 2.9 mm, respectively. A magnesium-rich secondary phases develops at the salt/refractory interface. X-ray diffraction identifies the material as forsterite (Mg2SiO4), which is reported to form synthetically in molten chloride salt solutions. These results suggest the selected hot face will adequately inhibit salt permeation. While there is optimism that the hot face brick will inhibit salt permeation, mortar joints are typically the weakest point of a refractory brick liner. From a thermochemical perspective, differing thermal expansion coefficients may result in the mortar and brick to grow independent of each other, creating gaps through which molten salt can penetrate. To address this issue, NREL has developed an in-house mortar composed of the down selected hot face brick that has been shown to be compatible with the salt. Compressive stress/strain analyses have been performed on the brick/ mortar composites to generate stress/strain curves. Modulus of elasticity and Poisson's ratio of the composite may be calculated from the stress/strain curves, in order to provide more representative data to finite element mechanical models for accurate approximation of stress on the tank shell and the amount of thermal expansion expected within the tank liner.
In the processing of propellants, volatiles, and metals subject area, the following topics are discussed: reduction of lunar regolith; reduction of carbon dioxide; and reduction of carbonaceous materials. Other areas addressed include: (1) production of structural and refractory materials; (2) resource discovery and characterization; (3) system automation and optimization; and (4) database development. The majority of these topics are discussed with respect to the development of lunar and mars bases. Some main topics of interest include: asteroid resources, lunar resources, mars resources, materials processing, construction materials, propellant production, oxygen production, and space-based oxygen production plants.