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None. From Objectives section: Evaluate the stability of potassium beta alumina under potassium AMTEC operating conditions. Evaluate the stability regime in which potassium beta alumina can be fabricated.
Experiments were done with a molten-salt catholyte (initially CuCl2 in AlCl3-NaCl) separated from molten Na by beta alumina. The open-circuit reduction potentials were 4.3 and 3 volts for Cu++ and Cu+, respectively. High polarization and nonrechargeability characterized the cell's operation. The cell's ohmic resistance during discharge was higher than what would be expected from only the ionic resistance of the beta-alumina.
The effective fiber strength of alumina fibers in an aluminum composite was increased to 173,000 psi. A high temperature heat treatment, combined with a glassy carbon surface coating, was used to prevent degradation and improve fiber tensile strength. Attempts to achieve chemical strengthening of the alumina fiber by chromium oxide and boron oxide coatings proved unsuccessful. A major problem encountered on the program was the low and inconsistent strength of the Dupont Fiber FP used for the investigation.
Research was conducted on reinforcing nickel based matrices with alumina trichites by using powder metallurgy. Alumina trichites previously coated with nickel are magnetically aligned. The felt obtained is then sintered under a light pressure at a temperature just below the melting point of nickel. The halogenated atmosphere technique makes it possible to incorporate a large number of additive elements such as chromium, titanium, zirconium, tantalum, niobium, aluminum, etc. It does not appear that going from laboratory scale to a semi-industrial scale in production would create any major problems.
The viscosity of a magma is an important parameter in connection with its effect on geologic processes such as melt segregation, magma vesiculation, and crystal fractionation. Though most models of geologic processes assume relatively low values for the magma viscosity less than 10,000 poise, it would be useful to have an empirical model for estimating viscosities when the process occurs during continuous cooling to a temperature region where the viscosity is expected to be very high. The considered work has been carried out to provide the experimental measurements of viscosity at low temperatures which would be used in formulating the empirical model. Ten iron-containing silicate compositions have been investigated by Klein et al. (1981), and four of these compositions have been selected for the present study with alumina. The study involves substitutions of Al2O3 for FeOx at Na2O/Al2O3 moles greater than one. For the four iron-containing silicate glasses with alumina, the viscosity at a given temperature is found to increase with increasing (Fe + Al).
The atom superposition and electron delocalization molecular orbital theory and large cluster models have been employed to study cation vacancy diffusion in alpha-Al2O3 and the bonding of alpha-Al2O3 to nickel, aluminum, and yttrium surfaces. Al(3+) diffusion barriers in alpha-Al2O3 by the vacancy mechanism are in reasonable agreement with experiment. The barrier to Y(3+) diffusion is predicted to be much higher. Since addition of yttrium to transition metal alloys is known to reduce the growth rate and stress convolutions in protective alumina scales, this result suggests the rate-limiting step in scale growth is cation vacancy diffusion. This may partially explain the beneficial effect of yttrium dopants on scale adhesion. The theory also predicts a very strong bonding between alumina and yttrium at the surface of the alloy. This may also be important to the adhesion phenomenon. It is also found that aluminum and yttrium atoms bond very strongly to nickel because of charge transfer from their higher lying valence orbitals to the lower lying nickel s-d band.
Measurements were made of the kinetics of thermal grooving at the intersection of rhombohedral twin boundaries with the (1 0 -1 0) plane in alumina, at temperatures from 1773 to 2273 K. An analysis of the values obtained on the basis of the model of Mullins (1957) indicated that surface diffusion was the dominant mass transport mechanism. Comparisons are made with the results of other investigations of alumina, and an equation is derived for the surface diffusion value.
Continuous length polycrystalline alumina fibers are candidates as reinforcement in high temperature composite materials. Interest therefore exists in characterizing the thermomechanical behavior of these materials, obtaining possible insights into underlying mechanisms, and understanding fiber performance under long term use. Results are reported on the time-temperature dependent strength behavior of Nextel 610 and Fiber FP alumina fibers with grain sizes of 100 and 300 nm, respectively. Below 1000 C and 100 hours, Nextel 610 with the smaller grain size had a greater fast fracture and rupture strength than Fiber FP. The time exponents for stress-rupture of these fibers were found to decrease from approximately 13 at 900 C to below 3 near 1050 C, suggesting a transition from slow crack growth to creep rupture as the controlling fracture mechanism. For both fiber types, an effective activation energy of 690 kJ/mol was measured for rupture. This allowed stress-rupture predictions to be made for extended times at use temperatures below 1000 C.
To understand magmatism at convergent margins, one must know the origin of their characteristic plagioclase-rich high-alumina basalts (HABs). Wet melting experiments on basalts at 3 kilobars yielded high-alumina liquids and a coexisting mineral assemblage with plagioclase crystallization in these melts, while mafic minerals underwent limited crystallization or even resorption. These results suggest that hydrous HAB liquids, presumably formed by fractionation of a hydrous basalt at depth, precipitate voluminous plagioclase as pressure drops during ascent and eruption. Plagioclase accumulation is not necessarily required to explain the petrogenesis of plagioclase-rich HAB.
Report discusses cleaning of ceramic (principally, alumina) substrates in preparation for sputter deposition of titanium intermediate films on substrates followed by sputter deposition of outer silver films. Principal intended application, substrates sliding parts in advanced high-temperature heat engines, and outer silver films serve as solid lubricants: lubricating properties described in "Solid Lubricant for Alumina" (LEW-15495).
Continuous-length polycrystalline aluminum-oxide-based fibers are being considered as reinforcements for advanced high-temperature composite materials. For these fine-grained fibers, basic issues arise concerning grain growth and microstructural instability during composite fabrication and the resulting effects on the fiber's thermo-mechanical properties. To examine these issues, commercially available Nextel 610 (alumina) and Altex (alumina-silica) fibers were annealed at 1100 and 1300 C for up to 100 hr in air. Changes in fiber microstructure, fiber tensile creep, stress rupture, and bend stress relaxation (BSR) that occurred with annealing were then determined. BSR tests were also used to compare as-received and annealed fibers to other polycrystalline oxide fibers. Annealing was shown to have a significant effect, particularly on the Altex fiber, and caused it to have increased creep resistance.
The single crystal superalloy Rene'N5 (with or without Y-doping and hydrogen annealing) was cyclically oxidized at 1150 C for 1000 hours. After considerable scale growth (>= 500 hours), even the adherent alumina scales formed on Y-doped samples exhibited delayed interfacial spallation during subsequent water immersion tests, performed up to one year after oxidation. Spallation was characterized by weight loss, the amount of spalled area, and acoustic emission response. Hydrogen annealing (prior to oxidation) reduced spallation both before and after immersion, but without measurably reducing the bulk sulfur content of the Y-doped alloys. The duration and frequency of sequential, co-located acoustic emission events implied an interfacial crack growth rate at least 10(exp -3) m/s, but possibly higher than 10(exp 2) m/s. This is much greater than classic moisture-assisted slow crack growth rates in bulk alumina (10(exp -6) to 10(exp -3) m/s), which may still have occurred undetected by acoustic emission. An alternative failure sequence is proposed: an incubation process for preferential moisture ingress leads to a local decrease in interfacial toughness, thus allowing fast fracture driven by stored strain energy.
Sintered aluminum oxide materials were formed using commercial methods from mechanically mixed powders of nano-and micrometer alumina. The powders were consolidated at 1500 and 1600 C with 3.2 and 7.2 ksi applied stress in argon. The conventional micrometer sized powders failed to consolidate. While 100 percent nanometer-sized alumina and its mixture with the micrometer powders achieved less than 99 percent density. Preliminary high temperature creep behavior indicates no super-plastic strains. However high strains (less than 0.65 percent) were generated in the nanometer powder, due to cracks and linked voids initiated by cavitation.
The development of advanced engines for aerospace applications depends on the availability of strong, tough materials that can withstand increasingly higher temperatures under oxidizing conditions. The need for such materials led to the study of an oxide-based composite composed of an alumina matrix reinforced with zirconia-coated sapphire fibers. Because the nonbrittle behavior of this system depends on the interface and its ability to prevent fiber-to-matrix bonding and reduce interfacial shear stress, the microstructure of the zirconia must be carefully controlled during both coating application and composite processing. When it was both porous and unstabilized, zirconia (which does not react easily with alumina) was found to be the most effective material tested in reducing interfacial shear strength between the fiber and matrix.
Solar-dynamic space power systems require durable, high-emittance surfaces on a number of critical components, such as heat receiver interior surfaces and parasitic load radiator (PLR) elements. An alumina-titania coating, which has been evaluated for solar-dynamic heat receiver canister applications, has been chosen for a PLR application (an electrical sink for excess power from the turboalternator/compressor) because of its demonstrated high emittance and high-temperature durability in vacuum. Under high vacuum conditions (+/- 10(exp -6) torr), the alumina-titania coating was found to be durable at temperatures of 1520 F (827 C) for approx. 2700 hours with no degradation in optical properties. This coating has been successfully applied to the 2-kW solar-dynamic ground test demonstrator at the NASA Lewis Research Center, to the 500 thermal-energy-storage containment canisters inside the heat receiver and to the PLR radiator. The solar-dynamic demonstrator has successfully operated for over 800 hours in Lewis large thermal/vacuum space environment facility, demonstrating the feasibility of solar-dynamic power generation for space applications.
Thermal expansion mismatch stresses and interfacial sulfur activity are the major factors producing primary Al2O3 scale spallation on high temperature alloys. However, moisture-induced delayed spallation appears as a secondary, but often dramatic, illustration of an additional mechanistic detail. A historical review of delayed failure of alumina scales and TBC s on superalloys is presented herein. Similarities with metallic phenomena suggest that hydrogen embrittlement from ambient humidity, resulting from the reaction Al+3H2O=Al(OH)3+3H(+)+3e(-), is the operative mechanism. This proposal was tested by standard cathodic hydrogen charging in 1N H2SO4, applied to Rene N5 pre-oxidized at 1150 C for 1000 1-hr cycles, and monitored by weight change, induced current, and microstructure. Here cathodic polarization at -2.0 V abruptly stripped mature Al2O3 scales at the oxide-metal interface. Anodic polarization at +2.0 V, however, produced alloy dissolution. Finally, with no applied voltage, the electrolyte alone produced neither scale spallation nor alloy dissolution. These experiments thus highlight the detrimental effects of hydrogen charging on alumina scale adhesion. It is proposed that interfacial hydrogen embrittlement is produced by moist air and is the root cause of both moisture-induced, delayed scale spallation and desktop TBC failures.
It has been well established that a few ppmw sulfur impurity may segregate to the interface of thermally grown alumina scales and the underlying substrate, resulting in bond degradation and premature spallation. This has been shown for NiAl and NiCrAl-based alloys, bare single crystal superalloys, or coated superalloys. The role of reactive elements (especially Y) has been to getter the sulfur in the bulk and preclude interfacial segregation. Pt additions are also very beneficial, however a similar thermodynamic explanation does not apply. The purpose of the present discussion is to highlight some observations of these effects on Rene'142, Rene'N5, PWA1480, and PWA1484. For PWA1480, we have mapped cyclic oxidation and spallation in terms of potential sulfur interfacial layers and found that a cumulative amount of about one monolayer is sufficient to degrade long term adhesion. Depending on substrate thickness, optimum performance occurs if sulfur is reduced below about 0.2-0.5 ppmw. This is accomplished in the laboratory by hydrogen annealing or commercially by melt-fluxing. Excellent 1150 C cyclic oxidation is thus demonstrated for desulfurized Rene'142, Rene'N5, and PWA1484. Alternatively, a series of N5 alloys provided by GE-AE have shown that as little as 15 ppmw of Y dopant was effective in providing remarkable scale adhesion. In support of a Y-S gettering mechanism, hydrogen annealing was unable to desulfurize these alloys from their initial level of 5 ppmw S. This impurity and critical doping level corresponds closely to YS or Y2S3 stoichiometry. In many cases, Y-doped alloys or alloys with marginal sulfur levels exhibit an oxidative sensitivity to the ambient humidity called Moisture-Induced Delayed Spallation (MIDS). After substantial scale growth, coupled with damage from repeated cycling, cold samples may spall after a period of time, breathing on them, or immersing them in water. While stress corrosion arguments may apply, we propose that the underlying cause is related to a hydrogen embrittlement reaction: Al alloy + 3 H2O = Al(OH)3 + 3H(+) + 3e(-). This mechanism is derived from an analogous moisture-induced hydrogen embrittlement mechanism originally shown for Ni3Al and FeAl intermetallics. Consequently, a cathodic hydrogen charging technique was used to demonstrate that electrolytic de-scaling occurs for these otherwise adherent alumina scales formed on Y-doped Rene'N5, in support of hydrogen effects. Finally, some TBC observations are discussed in light of all of the above. Plasma sprayed 8YSZ coatings, produced on PWA1484 without a bond coat, were found to survive more than 1000 1-hr cycles at 1100 C when desulfurized to below 0.1 ppmw. At higher sulfur (1.2 ppmw) levels, moisture sensitivity and delayed TBC failure, referred to as Desk Top Spallation, occurred at just 200 hr. Despite a large degree of scatter, a factor of 5 in life improvement is indicated for desulfurized samples in cyclic furnace tests, confirming the beneficial effect of low sulfur alloys on model TBC systems. (DTS and moisture effects are also observed on commercially applied PVD 7YSZ coatings on Rene'N5+Y with Pt-aluminide bond coats). These types of catastrophic failure were subverted on the model system by segmenting the substrate into a network of 0.010 high ribs, spaced in. apart, prior to plasma spraying. No failures occurred after 1000 cycles at 1150 C or after 2000 cycles at 1100 C, even after water immersion. The benefit is described in terms of elasticity models and a critical buckling stress.
Delayed interfacial scale failure takes place after cooling for samples of a Ni(Pt)Al-coated CMSX4 single crystal superalloy, cycled at 1150 C for up to 2000 hr. One sample exhibited premature coating grain boundary wrinkling, alumina scale spallation to bare metal, and a final weight loss of 3.3 mg/cm2 . Spallation under ambient conditions was monitored with time after cooldown and was found to continue for 24 hr. This produced up to 0.05 mg/cm2 additional loss for each hold, accumulating 0.7 mg/cm 2 (20 percent of the total) over the course of the test. After test termination, water immersion produced an additional 0.15 mg/cm2 loss. (A duplicate sample produced much less wrinkling and time dependent spalling, maintaining a net weight gain.) The results are consistent with the general phenomena of moisture-induced delayed spallation (MIDS) of mature, distressed alumina scales formed on oxidation resistant M-Al alloys. Relative ambient humidity is discussed as the factor controlling adsorbed moisture, reaction with the substrate, and hydrogen effects on interface strength.