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At least 145 records · Page 8

Preparation Of Strong, Dense Potassium Beta''-Alumina Ceramic

Improved process for making mechanically strong, dense, phase-pure potassium beta''-alumina solid electrolyte (K-BASE) results in material superior to all previous K-BASE preparations and similar to commercial Na-BASE in strength, phase purity and high-temperature ionic conductivity. Potassium-based alkali-metal thermal-to-electric conversion (AMTEC) cells expected to operate efficiently at lower heat-input temperatures and lower rejection temperatures than sodium-based AMTEC cells, making them appropriate for somewhat different applications.

Williams, Roger M.↗

Improved Synthesis Of Potassium Beta' '-Alumina

Improved formulations of precursor materials synthesize nearly-phase-pure potassium beta' '-alumina solid electrolyte (K-BASE) powder. Materials are microhomogeneous powders (or, alternatively, gels) containing K(+,) Mg(2+), and Al(3+). K-BASE powder produced used in potassium-working-fluid alkali-metal thermal-to-electric conversion (K-AMTEC), in which heat-input and heat-rejection temperatures lower than sodium-working-fluid AMTEC (Na-AMTEC). Additional potential use lies in purification of pottassium by removal of sodium and calcium.

Williams, Roger M.↗

Sulfur Impurities and the Microstructure of Alumina Scales

The relationship between the microstructure of alumina scales, adhesion, and sulfur content was examined through a series of nickel alloys oxidized in 1100 to 1200 deg. C cyclic or isothermal exposures in air. In cyclic tests of undoped NiCrAl, adhesion was produced when the sulfur content was reduced, without any change in scale microstructure. Although interfacial voids were not observed in cyclic tests of NiCrAl, they were promoted by long-term isothermal exposures, by sulfur doping, and in most exposures of NiAl. Two single crystal superalloys, PWA 1480 and Rene' N5, were also tested, either in the as-received condition or after the sulfur content had been reduced to less than 1 ppmw by hydrogen annealing. The unannealed alloys always exhibited spalling to bare metal, but interfacial voids were not observed consistently. Desulfurized PWA 1480 and Rene' N5 exhibited remarkable adhesion and no voidage for either isothermal or cyclic exposures. The most consistent microstructural feature was that, for the cases where voids did form, the scale undersides exhibited corresponding areas with ridged oxide grain boundaries. Voids were not required for spallation nor were other microstructural features essential for adhesion. These observations are consistent with the model whereby scale spallation is controlled primarily by interfacial sulfur segregation and the consequent degradation of oxide-metal bonding.

Smialek, James L.↗

Chemically Derived Dense Alumina-Zirconia Composites for Improved Mechanical and Wear Erosion Properties

As a result of this funded project high purity Zirconia-Toughened Alumina (ZTA) ceramic powders with and without yttria were produced using metal alkoxide precursors. ZTA ceramic powders with varying volume percents of zirconia were prepared (7, 15, and 22%). Aluminum tri-sec butoxide, zirconium propoxide, and yttrium isopropoxide were the reagents used. Synthesis conditions were varied to control the hydrolysis and the aging conditions for the sol to gel transition. FTIR analysis and rheological characterization were used to follow the structural evolution during the sol to gel transition. The greater extent of hydrolysis and the build-up of structure measured from viscoelastic properties were consistent. Heat treatment was conducted to produce submicron grain fully crystalline ZTA ceramic powders. This improved materials should have enhanced properties such strength, toughness, and wear resistance for advanced structural applications, for example engine components in high technology aerospace applications.

Source record↗

Mechanical Behavior of Sapphire Reinforced Alumina Matrix Composites at Elevated Temperatures

Zirconia coated sapphire reinforced alumina matrix composites have been tested both after heat treatment to 1400 C and at temperatures ranging from 800 C to 1200 C in. air. Interfacial shear stress has also been measured with fiber pushout tests performed in air at room temperature, 800 C and 1OOO C. Matrix crack spacing was measured for the tensile tested composites and used to estimate interfacial shear stress up to 1200 C. Electron microscopy was used to determine the source of fiber fracture and to study interfacial failure within the composite.

Jaskowiak, Martha H.↗

High Temperature Properties of an Alumina Enhanced Thermal Barrier

The heatshield material requirements for future space vehicles (Aerobraking Orbital Transfer Vehicle & National Aerospace Plane) will depend upon the desired flight capability, configuration and location on the vehicle. These requirements will be more demanding and different from those derived for the materials used in the Shuttle Orbiter thermal protection system. Research was therefore initiated into improving the thermal efficiency of this class of materials by first characterizing their thermal and structural capabilities. Alternate material systems have been developed, tested, and compared with the baseline Shuttle system. This research resulted in the development of several very low density, high porosity (80-90%) materials with enhanced durability and temperature capability. One of the developments was a family of materials referred to as Fibrous Refractory Composite Insulation (FRCI) utilizing a mixture of fibers, each serving a unique purpose. One composition of the FRCI family with two fibers was adopted as a baseline material for use on the third and fourth Orbiters in selected areas due to its strength at a lower density compared to earlier materials. A further improvement in the FRCI family of materials is the Alumina Enhanced Thermal Barrier (AETB), a three-fiber composite. It has a higher temperature capability (composition dependent) than the baseline FRCI as proven by convective heating tests of one composition. AETB was studied to better characterize its performance at high temperature and the mechanisms by which its properties change. In conclusion, the shrinkage of AETB is a factor of six better than baseline FRCI at 1260 C (2300 F) with about a 20% improvement in mechanical properties. This improvement could translate into a 110 C (200 F) higher temperature capability in use as a heat shield material, but further testing in a convective heating environment is required to determine the actual improvement attainable.

Leiser, Daniel B.↗

Characterization of the Sol-Gel Transition for Zirconia-Toughened Alumina Precursors

High purity ZTA ceramic powders with and without yttria were produced using metal alkoxide precursors. ZTA ceramic powders with varying volume percents of zirconia were prepared (7, 15, and 22%). Aluminum tri-sec butoxide, zirconium propoxide, and yttrium isopropoxide were the reagents used. Synthesis conditions were varied to control the hydrolysis and the aging conditions for the sol to gel transition. FTIR analysis and theological characterization were used to follow the structural evolution during the sol to gel transition. The greater extent of hydrolysis and the build-up of structure measured from viscoelastic properties were consistent. Heat treatment was conducted to produce submicron grain fully crystalline ZTA ceramic powders. In all experimental cases a-alumina and tetragonal zirconia phases were confirmed even in the absence of yttria.

Moeti, I.↗

Nonprotective Alumina Growth in Sulfur-Doped NiAl(Zr)

The 1200 C oxidation behavior of NiAl was examined at various levels of sulfur and zirconium dopants to test the possibility of a critical S/Zr ratio required for adhesion. Cyclic furnace testing for 200 1 -hr cycles and interrupted testing for 500 hr were used as screening tests. Pure NiAl and NiAl(Zr) with 0. 14 at.% Zr were chosen as model base compositions; they exhibited normal, slow-growing scales (3 Mg/sq cm) with excellent adhesion for the Zr-doped alloys. NiAl with about 120 ppma S exhibited a substantial weight loss (-20 Mg/sq cm) in cyclic tests and a very large weight gain (+60 Mg/sq cm) in interrupted tests. The major surface phase remained as alpha -Al2O3. Sulfur doping the NiAl(Zr) alloy caused massive weight gains of 80 - 100 Mg/sq cm, swelling, cracking, and nearly complete conversion into NiAl2O4, and alpha- Al2O3. The initial objective of determining critical S/Zr ratios for adhesion was therefore unattainable. Initiation of the catastrophic attack was examined after a 10 hr exposure, revealing a few sites of broad, raised, and cracked ridges. In cross-section, the ridges appeared as modular intrusions, with a complex, fractal, oxide-metal interface. They were primarily alumina (with occasional entrapped islands of NiAl2O4 or pure Ni metal). They possessed a unique microstructure consisting of 0.3 microns lamellae, separated by 0.1 microns open channels. This allowed for rapid growth controlled by gaseous diffusion. The microstructure is discussed in terms of SO2 evolution and a sulfur-driven de-passivation process.

Smialek, James L.↗

Crystallography of Alumina-YAG-Eutectic

Multiple descriptions of the alumina-YAG eutectic crystallography appear in the ceramic literature. The orientation between two phases in a eutectic system has direct impact on residual stress, morphology, microstructural stability, and high temperature mechanical properties. A study to demonstrate that the different crystallographic relationships can be correlated with different growth constraints was undertaken. Fibers produced by Laser-Heated Float Zone (LHFZ) and Edge-defined Film-fed Growth (EFG) were examined. A map of the orientation relationship between Al2O3 and Y3Al5O12 and their relationship to the fiber growth axis as a function of pull rate are presented. Regions in which a single orientation predominates are identified.

Farmer, Serene C.↗

Slow Crack Growth Behavior and Life/Reliability Analysis of 96 wt % Alumina at Ambient Temperature With Various Specimen/Loading Configurations

Extensive constant stress-rate testing for 96 wt % alumina was conducted in room-temperature distilled water using four different specimen/loading configurations: rectangular beam test specimens under four-point uniaxial flexure, square plate test specimens in ring-on-ring biaxial flexure, square plate test specimens in ball-on-ring biaxial flexure, and dog-boned tensile test specimens in pure tension. The slow crack growth (SCG) parameter n was almost independent of specimen/loading configurations, in either four-point uniaxial flexure, ring-on-ring biaxial flexure, ball-on-ring biaxial flexure, or pure tension, ranging from n = 35 to 47 with an average value of n = 41.1 +/- 4.5. The prediction of fatigue strength/reliability based on the four-point uniaxial flexure data by using the CARES/Life design code as well as a simple PIA model was in good agreement with both the ring-on-ring biaxial and the ball-on-ring biaxial flexure data. A poor prediction using the PIA model was observed for the dog-boned tensile test specimens, presumably due to different flaw population involved in the tensile test specimens.

Choi, Sung R.↗

Alumina Volatility in Water Vapor at Elevated Temperatures

The volatility of alumina in high temperature water vapor was determined by a weight loss technique. Sapphire coupons were exposed at temperatures between 1250 and 1500 C, water partial pressures between 0.15 and 0.68 atm in oxygen, total pressure of 1 atm, and flowing gas velocities of 4.4 cm/s. The pressure dependence of sapphire volatility was consistent with AI(OH)3(g) formation. The enthalpy of reaction to form Al(OH)3(g) from sapphire and water vapor was determined to be 210 +/- 20 kJ/mol, comparing favorably to other studies. Microstructural examination of tested sapphire coupons revealed surface etching features consistent with a volatilization process.

Opila, Elizabeth J.↗

Microgravity Studies of Liquid-Liquid Phase Transitions in Alumina-Yttria Melts

The scientific objective of this research is to increase the fundamental knowledge base for liquid- phase processing of technologically important oxide materials. The experimental objective is to define conditions and hardware requirements for microgravity flight experiments to test and expand the experimental hypotheses that: 1. Liquid phase transitions can occur in undercooled melts by a diffusionless process. 2. Onset of the liquid phase transition is accompanied by a large change in the temperature dependence of melt viscosity. Experiments on undercooled YAG (Y3A15012)- and rare earth oxide aluminate composition liquids demonstrated a large departure from an Arrhenian temperature dependence of viscosity. Liquid YAG is nearly inviscid at its 2240 K melting point. Glass fibers were pulled from melts undercooled by ca. 600 K indicating that the viscosity is on the order of 100 Pans (1000 Poise) at 1600 K. This value of viscosity is 500 times greater than that obtained by extrapolation of data for temperatures above the melting point of YAG. These results show that the liquids are extremely fragile and that the onset of the highly non-Arrhenian viscosity-temperature relationship occurs at a temperature considerably below the equilibrium melting point of the solid phases. Further results on undercooled alumina-yttria melts containing 23-42 mole % yttrium oxide indicate that a congruent liquid-liquid phase transition occurs in the undercooled liquids. The rates of transition are inconsistent with a diffusion-limited process. This research is directed to investigation of the scientifically interesting phenomena of polyamorphism and fragility in undercooled rare earth oxide aluminum oxide liquids. The results bear on the technologically important problem of producing high value rare earth-based optical materials.

Guynes, Buddy↗

Potassium Beta-Alumina/Molybdenum/Potassium Electrochemical Cells

potassium alkali metal thermal-to-electric converter (K-AMTEC) cells utilizing potassium beta alumina solid electrolyte (K-BASE) are predicted to have improved properties for thermal to electric conversion at somewhat lower temperatures than sodium AMTEC's.

thermal-to-electric converter vapor pressure ceram↗

Moisture-Induced Delayed Spallation and Interfacial Hydrogen Embrittlement of Alumina Scales

While interfacial sulfur is the primary chemical factor affecting Al2O3 scale adhesion, moisture-induced delayed spallation appears as a secondary, but impressive, mechanistic detail. Similarities with bulk metallic phenomena suggest that hydrogen embrittlement from ambient humidity, resulting from the reaction Al(sub alloy)+3(H2O)(sub air) = Al(OH)(-) (sub 3) +3H(+) may be the operative mechanism. This proposal was tested on pre-oxidized Rene N5 by standard cathodic hydrogen charging in 1N H2SO4, as monitored by weight change, induced current, and microstructure. 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 acid electrolyte produced neither scale spallation nor alloy dissolution. Thus, hydrogen charging was detrimental to alumina scale adhesion. Moisture-induced interfacial hydrogen embrittlement is concluded to be the cause of delayed scale spallation and desktop thermal barrier coating failures.

Smialek, James L.↗

High Temperature Characteristics of Coplanar Waveguide on R-Plane Sapphire and Alumina

This paper presents the characteristics of coplanar waveguide transmission lines on R-plane sapphire and alumina over the temperature range of 25 to 400 C and the frequency range of 45 MHz to 50 GHz. A Thru-Reflect-Line calibration technique and open circuited terminated stubs are used to extract the attenuation and effective permittivity. It is shown that the effective permittivity of the transmission lines and, therefore, the relative dielectric constant of the two substrates increase linearly with temperature. The attenuation of the coplanar waveguide varies linearly with temperature through 200 C, and increases at a greater rate above 200 C.

Ponchak, George E.↗

Heat Transfer Modeling and Validation for Optically Thick Alumina Fibrous Insulation

Combined radiation/conduction heat transfer through unbonded alumina fibrous insulation was modeled using the diffusion approximation for modeling the radiation component of heat transfer in the optically thick insulation. The validity of the heat transfer model was investigated by comparison to previously reported experimental effective thermal conductivity data over the insulation density range of 24 to 96 kg/cu m, with a pressure range of 0.001 to 750 torr (0.1 to 101.3 x 10(exp 3) Pa), and test sample hot side temperature range of 530 to 1360 K. The model was further validated by comparison to thermal conductivity measurements using the transient step heating technique on an insulation sample at a density of 144 kg/cu m over a pressure range of 0.001 to 760 torr, and temperature range of 290 to 1090 K.

Daryabeigi, Kamran↗