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Generation of Chloride Active Defects at the Aluminum Oxide Surface for the Study of Localized Corrosion Initiation

Description: The generation of surface defects on electron cyclotron resonance (ECR) plasma derived aluminum oxide films has been studied. We find that Cl active O vacancies can be generated using electron and ion irradiation yielding surface concentrations of 3 xl 013 to 1X1014 sites"cm-2. These values correspond to surface defect concentrations of 3 to 10% when compared to ordered, crystalline u-alumina. The vacancies appear to be responsible for increased surface O concentrations when immersed in water. Anodic polarization of irradiated films yields a decrease in the stable pitting potential which correlates with electron dose.
Date: December 7, 1998
Creator: Barbour, J.C.; Missert, N.; Son, K.-A; Wall, F.D. & Zavadil, K.R.
Partner: UNT Libraries Government Documents Department

Variations in the Nature of Metal Adsorption on Ultrathin Al(2)O(3) Films

Description: First-principles density-functional calculations are used to study metal adsorption (Li, K, Y, Nb, Ru, Pd, Pt, Cu, Ag, Au, and Al at 1/3-4 monolayer coverages) atop 5 ~ A1203 films on Al(Ill). The oxide-metal bond is ionic at Iow coverages but, with interesting exceptions, caused by polari@i ,~-cE!vED at high coverages where the overlayer is metallic. Binding trends are explained in terms of s'imp e concepts. Increasing overlayer thickness can cause the adsorbate-oxide interface structure to than . %lEc o ~ 1998 and while some metals wet, most do not.
Date: November 24, 1998
Creator: Bogicevic, A. & Jennison, D.R.
Partner: UNT Libraries Government Documents Department

Characterization of microstructure and crack propagation in alumina using orientation imaging microscopy (OIM). December 1996

Description: A more complete description requires the lattice orientations of a statistically significant number of grains, coupled with morphology such as grain size and shape; this can be obtained using orientation imaging microscopy (OIM), which uses crystallographic orientation data from Backscattered Electron Kikuchi patterns (BEKP) collected using a SEM. This report describes the OIM results for alumina; these include image quality maps, grain boundary maps, pole figures, and lattice misorientations depicted on MacKenzie plot and in Rodrigues space. High quality BEKP were obtained and the images and data readily reveal the grain morphology, texture, and grain boundary misorientations, including those for cracked boundaries. A larger number of grains should be measured to make statistical comparisons between materials with different processing histories.
Date: December 1, 1996
Creator: Glass, S.J.; Michael, J.R.; Readey, M.J.; Wright, S.I. & Field, D.P.
Partner: UNT Libraries Government Documents Department

Lightweight alumina refractory aggregate. Phase 2, Pilot scale development

Description: Kilogram quantities of refractory aggregate were prepared from both a paste and a pelletized form of extruder feed material in both bench and pilot-scale equipment. The 99{sup +} % alumina aggregate exhibited a bulk density approaching 2.5 g/cm{sup 3} and a fired strength slightly lower than fused alumina. Based on initial evaluation by two refractory manufacturers in brick or castable applications, the new aggregate offered adequate strength with thermal conductivity reductions up to 34%, depending on the temperature and application of the new aggregate in these initial trials. The new aggregate was simply substituted for Tabular{trademark} in the refractory formulation. Thus, there is room for improvement through formulation optimization with the lightweight aggregate. The new aggregate offers a unique combination of density, strength, and thermal properties not available in current aggregate. To this point in time, technical development has led to a pelletized formulation with borderline physical form leaving the Eirich mixer. The formulation requires further development to provide more latitude for the production of pelletized material without forming paste, while still reducing the bulk density slightly to reach the 2.5 g/cm{sup 3} target. The preferred, pelletized process flowsheet was outlined and a preliminary economic feasibility study performed based on a process retrofit into Alcoa`s Arkansas tabular production facilities. Based on an assumed market demand of 20,000 mt/year and an assumed selling price of $0.65/lb (25% more than the current selling price of Tabular{trademark}, on a volume basis), economics were favorable. Decision on whether to proceed into Phase 3 (full- scale demonstration) will be based on a formal market survey in 1994 October.
Date: November 1, 1994
Creator: Swansiger, T.G. & Pearson, A.
Partner: UNT Libraries Government Documents Department

Crystal phases and lattice dynamics of slip-cast {beta}{prime}-sialons

Description: The crystal structures and phonon densities of states (DOS) of {beta}{prime}-Sialon ceramics, Si{sub 6-z}Al{sub z}O{sub z}N{sub 8-z} (O {le} z {le} 6), prepared by a novel slip-cast method were studied by neutron scattering techniques. A Rietveld analysis of the diffraction patterns shows that samples of z < 4 form a single-phase solid solution of Si-Al-O-N isostructural to {beta}-Si{sub 3}N{sub 4} (space group P6{sub 3}/m). Within this structure there is a consistent preferred occupation of O on the 2c sites and N on the 6h sites. For z > 4 the materials exhibit multiple-phase structure. The observed phonon DOS of the O {le} z {le} 4 ceramics displays phonon bands at about 50 and 115 meV. These features are considerably broader than the corresponding ones in {beta}-Si{sub 3}N{sub 4} powder. As z increases, effects due to atomic disorder lead to an overlap of the two phonon bands and a complete fill up of the phonon gap at {approximately} 100 meV observed in Si{sub 3}N{sub 4}.
Date: December 31, 1995
Creator: Loong, C.K.; Richardson, J.W. Jr.; Suzuki, S. & Ozawa, M.
Partner: UNT Libraries Government Documents Department

In Situ Transmission Electron Microscopy Heating Studies of Particle Coalescence and Microstructure Evolution in Nanosized Ceramics

Description: Final report on in-situ transmission microscopy heating studies of particle coalescence and microstructure evolution in nanosized ceramics. Report includes summary of work on particle shape changes and stress effects, and novel infiltration techniques in the processing of alumina based ceramics.
Date: June 2, 2006
Partner: UNT Libraries Government Documents Department

Dynamics of metal/ceramic interface formation.

Description: We summarize the work of the Laboratory Directed Research and Development (LDRD) project 'Dynamics of Metal/Ceramic Interface Formation.' Low-energy electron microscopy (LEEM) was used to monitor in real time how the metal/ceramic interface between the alloy NiAl and its oxide formed. The interfaces were synthesized by exposing the clean alloy to oxygen at either low or high temperature. During low-temperature exposure, an initially amorphous oxide formed. With annealing, this oxide crystallizes into one type of alumina that has two orientational domains. While the oxide is relatively uniform, it contained pinholes, which coarsened with annealing. In marked contrast, high-temperature exposure directly produced rod-shaped islands of crystalline oxide. These rods were all aligned along the substrate's [001] direction and could be many microns in length. Real-time observations showed that the rods can both grow and shrink by addition and subtraction, respectively, at their ends.
Date: December 1, 2003
Creator: McCarty, Kevin F.
Partner: UNT Libraries Government Documents Department

Determination of Ideal Broth Formulations Needed to Prepare Hydrous Aluminum Oxide Microspheres via the Internal Gelation Process

Description: A simple test-tube methodology was used to determine optimum process parameters for preparing hydrous aluminum oxide microspheres by the internal gelation process. Broth formulations of aluminum, hexamethylenetetramine, and urea were found that can be used to prepare hydrous aluminum oxide gel spheres in the temperature range of 60-90 C. A few gel-forming runs were made in which microspheres were prepared with some of these formulations in order to equate the test-tube gelation times with actual gelation times. These preparations confirmed that the test-tube methodology is reliable for determining the ideal broths.
Date: February 1, 2009
Creator: Collins, Jack Lee & Pye, S. L.
Partner: UNT Libraries Government Documents Department

Thermal shock behavior of alumina/MoSi2 plasma sprayed laminated composites

Description: Alumina (Al{sub 2}O{sub 3}) is very susceptible to thermal shock, which leads to strength degradation. By reinforcing Al{sub 2}O{sub 3} with molybdenum disilicide (MoSi{sub 2}) layers, the tolerance to damage caused by thermal shock can be improved. The thermal shock resistance of plasma sprayed Al{sub 2}O{sub 3}/MoSi{sub 2} laminated composites were investigated. Three laminate microstructures having different layer thickness were fabricated by atmospheric plasma spraying while maintaining a 50/50-volume fraction. Quenching experiments done on 4-point bend bars showed a gradual decrease in the strength as the change in temperature ({Delta}T) increased. Thermal shock resistant parameters (R{prime} and R-quadruple prime) provided a representative numerical value of the thermal shock resistance for the laminated composites. The corresponding material properties for the different microstructures were determined experimentally in order to calculate the R{prime} and R quadruple prime values. The intermediate layered composite showed the highest R-quadruple prime va1ue at 1061 {micro}m, while the thin layered composite had the highest R{prime} value at 474 W/m.
Date: January 1, 2001
Creator: Castro, R. G. (Richard G.); Petrovic, J. J.; Vaidya, R. U. (Rajendra U.) & Mendoza, D. (Daniel)
Partner: UNT Libraries Government Documents Department

Low-energy deposition of high-strength Al(0) alloys from an ECR plasma

Description: Low-energy deposition of Al(O) alloys from an electron cyclotron resonance (ECR) plasma offers a scaleable method for the synthesis of thick, high-strength Al layers. This work compares alloy layers formed by an ECR-0{sub 2} plasma in conjunction with Al evaporation to 0-implanted Al (ion energies 25-200 keV); and it examines the effects of volume fraction of A1{sub 2}0{sub 3} phase and deposition temperature on the yield stress of the material. TEM showed the Al(O) alloys contain a dense dispersion of small {gamma}-Al{sub 2}0{sub 3} precipitates ({approximately}l nm) in a fine-grain (10-100 nm) fcc Al matrix when deposited at a temperature of {approximately}100C, similar to the microstructure for gigapascal-strength 0-implanted Al. Nanoindentation gave hardnesses for ECR films from 1.1 to 3.2 GPa, and finite-element modeling gave yield stresses up to 1.3 {plus_minus} 0.2 GPa with an elastic modulus of 66 GPa {plus_minus} 6 GPa (similar to pure bulk Al). The yield stress of a polycrystalline pure Al layer was only 0.19 {plus_minus} 0.02 GPa, which was increased to 0.87 {plus_minus} 0.15 GPa by implantation with 5 at. % 0.
Date: December 31, 1995
Creator: Barbour, J.C.; Follstaedt, D.M.; Knapp, J.A.; Myers, S.M.; Marshall, D.A. & Lad, R.J.
Partner: UNT Libraries Government Documents Department

Mechanical behavior of robocast alumina

Description: Direct fabrication of alumina parts by robocasting was completed. This method is based on three-dimensional deposition of binderless aqueous alumina slurries. Parts were made with different deposition paths and mechanical testing performed to determine the effects of bead alignment. Properties were also compared to alumina processed more traditionally.
Date: December 1, 1998
Creator: Denham, H.B.; Cesarano, J. III; King, B.H. & Calvert, P.
Partner: UNT Libraries Government Documents Department

Advanced process development for high reflector coatings on solar concentrator panels. Final letter report

Description: Objectives were to develop and demonstrate the manufacturing process for vacuum deposition of low-cost thin-film high reflectance coatings onto large solar concentrator panels; demonstrate thin-film deposition processes for commercialization of this technology by United Solar Technologies (UST); apply reflective coatings to solar concentrator panels for prototype application by UST.
Date: October 1, 1996
Creator: Martin, P.M.; Stewart, C.D.; Bennett, W.D. & Johnston, J.W.
Partner: UNT Libraries Government Documents Department

Microstructural Characterization of Water-Rich Boehmite (AlO(OH)): TEM Correlation of Apparently Divergent XRD and TGA Results

Description: An understanding of the solid-phase thermodynamics and aqueous speciation of aluminum is critical to our ability to understand and predict processes in a wide variety of geologic and industrial settings. Boehmite (AIO(OH)) is an important phase in the system Al<sub>2</sub>O<sub>3</sub>-H<sub>2</sub>O that has been the subject of a number of structural and thermodynamic studies since its initial synthesis [l] and discovery in nature [2]. Unfortunately, it has long been recognized that thermogravimetric analysis (TGA) of both synthetic and natural boehmite samples (that appear well crystallized by powder XRD methods) yields significant excess water - typically losing 16-16.5 wt. % on heating as compared with a nominal expected weight loss of 15.0 wt. % [3,4]. The boehmite used in our experiments was synthesized hydrothermally from acid-washed gibbsite (Al(OH)<suv>3</sub>) at 200°C. Powder XRD and SEM examination showed no evidence of the presence a contaminant phase. The TGA patterns do not suggest that this is due to adsorbed water, so a structural source is likely. We therefore undertook to examine this material by TEM to clarify this phenomenon.
Date: August 1999
Creator: Allard, L. F.; Anovitz, L. M.; Benezeth, P.; Coffey, D. W.; Palmer, D. A.; Porter, W. D. et al.
Partner: UNT Libraries Government Documents Department

Atomic structure of the {sigma}5 (210)/[001] symmetric tilt grain boundary in yttrium aluminum garnet

Description: The {Sigma}5(210)/[100] symmetric tilt grain boundary in YAG was produced by UHV diffusion bonding precisely oriented single crystals. The boundary has been characterized by HREM along two different directions, parallel and perpendicular to the tilt axis. Models of the atomic structure of the boundary were formed following the Coincident Site Lattice scheme. The resulting models are equivalent to twins formed at the atomic scale. The high resolution images show no rigid crystal translations away from the perfect mirror reflection relation. Comparison of the simulated images using the atomic model as input with the experimental images identifies the plane of mirror symmetry. The atomic model is shown to be in good agreement with the experimental images when viewed parallel to tilt axis, but disagrees with the images perpendicular to tilt axis. Agreement between simulated and experimental images can be improved by changing the composition of the grain boundary with respect to the bulk. To reach a more certain conclusion on the structure of the grain boundary will require additional theoretical calculations.
Date: June 24, 1996
Creator: Campbell, G.H. & King, W.E.
Partner: UNT Libraries Government Documents Department

Residual stress distribution in an Al{sub 2}O{sub 3}-Ni joint bonded with a composite layer

Description: Neutron diffraction was used to study the residual stress distribution in an axisymmetric Al{sub 2}O{sub 3}-Ni joint bonded with a 40 vol% Al{sub 2}O{sub 3}-60 vol% Ni composite layer. A series of measurements was taken along the axis of symmetry through the Al{sub 2}O{sub 3} and composite layers. It is shown that after taking into account the finite neutron diffraction sampling volume, both the trends and peak values of the experimental strain distribution were in excellent agreement with calculations of a simple finite element model, where the rule-of-mixtures approach was used to describe the constitutive behavior of the composite interlayer. In particular, the predicted steep strain gradient near the interface was confirmed by the experimental data.
Date: July 1, 1996
Creator: Wang, X.L.; Watkins, T.R.; Rabin, B.H.; Williamson, R.L. & Bruck, H.A.
Partner: UNT Libraries Government Documents Department

Tribological Characteristics of sputtered Au/Cr films on alumina substrates at elevated temperatures

Description: This paper describes research to evaluate the tribological properties of alumina pins sliding against thin sputtered gold films deposited on alumina disk substrates. A 250 {angstrom} thick chromium interlayer was first deposited onto the alumina test disks to enhance adhesion and high temperature wetting of the gold films. The Au/Cr films were tribotested in pure sliding in a pin-on-disk tribometer under a 4.9 N load at 1 m/s. The test atmosphere was room air at temperatures of 25, 500, and 800 C and the test duration varied from 60 to 540 min. The use of the Au/Cr films reduced friction by about a factor of two compared to the unlubricated alumina sliding couple. The coating prevented wear of the alumina substrate disks and reduced pin wear by one to two orders of magnitude. In addition, wear lives in excess of 200 000 sliding passes (9 hr) were observed during sliding at 800 C. Results suggest that these films show promise for the practical lubrication of many high temperature sliding components.
Date: December 31, 1993
Creator: Benoy, P.A. & DellaCorte, C.
Partner: UNT Libraries Government Documents Department

Investigation of the effect of microstructure on the R-Curve behavior of metal-ceramic composites

Description: An investigation was made into the effect of microstructure on the peak toughness and shape of the crack growth resistance curves for two ceramic-metal composites. An Al{sup 2}O{sup 3}/Al composite formed by Reactive Metal Penetration was used along with an AlN/Al composite formed using a reactive infiltration technique. The results indicate that the toughness increases with an increase in the volume fraction of the metal phase for a particular composite composition, and the peak toughness and shape of the R-Curve also depend on the composite microstructure and metal composition.
Date: July 1, 1995
Creator: Ellerby, D.T.; Flinn, B.D.; Scott, W.D.; Bordia, R.K.; Ewsuk, K.G.; Loehman, R.E. et al.
Partner: UNT Libraries Government Documents Department

Stability of eutectic interface during directional solidification

Description: Directional solidification of eutectic alloys shows different types of eutectic morphologies. These include lamellar, rod, oscillating and tilting modes. The growth of these morphologies occurs with a macroscopically planar interface. However, under certain conditions, the planar eutectic front becomes unstable and gives rise to a cellular or a dendritic structure. This instability leads to the cellular/dendritic structure of either a primary phase or a two-phase structure. The objective of this work is to develop a fundamental understanding of the instability of eutectic structure into cellular/dendritic structures of a single phase and of two-phases. Experimental studies have been carried out to examine the transition from a planar to two-phase cellular and dendritic structures in a ceramic system of Alumina-Zirconia (Al{sub 2}O{sub 3}-ZrO{sub 2}) and in a transparent organic system of carbon tetrabromide and hexachloroethane (CBr{sub 4}-C{sub 2}Cl{sub 6}). Several aspects of eutectic interface stability have been examined.
Date: April 23, 1996
Creator: Han, S.H.
Partner: UNT Libraries Government Documents Department

Development of high performance refractory fibers with enhanced insulating properties and longer service lifetimes: Phase 2, Improved refractory fiber and industrial benefit development. Final report

Description: This is Phase II of a three-phase study for the development of high performance refractory fibers with enhanced insulating properties and longer service lifetimes, for use in the aluminum, glass, cement, and iron and steel industries. Fiberization of 24 out of 25 compositions in the Al{sub 2}O{sub 3}-Si0{sub 2}-Zr0{sub 2} system were achieved. These 24 and three existing fiber compositions were evaluated: The shrinkage and the crystalline and vitreous phases were determined vs heat treatment time and temperature. Four theoretical models were developed: Shrinkage, devitrification kinetics, density change, and fiberization. Although some of the fibers formed during Phase II had properties as good as the reference ASZ fiber, no fiber had a significantly improved performance. This work, although not entirely successful, did produce significant benefits to refractory insulating fiber manufacturers and users: Mechanisms of both linear and thickness shrinkage for vitreous refractory fibers were determined, devitrification kinetics were quantified and used in models to predict shrinkage during service, and the mechanism of fiber formation in the melt spinning process was studied.
Date: May 1, 1995
Creator: Cai, Yifang; Curtis, J.M.; DePoorter, G.L.; Martin, P.C. & Munoz, D.R.
Partner: UNT Libraries Government Documents Department

Strain measurements in thermally grown alumina scales using ruby fluorescence

Description: We have measured strains in alumina scales thermally grown on Fe-Cr- Al alloys by exploiting the strain dependence of the ruby luminescence line. Measurements were done on Fe-5Cr-28Al and Fe-18Cr-10Al (at.%, bal. Fe) oxidized between 300-1300 C with periodic cycling to room temperature. Significantly different levels of strain buildup were observed in scales on these alloys. Results on similar alloys containing a dilute reactive element (Zr or Hf) are also presented. We observe that scales on alloys containing a reactive element (RE) can support higher strains than scales on RE-free alloys. With the luminescence technique, strain relief associated with spallation thresholds is readily observed. In early stage oxidation, the evolution of transition phases is monitored using Raman and fluorescence spectroscopies. The fluorescence technique also provides a sensitive probe of early stage formation of {alpha}-Al{sub 2}O{sub 3}. It appears that, in presence of Cr{sub 2}O{sub 3} or Fe{sub 2}O{sub 3}, the {alpha}-alumina phase can form at anomalously low temperatures.
Date: December 31, 1996
Creator: Veal, B. W.; Natesan, K.; Koshelev, I.; Grimsditch, M.; Renusch, D. & Hou, P. Y.
Partner: UNT Libraries Government Documents Department