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Surface Energy Anisotropy Effects on Pore-Channel Stability:Rayleigh Instabilities in m-Plane Sapphire

Description: Internal, high-aspect-ratio pore channels with their long axes parallel to the m(10{bar 1}0) plane of sapphire were generated through sequential application of photolithography, ion-beam etching and solid-state diffusion bonding. The axial orientation of channels within the m plane was systematically varied to sample a range of bounding-surface crystallographies. The morphologic evolution of these pore channels during anneals at 1700 C was recorded by postanneal optical microscopy. The development and growth of periodic axial variations in the pore channel radius was observed, and ultimately led to the formation of discrete pores. The wavelength and average pore spacing, assumed to reflect the kinetically dominant perturbation wavelength, varied with the in-plane pore channel orientation, as did the time for complete channel breakup. Results are compared to those previously obtained when pore channels were etched into c(0001)-plane sapphire and annealed under similar conditions. The results indicate a strong effect of surface stability on the evolution behavior.
Date: September 7, 2005
Creator: Santala, Melissa K. & Glaeser, Andreas M.
Partner: UNT Libraries Government Documents Department

High-temperature morphological evolution of lithographically introduced cavities in silicon carbide

Description: Internal cavities of controlled geometry and crystallography were introduced in 6H silicon carbide single crystals by combining lithographic methods, ion beam etching, and solid-state diffusion bonding. The morphological evolution of these internal cavities (negative crystals) in response to anneals of up to 128 h duration at 1900 degrees C was examined using optical microscopy. Surface energy anisotropy and faceting have a strong influence on both the geometric and kinetic characteristics of evolution. Decomposition of 12{bar 1}0 cavity edges into 101{bar 0} facets was observed after 16 h anneals, indicating that 12{bar 1}0 faces are not components of the Wulff shape. The shape evolution kinetics of penny-shaped cavities were also investigated. Experimentally observed evolution rates decreased much more rapidly with those predicted by a model in which surface diffusion is assumed to be rate-limiting. This suggests that the development of facets, and the associated loss of ledges and terraces during the initial stages of evolution results in an evolution process limited by the nucleation rate of attachment/detachment sites (ledges) on the facets.
Date: December 1, 2000
Creator: Narushima, Takayuki & Glaeser, Andreas M.
Partner: UNT Libraries Government Documents Department

Effects of Impurities on Alumina-Niobium InterfacialMicrostructures

Description: Optical microscopy, scanning electron microscopy, and transmission electron microscopy were employed to examine the interfacial microstructural effects of impurities in alumina substrates used to fabricate alumina-niobium interfaces via liquid-film-assisted joining. Three types of alumina were used: undoped high-purity single-crystal sapphire; a high-purity, high-strength polycrystalline alumina; and a lower-purity, lower-strength polycrystalline alumina. Interfaces formed between niobium and both the sapphire and high-purity polycrystalline alumina were free of detectable levels of impurities. In the lower-purity alumina, niobium silicides were observed at the alumina-niobium interface and on alumina grain boundaries near the interface. These silicides formed in small-grained regions of the alumina and were found to grow from the interface into the alumina along grain boundaries. Smaller silicide precipitates found on grain boundaries are believed to form upon cooling from the bonding temperature.
Date: June 20, 2005
Creator: McKeown, Joseph T.; Sugar, Joshua D.; Gronsky, Ronald & Glaeser,Andreas M.
Partner: UNT Libraries Government Documents Department

Joining of alumina via copper/niobium/copper interlayers

Description: Alumina has been joined at 1150 degrees C and 1400 degrees C using multilayer copper/niobium/copper interlayers. Four-point bend strengths are sensitive to processing temperature, bonding pressure, and furnace environment (ambient oxygen partial pressure). Under optimum conditions, joints with reproducibly high room temperature strengths (approximately equal 240 plus/minus 20 MPa) can be produced; most failures occur within the ceramic. Joints made with sapphire show that during bonding an initially continuous copper film undergoes a morphological instability, resulting in the formation of isolated copper-rich droplets/particles at the sapphire/interlayer interface, and extensive regions of direct bonding between sapphire and niobium. For optimized alumina bonds, bend tests at 800 degrees C-1100 degrees C indicate significant strength is retained; even at the highest test temperature, ceramic failure is observed. Post-bonding anneals at 1000 degrees C in vacuum or in gettered argon were used to assess joint stability and to probe the effect of ambient oxygen partial pressure on joint characteristics. Annealing in vacuum for up to 200 h causes no significant decrease in room temperature bend strength or change in fracture path. With increasing anneal time in a lower oxygen partial pressure environment, the fracture strength decreases only slightly, but the fracture path shifts from the ceramic to the interface.
Date: March 15, 2000
Creator: Marks, Robert A.; Chapman, Daniel R.; Danielson, David T. & Glaeser, Andreas M.
Partner: UNT Libraries Government Documents Department

Model studies of Rayleigh instabilities via microdesigned interfaces

Description: The energetic and kinetic properties of surfaces play a critical role in defining the microstructural changes that occur during sintering and high-temperature use of ceramics. Characterization of surface diffusion in ceramics is particularly difficult, and significant variations in reported values of surface diffusivities arise even in well-studied systems. Effects of impurities, surface energy anisotropy, and the onset of surface attachment limited kinetics (SALK) are believed to contribute to this variability. An overview of the use of Rayleigh instabilities as a means of characterizing surface diffusivities is presented. The development of models of morphological evolution that account for effects of surface energy anisotropy is reviewed, and the potential interplay between impurities and surface energy anisotropy is addressed. The status of experimental studies of Rayleigh instabilities in sapphire utilizing lithographically introduced pore channels of controlled geometry and crystallography is summarized. Results of model studies indicate that impurities can significantly influence both the spatial and temporal characteristics of Rayleigh instabilities; this is attributed at least in part to impurity effects on the surface energy anisotropy. Related model experiments indicate that the onset of SALK may also contribute significantly to apparent variations in surface diffusion coefficients.
Date: October 17, 2000
Creator: Glaeser, Andreas M.
Partner: UNT Libraries Government Documents Department

Processing of alumina-niobium interfaces via liquid-film-assistedjoining

Description: Alumina-niobium interfaces were fabricated at 1400 C via solid-state diffusion brazing of a 127-{micro}m-thick niobium foil between alumina blocks. Prior to brazing, some of the alumina mating surfaces, both polished and unpolished, were evaporation-coated with copper films {approx}1.4 {micro}m, {approx}3.0 {micro}m, and {approx}5.5 {micro}m thick to induce liquid-film-assisted joining at the brazing temperature. The effects of copper film thickness and surface roughness on fracture characteristics and ceramic-metal interfacial microstructure were investigated by room-temperature four-point bend tests, optical microscopy, profilometry, and atomic force microscopy. The average strength of bonds between niobium and polished alumina substrates increased with the introduction of copper film interlayers, and the scatter in strength tended to decrease, with an optimum combination of strength and Weibull modulus arising for a copper film thickness of 3.0 {micro}m. The strength characteristics of niobium bonded to unpolished alumina substrates were also improved by liquid-film-assisted joining, but were unaffected by the thickness of the copper interlayers.
Date: February 15, 2005
Creator: McKeown, Joseph T.; Sugar, Joshua D.; Gronsky, Ronald & Glaeser,Andreas M.
Partner: UNT Libraries Government Documents Department

Surface-Energy-Anisotropy-Induced Orientation Effects on RayleighInstabilities in Sapphire

Description: Arrays of controlled-geometry, semi-infinite pore channels of systematically varied crystallographic orientation were introduced into undoped m-plane (10{bar 1}0) sapphire substrates using microfabrication techniques and ion-beam etching and subsequently internalized by solid-state diffusion bonding. A series of anneals at 1700 C caused the breakup of these channels into discrete pores via Rayleigh instabilities. In all cases, channels broke up with a characteristic wavelength larger than that expected for a material with isotropic surface energy, reflecting stabilization effects due to surface-energy anisotropy. The breakup wavelength and the time required for complete breakup varied significantly with channel orientation. For most orientations, the instability wavelength for channels of radius R was in the range of 13.2R-25R, and complete breakup occurred within 2-10 h. To first order, the anneal times for complete breakup scale with the square of the breakup wavelength. Channels oriented along a <11{bar 2}0> direction had a wavelength of {approx} 139R, and required 468 h for complete breakup. Cross-sectional analysis of channels oriented along a <11{bar 2}0> direction showed the channel to be completely bounded by stable c(0001), r{l_brace}{bar 1}012{r_brace}, and s{l_brace}10{bar 1}1{r_brace} facets.
Date: January 1, 2006
Creator: Santala, Melissa & Glaeser, Andreas M.
Partner: UNT Libraries Government Documents Department

Reduced-Temperature Transient-Liquid-Phase Bonding of AluminaUsing a Ag-Cu-Based Brazing Alloy

Description: The mechanical properties and microstructural evolution ofmetal-ceramic bonds produced using a transient liquid phase (TLP) aredescribed. Alumina (Al2O3) was joined at 500 degrees C, 600 degrees C,and 700 degrees C using a multilayer In/Cusil-ABA (R) (commercialcopper-silver eutectic brazing alloy)/In interlayer. The introduction ofthin In cladding layers allows the system to bond at much lowertemperatures than those typically used for brazing with Cusil-ABA (R),thereby protecting temperature-sensitive components. After chemicalhomogenization, the interlayers retain an operating temperature rangesimilar to that of the brazed joints. TLP bonds made at 500 degrees C,600 degrees C, and 700 degrees C with holding times ranging from as lowas 1.5 h to 24 h had average fracture strengths above 220 MPa. Theeffects of bonding temperature and time on fracture strength aredescribed. Preliminary analysis of the interlayers shows that the Ag-Inor Cu-In intermetallic phases do not form. Considerations unique tosystems with two-phase core layers are discussed. Experiments usingsingle-crystal sapphire indicate rapid formation of a reaction layer at700 degrees C, suggesting the possibility of making strong bonds usinglower temperatures and/or shorter processing times.
Date: December 19, 2005
Creator: Hong, Sung Moo & Glaeser, Andreas M.
Partner: UNT Libraries Government Documents Department

Liquid-film assisted formation of alumina/niobium interfaces

Description: Alumina has been joined at 1400 degrees C using niobium-based interlayers. Two different joining approaches were compared: solid-state diffusion bonding using a niobium foil as an interlayer, and liquid-film assisted bonding using a multilayer copper/niobium/copper interlayer. In both cases, a 127-(mu)m thick niobium foil was used; =1.4-(mu)m or =3-(mu)m thick copper films flanked the niobium. Room-temperature four-point bend tests showed that the introduction of a copper film had a significant beneficial effect on the average strength and the strength distribution. Experiments using sapphire substrates indicated that during bonding the initially continuous copper film evolved into isolated copper-rich droplets/particles at the sapphire/interlayer interface, and extensive regions of direct bonding between sapphire and niobium. Film breakup appeared to initiate at either niobium grain boundary ridges, or at asperities or irregularities on the niobium surface that caused localized contact with the sapphire.
Date: June 16, 2002
Creator: Sugar, Joshua D.; McKeown, Joseph T.; Marks, Robert A. & Glaeser, Andreas M.
Partner: UNT Libraries Government Documents Department

Transient-Liquid-Phase and Liquid-Film-Assisted Joining ofCeramics

Description: Two joining methods, transient-liquid-phase (TLP) joining and liquid-film-assisted joining (LFAJ), have been used to bond alumina ceramics. Both methods rely on multilayer metallic interlayers designed to form thin liquid films at reduced temperatures. The liquid films either disappear by interdiffusion (TLP) or promote ceramic/metal interface formation and concurrent dewetting of the liquid film (LFAJ). Progress on extending the TLP method to lower temperatures by combining low-melting-point (<450 C) liquids and commercial reactive-metal brazes is described. Recent LFAJ work on joining alumina to niobium using copper films is presented.
Date: February 9, 2005
Creator: Sugar, Joshua D.; McKeown, Joseph T.; Akashi, Takaya; Hong, SungM.; Nakashima, Kunihiko & Glaeser, Andreas M.
Partner: UNT Libraries Government Documents Department