Surface step induced gap heating in the Shuttle Thermal Protection System
Previously cited in issue 5, p. 606, Accession no. A83-16533
Petley, D. H.↗
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Step Free Surface Heteroepitaxy of 3C-SiC Layers on Patterned 4H/6H-SiC Mesas and Cantilevers
Most SiC devices are implemented in homoepitaxial films grown on 4H/6H-SiC wafers with surfaces 3 degrees to 8 degrees off-axis from the (0001) basal plane. This approach has not prevented many substrate crystal defects from propagating into SiC epilayers, and does not permit the realization of SiC heteropolytype devices. This presentation describes recent advances in SiC epitaxial growth that begun to overcome the above shortcomings for arrays of mesas patterned into on-axis 4H/6H-SiC wafers. First, we demonstrated that atomic-scale surface steps can be completely eliminated from 4H/6H-SiC mesas via on-axis homoepitaxial step-flow growth, forming (0001) basal plane surfaces (up to 0.4 mm x 0.4 mm) for larger than previously thought possible. Step-free surface areas were then extended by growth fo thin lateral cantilevers from the mesa tops. These lateral cantilevers enabled substrate defects to be reduced and relocated in homoepitaxial films in a manner not possible with off-axis SiC growth. Finally, growth of vastly improved 3C-SiC heterofilms was achieved on 4H/6H-SiC mesas using the recently develop step-free surface heteroepitaxy process. These epitaxial growth developments should enable improved homojunction and heterojunction silicon carbide prototype devices.
Neudeck, Philip G.↗
Growth of Defect-Free 3C-Sic on 4H- and 6H-SIC Mesas Using Step-Free Surface Heteroepitaxy
A new growth process, herein named step-free surface heteroepitaxy, has achieved 3C-SiC films completely free of double positioning boundaries and stacking faults on 4H-SiC and 6H-SiC substrate mesas. The process is based upon the initial 2-dimensional nucleation and lateral expansion of a single island of 3C-SiC on a 4H- or 6H-SiC mesa surface that is completely free of bilayer surface steps. Our experimental results indicate that substrate-epilayer in-plane lattice mismatch (Delta/a = 0.0854% for 3C/4H) is at least partially relieved parallel to the interface in the initial bilayers of the heterofilm, producing an at least partially relaxed 3C-SiC film without dislocations that undesirably thread through the thickness of the epilayer. This result should enable realization of improved 3C-SiC devices.
Neudeck, Philip G.↗
Growth of Defect-Free 3C-SiC on 4H- and 6H-SiC Mesas Using Step-Free Surface Heteroepitaxy
A new growth process, herein named step-free surface heteroepitaxy, has achieved 3CSiC films completely free of double positioning boundaries and stacking faults on 4H-SiC and 6H-SiC substrate mesas. The process is based upon the initial 2-dimensional nucleation and lateral expansion of a single island of 3C-SiC on a 4H- or 6H-SiC mesa surface that is completely free of bilayer surface steps. Our experimental results indicate that substrate-epilayer in-plane lattice mismatch (delta a/a = 0.0854% for 3C/4H) is at least partially relieved parallel to the interface in the initial bilayers of the heterofilm, producing an at least partially relaxed 3C-SiC film without dislocations that undesirably thread through the thickness of the epilayer. This result should enable realization of improved 3C-SiC devices.
Neudeck, Philip G.↗
Characterization of 3C-SiC Films Grown on 4H- and 6H-SiC Substrate Mesas During Step-Free Surface Heteroepitaxy
This paper reports detailed structural characterization of 3C-SiC heteroepitaxial films grown on 4H- and 6H-SiC mesa surfaces. 3C-SiC heterofilms grown by the "step-free surface heteroepitaxy" process, free of double-positioning boundary (DPB) and stacking-fault (SF) defects, were compared to less-optimized 3C-SiC heterofilms using High Resolution X-ray Diffraction (HRXRD), High Resolution Cross-sectional Transmission Electron Microscopy (HRXTEM), molten potassium hydroxide (KOH) etching, and dry thermal oxidation. The results suggest that step free surface heteroepitaxy enables remarkably benign partial lattice mismatch strain relief during heterofilm growth.
Neudeck, Philip G.↗
LEED study of steps and facets on a Re surface
Low energy electron diffraction pattern from surface steps and facets resulting from recrystallization of Re single crystal
Feinstein, L. G.↗
Step Free Surface Heteroepitaxy of 3C-SiC Layers on Patterned 4H/6H-SiC Mesas and Cantilevers
The off-axis approach to SiC epitaxial growth has not prevented many substrate crystal defects from propagating into SiC epilayers, and does not permit the realization of SiC heteropolytype devices. This paper reviews recent advancements in SiC epitaxial growth that begin to overcome the above shortcomings for arrays of device-sized mesas patterned into on-axis 4H/6HSiC wafers. These on-axis mesa growth techniques have produced 4H/6H-SiC homoepilayers and 3C-SiC heteroepilayers with substantially lower dislocation densities. The results should enable improved homojunction and heterojunction silicon carbide prototype devices.
Neudeck, P. G.↗
Homoepitaxial "Web Growth" of SiC to Terminate C-Axis Screw Dislocations and Enlarge Step-Free Surfaces
Homoepitaxial CVD growth of thin lateral cantilevers emanating from the edges of mesa patterns dry-etched into on-axis commercial 4H-SiC substrates prior to growth is reported. Cantilevers on the order of a micrometer thick extending tens of micrometers from the edge of a mesa have been grown. The termination of vertically propagating screw dislocations, including a micropipe, that are overgrown by the cantilevers has been demonstrated, in large part because the crystal structure of the cantilevers is established laterally from the mesa sidewalls. This technique could help reduce performance-degrading dislocations in SiC electrical devices.
Neudeck, Philip G.↗
Homoepitaxial and Heteroepitaxial Growth on Step-Free SiC Mesas
This article describes the initial discovery and development of new approaches to SiC homoepitaxial and heteroepitaxial growth. These approaches are based upon the previously unanticipated ability to effectively supress two-dimensional nucleation of 3C-SiC on large basal plane terraces that form between growth steps when epitaxy is carried out on 4H- and 6H-SiC nearly on-axis substrates. After subdividing the growth surface into mesa regions, pure stepflow homoeptixay with no terrace nucleation was then used to grow all existing surface steps off the edges of screw-dislocation-free mesas, leaving behind perfectly on-axis (0001) basal plane mesa surfaces completely free of atomic-scale steps. Step-free mesa surfaces as large as 0.4 mm x 0.4 mm were experimentally realized, with the yield and size of step-free mesas being initally limited by substrate screw dislocations. Continued epitaxial growth following step-free surface formation leads to the formation of thin lateral cantilevers that extend the step-free surface area from the top edge of the mesa sidewalls. By selecting a proper pre-growth mesa shape and crystallographic orientation, the rate of cantilever growth can be greatly enhanced in a web growth process that has been used to (1) enlarge step-free surface areas and (2) overgrow and laterally relocate micropipes and screw dislocations. A new growth process, named step-free surface heteroepitaxy, has been developed to achieve 3C-SiC films on 4H- and 6H-SiC substrate mesas completely free of double positioning boundary and stacking fault defects. The process is based upon the controlled terrace nucleation and lateral expansion of a single island of 3C-SiC across a step-free mesa surface. Experimental results indicate that substrateepilayer lattice mismatch is at least partially relieved parallel to the interface without dislocations that undesirably thread through the thickness of the epilayer. These results should enable realization of improved SiC homojunction and heterojunction devices. In addition, these experiments offer important insights into the nature of polytypism during SiC crystal growth.
Neudeck, Philip G.↗
Investigation of the influence of a step change in surface roughness on turbulent heat transfer
The use is studied of smooth heat flux gages on the otherwise very rough SSME fuel pump turbine blades. To gain insights into behavior of such installations, fluid mechanics and heat transfer data were collected and are reported for a turbulent boundary layer over a surface with a step change from a rough surface to a smooth surface. The first 0.9 m length of the flat plate test surface was roughened with 1.27 mm hemispheres in a staggered, uniform array spaced 2 base diameters apart. The remaining 1.5 m length was smooth. The effect of the alignment of the smooth surface with respect to the rough surface was also studied by conducting experiments with the smooth surface aligned with the bases or alternatively with the crests of the roughness elements. Stanton number distributions, skin friction distributions, and boundary layer profiles of temperature and velocity are reported and are compared to previous data for both all rough and all smooth wall cases. The experiments show that the step change from rough to smooth has a dramatic effect on the convective heat transfer. It is concluded that use of smooth heat flux gages on otherwise rough surfaces could cause large errors.
Taylor, Robert P.↗
Optically Enhanced Bonding Workstation for Robust Bonding
Process control is one of the methods recommended by the FAA to reduce risk in fabrication of structurally bonded composite joints for aircraft structure based on guidance provided in circular AC-107B for certification of structurally bonded joints. An Optically Enhanced Bonding Workstation is presented here that reduces the risk in bonded joint fabrication. Results will be presented demonstrating the benefits of process monitoring and its ability to reduce risk in performing pre-bond composite surface preparation steps. This supports reduction in the timeline to certification of bonded composite structures through development of a robust bonding process upstream of any part certification steps. Sanding surface preparation has been identified as a high risk process step that is known to impact bond performance. Control of sanding during surface preparation can be performed using portable surface analysis tools previously identified including included gloss, color, Fourier Transform Infrared spectroscopy (FTIR) and optically stimulated electron emissions (OSEE). Threshold limits for the surface analysis tool measurements were determined based on an example objective bonding system utilizing a common EA9394 paste adhesive measured using standard double cantilever beam fracture toughness testing. The patented Optically Enhanced Bonding Workstation (OEBW), was tailored to monitor and control the epoxy composite surface preparation step. Surface analysis tool threshold limits were incorporated into the OEBW to demonstrate improved composite bond performance through process control. The surface analysis tools investigated here can easily be incorporated into an automated system due to their applicability to rapidly quantify the composite sanded surface treatment and their portability.
Kutscha, Eileen O.↗
Protein Crystal Growth Dynamics and Impurity Incorporation
The general concepts and theories of crystal growth are proven to work for biomolecular crystallization. This allowed us to extract basic parameters controlling growth kinetics - free surface energy, alpha, and kinetic coefficient, beta, for steps. Surface energy per molecular site in thermal units, alpha(omega)(sup 2/3)/kT approx. = 1, is close to the one for inorganic crystals in solution (omega is the specific molecular volume, T is the temperature). Entropic restrictions on incorporation of biomolecules into the lattice reduce the incorporation rate, beta, by a factor of 10(exp 2) - 10(exp 3) relative to inorganic crystals. A dehydration barrier of approx. 18kcal/mol may explain approx. 10(exp -6) times difference between frequencies of adding a molecule to the lattice and Brownian attempts to do so. The latter was obtained from AFM measurements of step and kink growth rates on orthorhombic lysozyme. Protein and many inorganic crystals typically do not belong to the Kossel type, thus requiring a theory to account for inequivalent molecular positions within its unit cell. Orthorhombic lysozyme will serve as an example of how to develop such a theory. Factors deteriorating crystal quality - stress and strain, mosaicity, molecular disorder - will be reviewed with emphasis on impurities. Dimers in ferritin and lysozyme and acetylated lysozyme, are microheterogeneous i.e. nearly isomorphic impurities that are shown to be preferentially trapped by tetragonal lysozyme and ferritin crystals, respectively. The distribution coefficient, K defined as a ratio of the (impurity/protein) ratios in crystal and in solution is a measure of trapping. For acetylated lysoyzme, K = 2.15 or, 3.42 for differently acetylated forms, is independent of both the impurity and the crystallizing protein concentration. The reason is that impurity flux to the surface is constant while the growth rate rises with supersaturation. About 3 times lower dimer concentration in space grown ferritin and lysozyme crystals might be examples explaining higher quality of the space grown protein crystal. Depletion of solution with respect to isomorphic impurities around a growing crystal may be K times deeper than with respect to the crystallizing protein.
Chernov, Alex A.↗
Atomic Force Microscope Observation of Growth and Defects on As-Grown (111) 3C-SiC Mesa Surfaces
This paper presents experimental atomic force microscope (AFM) observations of the surface morphology of as-grown (111) silicon-face 3C-SiC mesa heterofilms. Wide variations in 3C surface step structure are observed as a function of film growth conditions and film defect content. The vast majority of as-grown 3C-SiC surfaces consisted of trains of single bilayer height (0.25 nm) steps. Macrostep formation (i.e., step-bunching) was rarely observed, and then only on mesa heterofilms with extended crystal defects. As supersaturation is lowered by decreasing precursor concentration, terrace nucleation on the top (111) surface becomes suppressed, sometimes enabling the formation of thin 3C-SiC film surfaces completely free of steps. For thicker films, propagation of steps inward from mesa edges is sometimes observed, suggesting that enlarging 3C mesa sidewall facets begin to play an increasingly important role in film growth. The AFM observation of stacking faults (SF's) and 0.25 nm Burgers vector screw component growth spirals on the as-grown surface of defective 3C films is reported.
Neudeck, Philip G.↗
First steps in the oxidation of a /110/ nickel surface
Initial steps in oxidation of nickel surface studied using low energy back-reflection electron diffraction
NICKEL↗
Incompressible flow in stepped labyrinth seals
A steped labyrinth seal was experimentally investigated to determine the effects of pressure ratio, shaft speed, number of teeth, and tooth/step location upon the leakage through the seal for incompressible flow. The dependence of the flow coefficient upon the number of throttles and pressure ratio are similar to those for straight-through labyrinth seals. It can be noted that the axial location of the throttle with respect to the step had a special effect upon the flow coefficient. That is, the dependency of the flow coefficient upon rotation rate and the number of throttles changes with axial location. It was found that the minimum flow coefficient was obtained when the seal teeth were centered on the step surface. Axial pressure distribution measurements show that when the teeth are centered on the step, the pressure drop from cavity to cavity is almost uniform. It is speculated that the obtaining of this uniform pressure gradient is the cause for the enhanced performance of the stepped labyrinth seal when operated in that configuration.
Morrison, G. L.↗
Simulation studies for surfaces and materials strength
Three different investigations based on computer simulations were carried out. Simulation calculations were performed using model potentials with two- and three-body interactions which were represented by the Mie and the Axilrod-Teller potentials, respectively. In the first part, to analyze stability criteria for simple crystals, a parametrical investigation was performed and stability regions for five different crystalline structures were determined with respect to potential energy parameters. To simulate some of the basic surface processes such as diffusion and nucleation, in the second and third parts, silicon surfaces were considered as a specific example. In these studies diffusion of adatoms on stepped surfaces were simulated and energetics associated with the formation of kink sites were calculated.
Halicioglu, Timur↗
Step Bunching and Solution Flow
Imagine a sequence of equidistant steps parallel to one another on a crystal face growing from solution. Steps may be one or part of a lattice spacing high. With such ideal morphology, the most perfect material is expected to be produced. Sometimes this happens. Much more often, however, steps form bunches, acquire wavy shapes and interlace. With time, these spontaneous perturbations may be increased in amplitude, i.e. the stepped surface becomes morphologically unstable. Interferometric studies of Y.G. Kuznetsov, L.N. Rashkovich, P.G. Vekilov and N.A. Booth and the author demonstrated that the step bunching depends at least on direction and rate of solution flow over the interface, supersaturation and presence of impurities. In particular, if solution and step flow are parallel to one another, the steps convene into bunches. If these flows are antiparallel, the bunches disappear. As the step train propagates, the overall bunch height often increases infinitely. However, we have found recently that if the flow rate is large enough, (approximately 1 meter per second), the bunch height may be limited. All these phenomena come from interaction between steps. The interaction mechanisms are still not fully understood. I plan to overview major approaches to the still unresolved problem on how these dissipative structures on growing crystal face appear and evolve.
Chernov, A. A.↗
Enlargement of Step-Free SiC Surfaces by Homoepitaxial Web-Growth of Thin SiC Cantilevers
Lateral homoepitaxial growth of thin cantilevers emanating from mesa patterns that were reactive ion etched into on-axis commercial SiC substrates prior to growth is reported. The thin cantilevers form after pure stepflow growth removes almost all atomic steps from the top surface of a mesa, after which additional adatoms collected by the large step-free surface migrate to the mesa sidewall where they rapidly incorporate into the crystal near the top of the mesa sidewall. The lateral propagation of the step-free cantilevered surface is significantly affected by pregrowth mesa shape and orientation, with the highest lateral expansion rates observed at the inside concave comers of V-shaped pregrowth mesas with arms lengthwise oriented along the {1100} direction. Complete spanning of the interiors of V's and other mesa shapes with concave comers by webbed cantilevers was accomplished. Optical microscopy, synchrotron white beam x-ray topography and atomic force microscopy analysis of webbed regions formed over a micropipe and closed-core screw dislocations show that c-axis propagation of these defects is terminated by the webbing. Despite the nonoptimized process employed in this initial study, webbed surfaces as large as 1.4 x 10(exp -3) square centimeters, more than four times the pregrowth mesa area, were grown. However, the largest webbed surfaces were not completely free of bilayer steps, due to unintentional growth of 3C-SiC that occurred in the nonoptimized process. Further process optimization should enable larger step-free webs to be realized.
Neudeck, Philip G.↗