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At least 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
NASA NTRS2014

Structural Characterization of Lateral-grown 6H-SiC am-plane Seed Crystals by Hot Wall CVD Epitaxy

The performance of commercially available silicon carbide (SiC) power devices is limited due to inherently high density of screw dislocations (SD), which are necessary for maintaining polytype during boule growth and commercially viable growth rates. The NASA Glenn Research Center (GRC) has recently proposed a new bulk growth process based on axial fiber growth (parallel to the c-axis) followed by lateral expansion (perpendicular to the c-axis) for producing multi-faceted m-plane SiC boules that can potentially produce wafers with as few as one SD per wafer. In order to implement this novel growth technique, the lateral homoepitaxial growth expansion of a SiC fiber without introducing a significant number of additional defects is critical. Lateral expansion is being investigated by hot wall chemical vapor deposition (HWCVD) growth of 6H-SiC am-plane seed crystals (0.8mm x 0.5mm x 15mm) designed to replicate axially grown SiC single crystal fibers. The post-growth crystals exhibit hexagonal morphology with approximately 1500 m (1.5 mm) of total lateral expansion. Preliminary analysis by synchrotron white beam x-ray topography (SWBXT) confirms that the growth was homoepitaxial, matching the polytype of the respective underlying region of the seed crystal. Axial and transverse sections from the as grown crystal samples were characterized in detail by a combination of SWBXT, transmission electron microscopy (TEM) and Raman spectroscopy to map defect types and distribution. X-ray diffraction analysis indicates the seed crystal contained stacking disorders and this appears to have been reproduced in the lateral growth sections. Analysis of the relative intensity for folded transverse acoustic (FTA) and optical (FTO) modes on the Raman spectra indicate the existence of stacking faults. Further, the density of stacking faults is higher in the seed than in the grown crystal. Bundles of dislocations are observed propagating from the seed in m-axis lateral directions. Contrast extinction analysis of these dislocation lines reveals they are edge type basal plane dislocations that track the growth direction. Polytype phase transition and stacking faults were observed by high-resolution TEM (HRTEM), in agreement with SWBXT and Raman scattering.

Single Crystal↗
NASA NTRS1980

Dislocation dissociation in some f.c.c. metals

The dissociation of a perfect screw dislocation into a stacking fault in an f.c.c. lattice is modeled by the modified lattice statics. The interatomic potentials are obtained from the work of Esterling and Swaroop and differ substantially from those empirical potentials usually employed in defect simulations. The calculated stacking fault widths for aluminum, copper, and silver are in good agreement with weak beam microscopy results.

Esterling, D. M.↗
NASA NTRS1998

Ground Based Program for the Physical Analysis of Macromolecular Crystal Growth

During the past year we have focused on application of in situ Atomic Force Microscopy (AFM) for studies of the growth mechanisms and kinetics of crystallization for different macromolecular systems. Mechanisms of macrostep formation and their decay, which are important in understanding of defect formation, were studied on the surfaces of thaumatin, catalase, canavalin and lysozyme crystals. Experiments revealed that step bunching on crystalline surfaces occurred either due to two- or three-dimensional nucleation on the terraces of vicinal slopes or as a result of uneven step generation by complex dislocation sources. No step bunching arising from interaction of individual steps in the course of the experiment was observed. The molecular structure of the growth steps for thaumatin and lipase crystals were deduced. It was further shown that growth step advance occurs by incorporation of single protein molecules. In singular directions growth steps move by one-dimensional nucleation on step edges followed by lateral growth. One-dimensional nuclei have different sizes, less then a single unit cell, varying for different directions of step movement. There is no roughness due to thermal fluctuations, and each protein molecule which incorporated into the step remained. Growth kinetics for catalase crystals was investigated over wide supersaturation ranges. Strong directional kinetic anisotropy in the tangential step growth rates in different directions was seen. The influence of impurities on growth kinetics and cessation of macromolecular crystals was studied. Thus, for catalase, in addition to pronounced impurity effects on the kinetics of crystallization, we were also able to directly observe adsorption of some impurities. At low supersaturation we repeatedly observed filaments which formed from impurity molecules sedimenting on the surfaces. Similar filaments were observed on the surfaces of thaumatin, canavalin and STMV crystals as well, but the frequency was low compared with catalase crystallization. Cessation of growth of xylanase and lysozyme crystals was also observed and appeared to be a consequence of the formation of dense impurity adsorption layers. Attachment: "An in situ AFM investigation of catalase crystallization", "Atomic force microscopy studies of living cells: visualization of motility, division, aggregation, transformation, and apoptosis", AFM studies on mechanisms of nucleation and growth of macromolecular crystals", and "In situ atomic force microscopy studies of surface morphology, growth kinetics, defect structure and dissolution in macromolecular crystallization".

Malkin, Alexander J.↗
NASA NTRS1995

Temperature Dependent Cyclic Deformation Mechanisms in Haynes 188 Superalloy

The cyclic deformation behavior of a wrought cobalt-base superalloy, Haynes 188, has been investigated over a range of temperatures between 25 and 1000 C under isothermal and in-phase thermomechanical fatigue (TMF) conditions. Constant mechanical strain rates (epsilon-dot) of 10(exp -3)/s and 10(exp -4)/s were examined with a fully reversed strain range of 0.8%. Particular attention was given to the effects of dynamic strain aging (DSA) on the stress-strain response and low cycle fatigue life. A correlation between cyclic deformation behavior and microstructural substructure was made through detailed transmission electron microscopy. Although DSA was found to occur over a wide temperature range between approximately 300 and 750 C the microstructural characteristics and the deformation mechanisms responsible for DSA varied considerably and were dependent upon temperature. In general, the operation of DSA processes led to a maximum of the cyclic stress amplitude at 650 C and was accompanied by pronounced planar slip, relatively high dislocation density, and the generation of stacking faults. DSA was evidenced through a combination of phenomena, including serrated yielding, an inverse dependence of the maximum cyclic hardening with epsilon-dot, and an instantaneous inverse epsilon-dot sensitivity verified by specialized epsilon-dot -change tests. The TMF cyclic hardening behavior of the alloy appeared to be dictated by the substructural changes occuring at the maximum temperature in the TMF cycle.

Rao, K. Bhanu Sankara↗
NASA NTRS1973

Correlation of creep rate with microstructural changes during high temperature creep

The techniques of electron microscopy were used to examine the microstructural changes which occur during primary creep for two important types of engineering alloys: (1) alloys strengthened by solid-solution additions, and (2) dispersion-strengthened alloys. The metals chosen for study are unalloyed titanium, Ti-6Al-4V, and the cobalt-base alloy, Haynes 188. Results to date on NGR 47-004-108 show that development of prior dislocation substructure in Haynes 188 by 10% prestrain and annealing for one hour at 1800 F increases the time to reach 0.5% creep strain at 1600 F by more than an order of magnitude for creep stresses from 3 to 20 ksi. For creep at 1800 F, similar results were obtaind for stresses above 7 ksi, but the prior substructure decreases creep resistance below 7 ksi. This effect appears to be related to instability of grain structure at 1800 F in prestrained material.

Young, C. T.↗
NASA NTRS1981

Experiment K-314: Fetal and neonatal rat bone and joint development following in Utero spaceflight

Infant rat limb specimens from Soviet and U.S. ground-based studies were examined by radiography, macrophotography, histologic sectioning and staining and scanning electron microscopy. A comparison was conducted between vivarium and flight-type diets suggesting that nutritional obesity may adversely affect pregnancy. Data were obtained on maturation of ossification centers, orientation of collagen fibers in bone, tendon and ligaments, joint surface texture and spatial relationships of bones of the hind limb. Computer reconstructions of the knee and hip show promise as a means of investigating the etiology of congenital hip dislocation.

Sabelman, E. E.↗
NASA NTRS1975

Structure-property relationships in thermomechanically treated beryllia dispersed nickel alloys

BeO dispersed nickel alloys, produced by powder metallurgy techniques, were studied extensively in stress rupture at 815, 982, and 1093 C (1088, 1255, and 1366 K) and by transmission electron microscopy. The alloys were subjected to a variety of thermomechanical treatments (TMT) to determine the benefits of TMT on properties. It is shown that the use of intermediate annealing treatments after 10 pct reduction steps is highly beneficial on both low and high temperature properties. It is indicated that the high temperature strength is not primarily dependent on the grain aspect ratio or texture but depends strongly on the dislocation density and distribution of dislocations in a stable substructure which is pinned by the fine oxide dispersion.

Grewal, M. S.↗
NASA NTRS1988

Studies of molecular-beam epitaxy growth of GaAs on porous Si substrates

GaAs has been grown on porous Si directly and on Si buffer layer-porous Si substrates by molecular-beam epitaxy. In the case of GaAs growth on porous Si, transmission electron microscopy (TEM) reveals that the dominant defects in GaAs layers grown on porous Si are microtwins and stacking faults, which originate from the GaAs/porous Si interface. GaAs is found to penetrate into the porous Si layers. By using a thin Si buffer layer (50 nm), GaAs penetration diminishes and the density of microtwins and stacking faults is largely reduced and localized at the GaAs/Si buffer interface. However, there is a high density of threading dislocations remaining. Both Si (100) aligned and four degree tilted substrates have been examined in this study. TEM results show no observable effect of the tilted substrates on the quality of the GaAs epitaxial layer.

Mii, Y. J.↗
NASA NTRS1982

Pre- and post-annealing of mechanical damage in silicon wafers

Basic properties of mechanical damage in silicon consisting of cracks and abrasion were studied using transmission electron microscopy. The crystallographic structure of mechanical damage was determined before and after high temperature annealing. The main findings include that stresses in silicon around crack tips are not plastically relieved at room temperature and that abrasion at room temperature introduces shear loops into the silicon. It was also found that cracks of micron size can be annealed out, specifically, if cleavage occurs on 111 planes. The healing products of such cracks are 60 deg and 90 deg dislocations. Submicron cracks transform into stacking faults during annealing. Likewise high concentrations of shear loops due abrasion were found to anneal into stacking faults. A one to one correlation between surface areas containing small cracks and stacking faults was made. Measurements of damage removal on silicon surfaces through chemical-mechanical etching techniques are presented. It is shown that silicon dioxide repolishes damaged silicon surfaces most effectively.

Schwottke, G. H.↗
NASA NTRS1998

Experiment 1: Orbital Processing of High-Quality Zn-Alloyed CdTe Compound Semiconductors

Zinc-alloyed cadmium telluride (Zn:CdTe) crystals were grown in unit gravity and in microgravity for comparative analysis. Two crystals were grown on USML-1/STS-50 in 1992, and two additional crystals were grown on USML-2/STS-73 in 1995. The Crystal Growth Furnace (CGF) in the seeded Bridgman-Stockbarger crystal growth geometry was utilized on both missions. Crystals grown on USML-1/STS-50 were found to have solidified with partial wall contact due to the near-absence of the hydrostatic pressure in microgravity, a residual g-vector that was not axial, and the nonwetting sample/ampoule wetting conditions. Crystals grown on USML-2/STS-73 included: a sample/ampoule identical to the USML-1/STS-73 sample/ampoule, with the addition of a restraining spring to simulate hydrostatic pressure internally, and a tapered ampoule which accomplished 2.2 cm of crystal growth without wall contact. Infrared transmission of all ground and flight samples was found to be 63-66 percent, very close to the theoretical 66 percent, suggesting good stoichiometric control. Infrared microscopy confirmed that the primary precipitates were Te and their size (1-10 microns) and density suggested that the flight- and ground-base samples experienced similar thermal histories. Longitudinal macrosegregation, calculated using scaling analysis, was predicted to be low. Nearly diffusion controlled growth was achieved even in unit gravity and macrosegregation data could be fit with a diffusion controlled model. Radial segregation was monitored and was found to vary with fraction solidified, particularly through the shoulder region, where the sample cross section was varying significantly. It was also disturbed in the flight samples in regions where asymmetric wall contact was noted. In regions where a steady state was established, the radial segregation was invariant within our experimental measurement error. Flight samples were found to be much higher in structural perfection than samples processed in unit gravity under identical growth conditions. In regions where solidification had occurred without wall contact, the free surfaces evidenced virtually no twinning, although twins appeared in the flight samples in regions of wall contact and were pervasive in the ground samples. These results were confirmed using optical microscopy and synchrotron x-ray white beam topography. Full-width half-maximum rocking curve widths (FWHM), recorded in arc-seconds, were significantly reduced from 20 a-s (1 g) to 9 a-s (micro-g) for the best regions of the crystals. The 9 a-s (FWHM) rocking curve value in the unconfined flight samples equals the best value reported terrestrially for this material. The ground samples exhibited a fully developed (111)[110] dislocation mosaic structure, whereas dislocations within the flight samples were discrete and no mosaic structure was evident. The defect density was quantitatively reduced from 75,000 (1 g) to 800 (micro-g) +/-50 percent. Dislocation etch pit density results were confirmed using transmission synchrotron white beam and monochromated beam topography. The low defect density is thought to have resulted from the near absence of hydrostatic pressure, which allowed the molten boule to solidify with little or no wall contact. This minimized the transfer of hoop stresses during solidification and post-solidification processing.

Larson, D. J., Jr.↗
NASA NTRS1976

Oxidation of metals and alloys in controlled atmospheres using in situ transmission electron microscopy and Auger spectrography

Single-crystalline thin films of copper were oxidized at an isothermal temperature of 425 C and at an oxygen partial pressure of .005 Torr in situ in a high-resolution electron microscope. The specimens were prepared by epitaxial vapor deposition onto polished 100 and 110 faces of rocksalt and mounted in a hot stage inside an ultra-high-vacuum specimen chamber of the microscope. Large amounts of sulfur, carbon, and oxygen were detected by Auger electron spectroscopy on the surface of the as-received films and were removed in situ by ion-sputter etching immediately prior to the oxidation. The nucleation and growth characteristics of Cu2O on Cu were studied. Results show that neither stacking faults nor dislocations are associated with the Cu2O nucleation sites. The growth of Cu2O nuclei is linear with time. The experimental findings, including results from oxygen dissolution experiments and from repetitive oxidation-reduction-oxidation sequences, fit well into the framework of an oxidation process involving (a) the formation of a surface-charge layer, (b) oxygen saturation in the metal and (c) nucleation, followed by surface diffusion of oxygen and bulk diffusion of copper for lateral and vertical oxide growth, respectively.

Rao, D. B.↗
NASA NTRS1986

Effect of multiple strain-anneal cycles on the 1000 C creep behaviour of gamma/gamma prime-alpha

Various multiple strain-anneal cycles (1000 C) were imposed on specimens of the directionally solidified eutectic (DSE) alloy gamma/gamma prime-alpha to identify thermomechanical processing methods (TMP) which would improve the creep behavior. Specimens of the Ni-32.3Mo-6.3Al wt pct alloy were grown with a modified Bridgeman technique. Some of the cylindrical specimens were alternately heat-treated at 900 C, then strained, or heat-treated only, while other specimens were annealed at 900 C after swaging and then worked at ambient temperature. The specimens were all examined microstructurally using transmission electron microscopy, some before and after being exposed to constant-load compression tests at 1000 C. The creep strain increased for all TMP specimens for strain rates of at least 2 millionths per sec. Strain rates of about 2 ten millionths per sec were only improved with strain annealing with 13 percent work at ambient temperature. A slight improvement, compared to as-grown materials, was observed in the 1000 C creep behavior of materials annealed at 900 C. Strain-annealing was found to introduce three-dimensional dislocation networks into the gamma-prime matrix.

Whittenberger, J. D.↗
NASA NTRS1981

EBIC/TEM investigations of defects in solar silicon ribbon materials

Transmission electron microscopy was used to investigate the defect structure of edge defined film growth (EFG) material, web dentritic ribbons (WEB), and ribbon to ribbon recrystallized material (RTR). The most common defects in all these materials are coherent first order twin boundaries. These coherent twins can be very thin, a few atomic layers. Bundles of the twins which contain odd numbers of twins will in optical images appear as a seemingly single first twin boundary. First-order coherent twin boundaries are not electrically active, except at locations where they contain intrinsic (grain boundary) dislocations. These dislocations take up small deviations from the ideal twin relation and play the same role in twin boundaries as conventional and play the some role in twin boundaries as conventional edge and screw dislocations in small angle tilt and twist boundaries.

Ast, D. G.↗
NASA NTRS1998

Microstructural Characterization of Aluminum-Lithium Alloys 1460 and 2195

Transmission electron microscopy (TEM) and differential scanning calorimetry (DSC) techniques were employed to characterize the precipitate distributions in lithium-containing aluminum alloys 1460 and 2195 in the T8 condition. TEM examinations revealed delta prime and T1 as the primary strengthening precipitates in alloys 1460 and 2195 respectively. TEM results showed a close similarity of the Russian alloy 1460 to the U.S. alloy 2090, which has a similar composition and heat treatment schedule. DSC analyses also indicate a comparable delta prime volume fraction. TEM study of a fractured tensile sample of alloy 1460 showed that delta prime precipitates are sheared by dislocations during plastic deformation and that intense stress fields arise at grain boundaries due to planar slip. Differences in fracture toughness of alloys 1460 and 2195 are rationalized on the basis of a literature review and observations from the present study.

Wang, Z. M.↗
NASA NTRS1992

Optical and TEM study of shock metamorphism from the Sedan test site

Thus far, detailed petrologic studies of shock metamorphism have been performed on samples recovered from laboratory experiments and on a few natural impactites. The loading history of these samples is quite different: In particular, laboratory experiments spend only a short time (less than 1 microsec) at peak pressure, whereas natural impactites may have stress pulses from 0.1 - 1 ms. On the other hand, laboratory experiments have known stress histories; natural impactites do not. Natural samples are also subjected to thousands or millions of years of postshock annealing and/or weathering. A useful intermediate case is that of nuclear detonation. Stress pulses for these events can reach 0.1 ms or higher, and samples are obtained in pristine condition. All three types of loading produce stresses of hundreds of kilobars. Samples studied were taken from the Sedan nulcear test site, and consist of a coarse-grained granodiorite containing quartz, K-feldspar, cordierite, and hornblende. Samples were studied optically in this section, then were thinned with an ion mill and studied by transmission electron microscopy (TEM). Optically, quartz and K-feldspar displayed numerous sets of planar deformation features (PDF's) identical to the nondecorated PDF's seen in laboratory samples and many natural impactites. TEM study showed that the PDF's in quartz and feldspar corresponded to densely packed wide transformation lamellae identical to those described in laboratory studies. The transformation lamellae in both minerals were amorphous, with no sign of high-pressure phases. In the case of K-feldspar only, narrow sublamellae extended outward from some wide lamellae. Quartz, which was more abundant and studied more extensively, contained no shock-induced dislocations. Some planar features were also seen in cordierite, but could not be identified due to rapid beam damage. No shock defects were seen in hornblende in TEM. The shock-induced defects present at the Sedan site are very similar to those seen in shock recovery experiments, and also to those present at certain natural events (e.g., Meteor Crater). This suggests that shock deformation in quartz is not strongly dependent on shock pulse duration, and that laboratory recovery experiments are useful simulations of natural impact events.

Gratz, A. J.↗
NASA NTRS1994

Nucleation, growth, and strain relaxation of lattice-mismatched 3-5 semiconductor epitaxial layers

We have investigated the early stages of evolution of highly strained 2-D InAs layers and 3-D InAs islands grown by metal-organic chemical vapor deposition (MOCVD) on (100) and (111)B GaAs substrates. The InAs epilayer/GaAs substrate combination has been chosen because the lattice-mismatch is severe (approximately 7.2 percent), yet these materials are otherwise very similar. By examining InAs-on-GaAs composites instead of the more common In(x)Ga(1-x)As alloy we remove an additional degree of freedom (x) and thereby simplify data interpretation. A matrix of experiments is described in which the MOCVD growth parameters - susceptor temperature, Thin flux, and AsH3 flux - have been varied over a wide range. Scanning electron microscopy, atomic force microscopy, transmission electron microscopy, and electron microprobe analysis have been employed to observe the thin film surface morphology. In the case of 3-D growth, we have extracted activation energies and power-dependent exponents that characterize the nucleation process. As a consequence, optimized growth conditions have been identified for depositing approximately 250 A thick (100) and (111)B oriented InAs layers with relatively smooth surfaces. Together with preliminary data on the strain relaxation of these layers, the above results on the evolution of thin InAs films indicate that the (111)B orientation is particularly promising for yielding lattice-mismatched films that are fully relaxed with only misfit dislocations at the epilayer/substrate interface.

Welser, R. E.↗
NASA NTRS1994

Nucleation, Growth, and Strain Relaxation of Lattice-Mismatched III-V Semiconductor Epitaxial Layers

We have investigated the early stages of evolution of highly strained 2-D InAs layers and 3-D InAs islands grown by metal-organic chemical vapor deposition (MOCVD) on (100) and (111) B GaAs substrates. The InAs epilayer / GaAs substrate combination has been chosen because the lattice-mismatch is severe (approx. 7.20%), yet these materials are otherwise very similar. By examining InAs-on-GaAs composites Instead of the more common In(x)Ga(1-x)As alloy, we remove an additional degree of freedom (x) and thereby simplify data interpretation. A matrix of experiments is described in which the MOCVD growth parameters -- susceptor temperature, TMIn flux, and AsH3 flux -- have been varied over a wide range. Scanning electron microscopy, atomic force microscopy, transmission electron microscopy, and electron microprobe analysis have been employed to observe the thin film surface morphology. In the case of 3-D growth, we have extracted activation energies and power-dependent exponents that characterize the nucleation process. As a consequence, optimized growth conditions have been identified for depositing approx. 250 A thick (100) and (111)B oriented InAs layers with relatively smooth surfaces. Together with preliminary data on the strain relaxation of these layers, the above results on the evolution of thin InAs films indicate that the (111)B orientation is particularly promising for yielding lattice-mismatched films that are fully relaxed with only misfit dislocations at the epilayer / substrate interface.

Welser, R. E.↗
NASA NTRS1982

Fatigue and creep-fatigue deformation of several nickel-base superalloys at 650 C

Transmission electron microscopy has been used to study the bulk deformation characteristics of seven nickel-base superalloys tested in fatigue and creep-fatigue at 650 C. The alloys were Waspalloy, HIP Astroloy, H plus F Astroloy, H plus F Rene 95, IN 100, MERL 76, and NASA IIB-7. The amount of bulk deformation observed in all the alloys was low. In tests with inelastic strain amplitudes less than about 0.003, only some grains exhibited yielding and the majority of those had the 110 line near the tensile axis. Deformation occurred on octahedral systems for all of the alloys except MERL 76 which also showed abundant primary cube slip. Creep-fatigue cycling occasionally produced extended faults between partial dislocations, but otherwise deformation was much the same as for fatigue cycling.

Miner, R. V.↗