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All sourcesNASA NTRSDOE OSTI
NASA NTRS1966

Concave-convex growth spirals.

The simple model for introduction of a screw dislocation into a crystal leaves a step in those surfaces of the crystal that intersect the axis of the screw dislocation such that the Burgers vector has a finite component perpendicular to the surfaces. When two parallel surfaces of a crystal intersect the same screw dislocation, the resultant step, on opposite sides of the crystal, face in opposite directions. Consequently, when two such surfaces grow by accretion of the molecules at the steps, the steps wind themselves into spirals that appear to have opposite senses of rotation when viewed along the axis of the screw dislocation. Furthermore, the growth structure that results is a plano convex cone or pyramid centered on the screw dislocation. When growth occurs simultaneously on both sides of a crystal, a doubly convex structure will develop under the control of a singe screw dislocation.

Crystal growth↗
NASA NTRS1960

Factors Affecting the Ductility and Strength of NaCl Single Crystals Tested in Flexure

An experimental investigation has revealed that the initial deformation of NaCl single crystals is anelastic rather than Hookean. This anelastic deformation is manifested by a low slope foot in the load‐deflection curve. The magnitude of the foot is dictated by the pretreatment given the specimen. Treatments which increase or decrease the fresh dislocation density respectively increase or decrease the length of the initial anelastic foot. The order of increasing ductility and strength with specimen pretreatment was found to be (1) heated at 135 C, (2) as cleaved, (3) coated with silver, (4) heated at 135 C and then water polished, (5) water polished and then coated with silver, (6) water polished, (7) water polished and then heated at 135 C, (8) annealed at 700 C, and (9) annealed at 700 C and then water polished. The experimental results have been discussed in terms of the role played in deformation and fracture by surface cracks, grown‐in dislocations, and fresh dislocations.

Stearns, C. A.↗
NASA NTRS1999

Effects of Internal and External Hydrogen on Inconel 718

Internal hydrogen embrittlement (IHE) and hydrogen environment embrittlement (HEE) tensile and bend crack growth tests were performed on Inconel 718. For the IHE tests, the specimens were precharged to approximately 90 ppm hydrogen by exposure to 34.5 MPa H2 at 650 C. The HEE tests were performed in 34.5 MPa H2. Parameters evaluated were test temperature, strain rate for smooth and notch specimen geometries. The strain rate effect was very significant at ambient temperature for both IHE and HEE and decreased with increasing temperatures. For IHE, the strain rate effect was neglible at 260'C, and for HEE the strain rate effect was neglible at 400 C. At low temperatures, IHE was more severe than HEE, and at high temperatures HEE was more severe than IHE with a cross over temperature about 350 C. At 350 C, the equilibrium hydrogen concentration in Inconel 718 is about 50% lower than the hydrogen content of the precharged IHE specimens. Dislocation hydrogen sweeping of surface absorbed hydrogen was the likely transport mechanism for increasing the hydrogen concentration in the HEE tests sufficiently to produce the same degree of embrittlement as that of the more highly hydrogen charged IHE specimens. The main IHE fracture characteristic was formation of large, brittle flat facets, which decreased with increasing test temperature. The IHE fracture matrix surrounding the large facets ranged between brittle fine faceted to microvoid ductility depending upon strain rate, specimen geometry as well as temperature. The HEE fractures were characteristically fine featured, transgranular and brittle with a significant portion forming a "saw tooth" crystallographic pattern. Both IHE and HEE fractures were predominantly along the {1 1 1) slip and twin boundaries. With respect to embrittlement mechanism, it was postulated that dislocation hydrogen sweeping and hydrogen enhanced localized plasticity were active in HEE and IHE for concentrating hydrogen along (1 1 1) slip and twin planes. Final brittle failure occurred by hydrogen induced planer decohesion.

Walter, R. J.↗
NASA NTRS1990

Effect of dislocations on the open-circuit voltage, short-circuit current and efficiency of heteroepitaxial indium phosphide solar cells

Excellent radiation resistance of indium phosphide solar cells makes them a promising candidate for space power applications, but the present high cost of starting substrates may inhibit their large scale use. Thin film indium phosphide cells grown on Si or GaAs substrates have exhibited low efficiencies, because of the generation and propagation of large number of dislocations. Dislocation densities were calculated and its influence on the open circuit voltage, short circuit current, and efficiency of heteroepitaxial indium phosphide cells was studied using the PC-1D. Dislocations act as predominant recombination centers and are required to be controlled by proper transition layers and improved growth techniques. It is shown that heteroepitaxial grown cells could achieve efficiencies in excess of 18 percent AMO by controlling the number of dislocations. The effect of emitter thickness and surface recombination velocity on the cell performance parameters vs. dislocation density is also studied.

Jain, Raj K.↗
NASA NTRS1972

High-temperature creep of polycrystalline chromium.

Chromium prepared by the iodide process was consolidated into 100-g buttons by arc melting and fabricated to sheet by rolling. Test specimens machined from the wrought sheet were annealed in palladium-purified hydrogen, followed by a purification anneal, in order to produce stable grain structures for testing. Observations of surface slip lines and dislocation substructures suggest that a diffusion-controlled, dislocation-climb mechanism is operative in the creep of chromium over the temperature range investigated.

Stephens, J. R.↗
NASA NTRS1991

Identification of dislocation etch pits in n-type GaAs by NIR transmission microscopy

An optical method is described for identifying dislocation etch pits in n-type GaAS, using near-IR brightfield transmission microscopy. Dislocations are revealed in a nondestructive manner through contrasts that are likely due to impurity decoration of the dislocation lines. By subjecting the same wafers to a photoetching technique, it was established that each etch pit on the surface is associated with a dislocation and that the termination of each (decorated) dislocation is an etch pit.

Cao, X. Z.↗
NASA NTRS1999

Electrical Impact of SiC Structural Crystal Defects on High Electric Field Devices (Invited)

As illustrated by the invited paper at this conference and other works, SiC wafers and epilayers contain a variety of crystallographic imperfections, including micropipes, closed-core screw dislocations, grain boundaries, basal plane dislocations, heteropolytypic inclusions, and surfaces that are often damaged and contain atomically rough features like step bunching and growth pits or hillocks. Present understanding of the operational impact of various crystal imperfections on SiC electrical devices is reviewed, with an emphasis placed on high-field SiC power devices and circuits.

Neudeck, Philip G.↗
NASA NTRS1972

The effect of alloy composition on the mechanism of stress-corrosion cracking of titanium alloys in aqueous environments

A detailed study was made of the relation between the size distribution of Ti3Al particles in a Ti-8Al alloy and the tensile properties measured in air and in saltwater. The size distribution of Ti3Al was varied by isothermal aging for various times at temperatures in the range 770 to 970 K (930 to 1290 F). The aging kinetics were found to be relatively slow. Quantitative measurements of the particle coarsening rate at 920 K (1200 F) showed good agreement with the predicted behavior for coarsening controlled by matrix diffusion, and suggested that the specific free energy of the Ti3Al alpha interface in negligible small. In all cases, the Ti3Al particles were sheared by the glide dislocations. It was concluded that there is a definite correlation between the presence of deformable Ti3Al particles and an alloy's susceptibility to aqueous stress corrosion cracking. Furthermore, the appearance of the surface slip lines and the dislocation substructure in deformed specimens suggest that the specific effect of the Ti3Al particles is to cause a nonhomogeneous planar slip character and an enhanced chemical potential of the slip bands.

Wood, R. A.↗
NASA NTRS2004

Web Growth Used to Confine Screw Dislocations to Predetermined Lateral Positions in 4H-SiC Epilayers

Silicon-carbide- (SiC-) based power devices could enable substantial aerospace electronics benefits over today's silicon-based electronics. However, present-day SiC wafers contain electrically harmful dislocations (including micropipes) that are unpredictably distributed in high densities across all commercial 4H- and 6H-SiC wafers. The NASA Glenn Research Center recently demonstrated a crystal growth process that moves SiC wafer dislocations to predetermined lateral positions in epitaxial layers so that they can be reproducibly avoided during subsequent SiC electronic device fabrication. The process starts by reactive ion etching mesa patterns with enclosed trench regions into commercial on-axis (0001) 4H- or 6H-SiC substrates. An example of a pregrowth mesa geometry with six enclosed triangular-shaped trench regions is shown. After the etch mask is stripped, homoepitaxial growth is carried out in pure stepflow conditions that enable thin cantilevers to grow laterally from the tops of mesas whose pregrowth top surfaces are not threaded by substrate screw dislocations. The image in the bottom figure shows the postgrowth structure that forms after the lateral cantilevers expand to coalesce and completely roof over each of the six triangular trench regions. Atomic force microscope (AFM) measurements of the roof revealed that three elementary screw dislocation growth spirals, each shown in the AFM insets of the bottom image on the previous page, formed in the film roof at three respective points of cantilever film coalescence. The image above shows the structure following an etch in molten potassium hydroxide (KOH) that produced surface etch pits at the dislocation defects. The larger KOH etch pits--S1, S2, and S3--shown in this image correspond to screw dislocations relocated to the final points of cantilever coalescence. The smaller KOH etch pits are consistent with epilayer threading edge dislocations from the pregrowth substrate mesa (P1, P3, and P4) and a final cantilever coalescence point (P2). No defects (i.e., no etch pits) are observed in other cantilevered portions of the film surface. On the basis of the principle of dislocation Burgers vector conservation, we hypothesize that all vertically propagating substrate dislocations in an enclosed trench region become combined into a single dislocation in the webbed film roof at the point of final roof coalescence. The point of final roof coalescence, and therefore the lateral location of a webbed roof dislocation, can be designed into the pregrowth mesa pattern. Screw dislocations with predetermined lateral positions can then be used to provide the new growth steps necessary for growing a 4H/6H-SiC epilayer with a lower dislocation density than the substrate. Devices fabricated on top of such films can be positioned to avoid the preplaced dislocations.

Powell, J. Anthony↗
NASA NTRS1986

Dislocation mechanism based model for stage II fatigue crack propagation rate

Repeated plastic deformation, which of course depends on dislocation mechanism, at or near the crack tip leads to the fatigue crack propagation. By involving the theory of thermally activated flow and the cumulative plastic strain criterion, an effort is made here to model the stage II fatigue crack propagation rate in terms of the dislocation mechanism. The model, therefore, provides capability to ascertain: (1) the dislocation mechanism (and hence the near crack tip microstructures) assisting the crack growth, (2) the relative resistance of dislocation mechanisms to the crack growth, and (3) the fracture surface characteristics and its interpretation in terms of the dislocation mechanism. The local microstructure predicted for the room temperature crack growth in copper by this model is in good agreement with the experimental results taken from the literature. With regard to the relative stability of such dislocation mechanisms as the cross-slip and the dislocation intersection, the model suggests an enhancement of crack growth rate with an ease of cross-slip which in general promotes dislocation cell formation and is common in material which has high stacking fault energy (produces wavy slips). Cross-slip apparently enhances crack growth rate by promoting slip irreversibility and fracture surface brittleness to a greater degree.

Mazumdar, P. K.↗
NASA NTRS1971

Mechanism of underthrusting in southwest Japan: A model of convergent plate interactions

An elastic rebound mechanism consistent with underthrusting at the time of the magnitude 8.2 Nankaido earthquake of 21 December, 1946 accounts for a reversal in sense between seismic and preseismic changes in elevation throughout a large portion of southwest Japan. It is shown that the seismic movements during the earthquake were generated by slip on a complex thrust fault that is inferred to intersect the surface near the base of the continental slope. The preseismic deformation is explained by strain accumulation equivalent to a virtual dislocation with the same orientation as the fault surface but a sense opposite to that of the real dislocation that occurred at the time of the earthquake. Adjustments by slip along the fault surface and extensions of that surface can account for postseismic movements.

Fitch, T. J.↗
NASA NTRS1999

Carboxylic and dicarboxylic acids extracted from crushed magnesium oxide single crystals

Carboxylic and dicarboxylic acids (glycolic, oxalic, malonic and succinic) have been extracted with tetrahydrofuran (THF) and H2O from large synthetic MgO crystals, crushed to a medium fine powder. The extracts were characterized by infrared spectroscopy and 1H-NMR. The THF extracts were derivatized with tert-butyldimethylsilyl (t-BDMS) for GC-MS analysis. A single crystal separated from the extract was used for an x-ray structure analysis, giving the monoclinic unit cell, space group P21/c with ao = 5.543 A, bo = 8.845 A, co = 5.086 A, and beta = 91.9 degrees, consistent with beta-succinic acid, HOOC(CH2)COOH. The amount of extracted acids is estimated to be of the order of 0.1 to 0.5 mg g-1 MgO. The MgO crystals from which these organic acids were extracted grew from the 2860 degrees C hot melt, saturated with CO/CO2 and H2O, thereby incorporating small amounts of the gaseous components to form a solid solution (ss) with MgO. Upon cooling, the ss becomes supersaturated, causing solute carbon and other solute species to segregate not only to the surface but also internally, to dislocations and subgrain boundaries. The organic acids extracted from the MgO crystals after crushing appear to derive from these segregated solutes that formed C-C, C-H and C-O bonds along dislocations and other defects in the MgO structure, leading to entities that can generically be described as (HxCyOz)n-. The processes underlying the formation of these precursors are fundamental in nature and expected to be operational in any minerals, preferentially those with dense structures, that crystallized in H2O-CO2-laden environments. This opens the possibility that common magmatic and metamorphic rocks when weathering at the surface of a tectonically active planet like Earth may be an important source of abiogenically formed complex organic compounds.

NASA Discipline Exobiology↗
NASA NTRS1998

Carboxylic and Dicarboxylic Acids Extracted from Crushed Magnesium Oxide Single Crystals

Carboxylic and dicarboxylic acids (glycolic, oxalic, malonic and succinic) have been extracted with tetrahydrofuran (THE) and H2O from large synthetic MgO crystals, crushed to a medium fine powder. The extracts were characterized by infrared spectroscopy and (sup 1)H-NMR (Nuclear Magnetic Resonance). The THF extracts were derivatized with tert-butyldimethylsilyl (t-BDMS) for GC-MS (Gas Chromatography - Mass Spectroscopy) analysis. A single crystal separated from the extract was used for an x-ray structure analysis, giving the monoclinic unit cell, space group P2(sub 1)/c with a(sub o) = 5.543 A, b(sub o) = 8.845 A, c(sub o) = 5.086 A, and beta = 91.9 degrees, consistent with beta-succinic acid, HOOC(CH2)COOH. The amount of extracted acids is estimated to be of the order of 0.1 to 0.5 mg/g MgO. The MgO crystals from which these organic acids were extracted grew from the 2360 C hot melt, saturated with CO/CO2 and H2O, thereby incorporating small amounts of the gaseous components to form a solid solution (ss) with MgO. Upon cooling, the ss becomes supersaturated, causing solute carbon and other solute species to segregate not only to the surface but also internally, to dislocations and subgrain boundaries. The organic acids extracted from the MgO crystals after crushing appear to derive from these segregated solutes that formed C-C, C-H, and C-O bonds along dislocations and other defects in the MgO structure, leading to entities that can generically be described as (HxCyOz)(sup n-). The processes underlying the formation of these precursors are fundamental in nature and expected to be operational in any minerals, preferentially those with dense structures, that crystallized in H2O-CO2-laden environments. This opens the possibility that common magmatic and metamorphic rocks when weathering at the surface of a tectonically active planet like Earth may be an important source of abiogenically formed complex organic compounds.

Freund, Friedemann↗
NASA NTRS2005

Silicon Carbide Growth

Andrew Trunek has focused on supporting the Sic team through the growth of Sic crystals, making observations and conducting research that meets the collective needs and requirements of the team while fulfilling program commitments. Cancellation of the Ultra Efficient Engine Technology (UEET) program has had a significant negative impact on resources and research goals. This report highlights advancements and achievements made with this cooperative agreement over the past year. NASA Glenn Research Center (GRC) continues to make advances in silicon carbide (SiC) research during the past year. Step free surfaces were used as substrates for the deposition of GaN epilayers that yielded very low dislocation densities. Defect free 3C- SiC was successfully nucleated on step free mesas and test diodes were fabricated. Web growth techniques were used to increase the usable surface area of dislocation free SiC by approximately equal to 40%. The greatest advancement has been attained on stepped surfaces of SiC. A metrology standard was developed using high temperature etching techniques titled "Nanometer Step Height Standard". This development culminated in being recognized for a 2004 R&D100 award and the process to produce the steps received a NASA Space Act award.

Source record↗
NASA NTRS2005

Geometry of Thrust Faults Beneath Amenthes Rupes, Mars

Amenthes Rupes is a 380 km-long lobate fault scarp located in the eastern hemisphere of Mars near the dichotomy boundary. The scarp is marked by about 1 km of vertical separation across a northeast dipping thrust fault (top to the SW) and offsets heavily-cratered terrain of Late Noachian age, the visible portion of which was in place by 3.92 Ga and the buried portion in place between 4.08 and 4.27 Ga. The timing of scarp formation is difficult to closely constrain. Previous geologic mapping shows that near the northern end of Amenthes Rupes, Hesperian age basalts terminate at the scarp, suggesting that fault slip predated the emplacement of these flows at 3.69 to 3.9 Ga. Maxwell and McGill also suggest the faulting ceased before the final emplacement of the Late Hesperian lavas on Isidis Planitia. The trend of the faults at Amenthes, like many thrust faults at the dichotomy boundary, parallels the boundary itself. Schultz and Watters used a dislocation modeling program to match surface topography and vertical offset of the scarp at Amenthes Rupes, varying the dip and depth of faulting, assuming a slip of 1.5 km on the fault. They modeled faulting below Amenthes Rupes as having a dip of between 25 and 30 degrees and a depth of 25 to 35 km, based on the best match to topography. Assuming a 25 degree dip and surface measurements of vertical offset of between 0.3 and 1.2 km, Watters later estimated the maximum displacement on the Amenthes Rupes fault to be 2.90 km. However, these studies did not determine the geometry of the thrust using quantitative constraints that included shortening estimates. Amenthes Rupes deforms large preexisting impact craters. We use these craters to constrain shortening across the scarp and combine this with vertical separation to infer fault geometry. Fault dip was also estimated using measurements of scarp morphology. Measurements were based on 460 m (1/128 per pixel) digital elevation data from the Mars Orbiter Laser Altimeter (MOLA), an instrument on the Mars Global Surveyor (MGS) satellite.

Vidal, A.↗
NASA NTRS1998

Determining the Molecular Growth Mechanisms of Tetragonal Lysozyme Crystals

Studies of the growth of tetragonal lysozyme crystals employing atomic force microscopy (AFM) have shown the advantages of this technique in investigating the growth mechanisms of protein crystals [1]. The resolution of these studies was in the micron range, which revealed surface features such as the occurrence of dislocations and 2D nucleation islands, similar to those found in inorganic systems. They clearly showed that the crystals grew by these surface growth mechanisms. However, the studies also revealed some surprising features, such as bimolecular growth step heights and pronounced growth anisotropies on the (110) face, which could not be explained. In previous studies we employed Periodic Bond Chain (PBC) theory to tetragonal lysozyme crystal growth and found that the crystals were constructed by strongly bonded molecular chains forming helices about the 43 axes [2,3]. The helices were connected to each other with weaker bonds. The growth process was shown to proceed by the formation of these 43 helices, resulting in bimolecular growth steps on the (110) face. It was also shown to explain many other observations on tetragonal lysozyme crystal growth. Although PBC analysis is not a new technique [4], it has not been widely used as the mechanisms predicted from it could not be experimentally verified. In this study the growth process of these crystals was investigated, particularly for the (110) face, employing some newly developed high resolution AFM techniques. These techniques allowed individual lysozyme molecules on the crystal faces to be resolved and predictions from PBC analyses to be tested. The analyses had shown that of the two possible packing arrangements on (110) faces, only one would actually occur. Employing the first of the newly developed techniques, these faces were scanned by high resolution AFM. The resulting images were then compared with the theoretically constructed images for the two possible packing arrangements on the (110) face. The theoretical images were constructed by convolution of the crystal surface shape obtained from crystallographic data with the AFM tip shape. The comparison confirmed the prediction that the molecular packing arrangement of these faces corresponded to that for complete 43 helices. The second AFM technique that was developed was used to follow the growth process by measuring the dimensions of individual growth units on the (110) face. Linescans across a growth step, performed near the saturation limit of the crystals, allowed the growth unit dimensions to be measured. These measurements showed that growth on the (110) face proceeded by the formation of new 43 helices from the addition of at least tetramer units in the [110] direction. In the [001] direction growth proceeded by the addition of various aggregate units corresponding to the 4(sub 3) helices.

Li, Huayu↗
NASA NTRS1991

Crystal regularity with high-resolution synchrotron X-radiation diffraction imaging

New, high-resolution sources of X-radiation such as monochromatic synchrotron radiation beams with subarcsec divergence allow observation of regularities in a range of crystals with sufficient clarity for comprehensive analyses, whose results can deepen understanding of the nature of various crystal irregularities, their sources, and their effects on device performance. An account is presented of the results thus achievable with irregularities encountered in lattice orientation and strain, grain and subgrain boundaries, dislocations, domain boundaries, additional phases, and surface scratches. Significant achievements to date encompass the observation of critical anomalies in lead tin telluride, the reconciliation of disparate observations of GaAs, the determination of the performance effects of irregularities in mercuric iodide, and the characterization of the origins of crystal growth in bismuth silicon oxide.

Steiner, Bruce↗
NASA NTRS1984

Orientation and Morphology Effects in Rapid Silicon Sheet Solidification

Radial growth anisotropies and equilibrium forms of point nucleated, dislocation free silicon sheets spreading horizontally on the free surface of a silicon melt were measured for (100), (110), (111), and (112) sheet planes. The growth process was recorded. Qualitative Wulff surface free energy polar plots were deduced from the equilibrium shapes for each sheet plane. Predicted geometries for the tip shape of unidirectional, dislocation free, horizontally grown sheets growing in various directions within the planes were analyzed. Polycrystalline sheets and dendrite propagation were analyzed. For dendrites, growth rates on the order of 2.5 m/min and growth rate anisotropies of 25 are measured.

Ciszek, T. F.↗