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At least 271 records · Page 15

High temperature creep behavior of single crystal gamma prime and gamma alloys

The creep behavior of single crystals of gamma-prime and gamma alloys were investigated and compared to the response of two-phase superalloys tested previously. High temperature deformation in the gamma alloys was characteristic of a climb-controlled mechanism, whereas the gamma-prime based materials exhibited glide-controlled creep behavior. The superalloys were much more creep resistant than their constituent phases, which indicates the importance of the gamma/gamma-prime interface as a barrier for dislocation motion during creep.

Nathal, M. V.↗

Orientation and temperature dependence of some mechanical properties of the single-crystal nickel-base superalloy Rene N4. I - Tensile behavior

Single crystal specimens of a nickel-base superalloy with axes near 001, 011, and -112 were tested in tension at room temperature, 760, and 980 C. The alloy Rene N-4, was developed for gas turbine engine blades and has the nominal composition 3.7 Al, 4.2 Ti, 4 Ta, 0.5 Nb, 6 W, 1.5 Mo, 9 Cr, 7.5 Co, balance Ni, (all in weight percent). Analysis of slip band traces, specimen axis rotation, and dislocation Burgers vectors showed that at 760 and 980 C primary cube slip supplanted normal octahedral slip for the -112 line-oriented specimens. The other two orientations, which have lower resolved shear stresses on the cube system, exhibited octahedral slip at all three temperatures. The critical resolved shear stress is considerably greater on the cube system than on the octahedral system at room temperature. However, at 760 and 980 C the critical resolved shear stresses on the two systems are about the same. While the room temperature and 980 C yield strengths for the two orientations exhibiting octahedral slip could be rationalized on the basis of resolved shear stress, those at 760 C could not. Such violations of Schmid's law have previously been observed in other superalloys and single phase gamma-prime.

Miner, R. V.↗

Web-dendritic ribbon growth

A web furnace was constructed for pulling dendritic-web samples. The effect of changes in the furnace thermal geometry on the growth of dendritic-web was studied. Several attempts were made to grow primitive dendrites for use as the dendritic seed crystals for web growth and to determine the optimum twin spacing in the dendritic seed crystal for web growth. Mathematical models and computer programs were used to determine the thermal geometries in the susceptor, crucible melt, meniscus, and web. Several geometries were determined for particular furnace geometries and growth conditions. The information obtained was used in conjunction with results from the experimental growth investigations in order to achieve proper conditions for sustained pulling of two dendrite web ribbons. In addition, the facilities for obtaining the following data were constructed: twin spacing, dislocation density, web geometry, resistivity, majority charge carrier type, and minority carrier lifetime.

Hilborn, R. B., Jr.↗

Temperature dependence of hardness in yttria-stabilized zirconia single crystals

The temperature dependence of hardness and microcracking in single-crystal 9.5-mol pct-Y2O3-fully-stabilized cubic-ZrO2 was studied as a function of orientation. Crack lengths increased with increased temperature up to 500 C; above 800 C, no cracks were found, indicating an indentation brittle-to-ductile transition of about 800 C. The temperature dependence of hardness was reduced around 500 C. Etching studies to delineate the plastic zone around and below indents identified the operative slip systems. The role of dislocations and their interactions within the plastic zone on the hardness and indentation fracture behavior of cubic-ZrO2 are discussed.

Morscher, Gregory N.↗

The effect of hydrogen and microstructure on the deformation and fracture behavior of a single crystal nickel-base superalloy

A study was conducted on the effects of internal hydrogen and microstructure on the deformation and fracture of a single crystal nickel-base superalloy. In particular, room temperature plane strain fracture toughness and tensile tests were performed on hydrogen-free and hydrogen charged samples of PWA 1480. The role of microstructure was incorporated by varying the levels of porosity and eutectic gamma/gamma prime through hot isostatic pressing and heat treatment. The room temperature behavior of PWA 1480 was unusual because precipitate shearing was not the primary deformation mechanism at all strains. At strains over 1 percent, dislocations were trapped in the gamma matrix and an attempt was made to relate this behavior to compositional differences between PWA 1480 and other superalloys. Another unique feature of the tensile behavior was cleavage of the eutectic gamma/gamma prime, which is believed to initiate the failure process. Fracture occurred on (111) planes and is likely a result of shear localization along these planes. Elimination of the eutectic gamma/gamma prime greatly improved the tensile ductility, but pososity had no effect on tensile properties. Large quantities of hydrogen (1.74 at. percent) were gas-phase charged into the material, but surprisingly this was not a function of the amount of porosity or eutectic gamma/gamma prime present. Desorption experiments suggest that the vast majority of hydrogen is at reversible lattice trapping sites. This large, uniform concentration of hydrogen dramatically reduced the tensile strain to failure, but only slightly affected the reduction in area. Available hydrogen embrittlement models were examined in light of these results and it was found that the hydrogen enhanced localized plasticity model can explain much of the tensile behavior. K(IC) fracture toughness tests were conducted, but it was necessary to also perform J(IC) tests to provide valid data.

Walston, William S.↗

Collisional Processing of Comet and Asteroid Surfaces: Velocity Effects on Absorption Spectra

A new paradigm has emerged where 3.9 Gyr ago, a violent reshuffling reshaped the placement of small bodies in the solar system (the Nice model). Surface properties of these objects may have been affected by collisions caused by this event, and by collisions with other small bodies since their emplacement. These impacts affect the spectrographic observations of these bodies today. Shock effects (e.g., planar dislocations) manifest in minerals allowing astronomers to better understand geophysical impact processing that has occurred on small bodies. At the Experimental Impact Laboratory at NASA Johnson Space Center, we have impacted forsterite and enstatite across a range of velocities. We find that the amount of spectral variation, absorption wavelength, and full width half maximum of the absorbance peaks vary non-linearly with the velocity of the impact. We also find that the spectral variation increases with decreasing crystal size (single solid rock versus granular). Future analyses include quantification of the spectral changes with different impactor densities, temperature, and additional impact velocities. Results on diopside, fayalite, and magnesite can be found in Lederer et al., this meeting.

Lederer, S. M.↗

Creep substructure formation in sodium chloride single crystals in the power law and exponential creep regimes

Creep tests conducted on NaCl single crystals in the temperature range from 373 to 1023 K show that true steady state creep is obtained only above 873 K when the ratio of the applied stress to the shear modulus is less than or equal to 0.0001. Under other stress and temperature conditions, corresponding to both power law and exponential creep, the creep rate decreases monotonically with increasing strain. The transition from power law to exponential creep is shown to be associated with increases in the dislocation density, the cell boundary width, and the aspect ratio of the subgrains along the primary slip planes. The relation between dislocation structure and creep behavior is also assessed.

Raj, S. V.↗

X-ray analysis of fatigue damage in copper

A Warren-Averbach x-ray line profile analysis was applied to, broadened x-ray diffraction peaks from copper deformed in fatigue. The copper specimens were fatigued by four point bending at various strain amplitudes, and measurements were made at various fractions of the total fatigue life. The analysis results in an estimation of 1) an average coherently diffracting domain size in a direction normal to the diffracting planes; and 2) a strain distribution function. The strain distribution function is in terms of the root mean square strain, <ϵ^(2)> where ϵ is averaged over a given distance at all points in the diffracting crystals. This rms strain is expressed as a function of averaging distance for a direction normal to the diffracting planes. The rms strains were found to be a function of the fatigue strain amplitude level, increasing with amplitude and reaching a maximum limiting value during the first 2% of the fatigue life. The strains were normally larger in the 4lO0 direction compared to the <111> direction and the absolute values were quite small. These results may be explained by assuming the dislocations are present in the form of dipoles because the lattice strain around a dipole is much less than around single dislocations. Conclusions arrived at in this analysis are in agreement with current theories of fatigue damage in metals. The result that maximum hardening is achieved during the initial few percent of the fatigue life is confirmed by many other investigators using entirely different analytical techniques. It is felt that the structure of the material is changing during this initial hardening stage to an eventual steady state characteristic of the testing conditions. A unique substructure is developed which thereafter persists, and the remainder of the fatigue test is taken up by crack propagation through this substructure until ultimate failure occurs by fracture. The formation of this steady state structure is dependent on the maximum fatigue strain amplitude and on the frequency and temperature of cycling for a particular material.

COPPER↗

Oxide nucleation on thin films of copper during in situ oxidation in an electron microscope

Single-crystal copper thin films were oxidized at an isothermal temperature of 425 C and at an oxygen partial pressure of 0.005 torr. Specimens were prepared by epitaxial vapor deposition onto polished faces of rocksalt and were mounted in a hot stage inside the ultrahigh-vacuum chamber of a high-resolution electron microscope. An induction period of roughly 30 min was established which was independent of the film thickness but depended strongly on the oxygen partial pressure and to exposure to oxygen prior to oxidation. Neither stacking faults nor dislocations were found to be associated with the Cu2O nucleation sites. The experimental data, including results from oxygen dissolution experiments and from repetitive oxidation-reduction-oxidation sequences, fit well into the framework of an oxidation process involving the formation of a surface charge layer, oxygen saturation of the metal with formation of a supersaturated zone near the surface, and nucleation followed by surface diffusion of oxygen and bulk diffusion of copper for lateral and vertical oxide growth, respectively.

Heinemann, K.↗

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↗

Behavior of Particle Depots in Molten Silicon During Float-Zone Growth in Strong Static Magnetic Fields

In the photovoltaics industry, the largest market share is represented by solar cells made from multicrystalline silicon, which is grown by directional solidification. During the growth process, the silicon melt is in contact with the silicon nitride coated crucible walls and the furnace atmosphere which contains carbon monoxide. The dissolution of the crucible coating, the carbon bearing gas, and the carbon already present in the feedstock, lead to the precipitation of silicon carbide, and silicon nitride, at later stages of the growth process. The precipitation of Si3N4 and SiC particles of up to several hundred micrometers in diameter leads to severe problems during the wire sawing process for wafering the ingots. Furthermore the growth of the silicon grains can be negatively influenced by the presence of particles, which act as nucleation sources and lead to a grit structure of small grains and are sources for dislocations. If doped with Nitrogen from the dissolved crucible coating, SiC is a semi conductive material, and can act as a shunt, short circuiting parts of the solar cell. For these reasons, the incorporation of such particles needs to be avoided. In this contribution we performed model experiments in which the transport of intentionally added SiC particles and their interaction with the solid-liquid interface during float zone growth of silicon in strong steady magnetic fields was investigated. SiC particles of 7μm and 60μm size are placed in single crystal silicon [100] and [111] rods of 8mm diameter. This is achieved by drilling a hole of 2mm diameter, filling in the particles and closing the hole by melting the surface of the rod until a film of silicon covers the hole. The samples are processed under a vacuum of 1x10(exp -5) mbar or better, to prevent gas inclusions. An oxide layer to suppress Marangoni convection is applied by wet oxidation. Experiments without and with static magnetic field are carried out to investigate the influence of melt convection on the distribution of particles and their incorporation into the crystal. The field strengths applied by a superconducting magnet are 1T, 3T, 4.5T, and 5T. The increase in field strength dampens the melt flow, and so this study provides comparative data to the crystal growth experiment to be carried out onboard the sounding rocket mission TEXUS 51, where purely diffusive growth condition will be achieved under microgravity conditions.

Jauss, T.↗

Influence of cobalt, tantaum and tungsten on the high temperature mechanical properties of single crystal nickel-base superalloys

For alloys with the baseline refractory metal level of 3 percent Ta and 10 percent W, decreases in Co level from 10 to 0 percent resulted in increased tensile strength and creep resistance. Substitution of W for Ta resulted in decreased creep life at high stresses but improved life at low stresses. Substitution of Ni for Ta caused large reductions in tensile strength and creep resistance, and corresponding increases in ductility. For these alloys with low Ta plus W totals, strength was independent of Co level. The increases in tensile strength with increases in refractory metal content were related to the increases in gamma volume fraction and solid solution hardening. Increases in strength as Co level decreased were considered to be the result of coherency strain hardening from the increased lattice mismatch. Dislocation shear through the gamma-gamma interface is considered to be the rate limiting step in the deformation process.

Nathal, M. V.↗

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.↗

The Cyclic Stress-Strain Behavior of a Single Crystal Nickel-Base Superalloy

The cyclic stress-strain response and similar deformation structures of the single crystal nickel based superalloy was described under a specific set of conditions. The isothermal low cycle fatigue response and deformation structures were described at a typical intermediate temperature and at high temperature. Specimens oriented near the (001) and (111) crystallographic orientations were tested at 1050 C, where more moderate orientation effects were expected. This enabled the description of the deformation structures at each of the 2 temperatures and their relationship to the observed cyclic stress-strain behavior. The initial yield strength of all specimens tested at 650 C was controlled by the shearing of the gamma prime precipitates by dislocation pairs. Low cycle fatigue tests at 650 C had cyclic hardening, which was associated with dislocation interactions in the gamma matrix. The initial yield strength of specimens tested at 1050 C was associated with dislocation bypassing of the gamma prime precipitates. Low cycle fatigue tests at 1050 C had cyclic softening, associated with extensive dislocation recovery at the gamma-gamma prime interfaces along with some gamma prime precipitate coarsening.

Gabb, Timothy P.↗

Accelerated fatigue crack growth behavior of PWA 1480 single crystal alloy and its dependence on the deformation mode

An investigation of the fatigue crack growth (FCG) behavior of PWA 1480 single crystal nickel base superalloy was conducted. Typical Paris region behavior was observed above a delta K of 8 MPa sq rt of m. However, below that stress intensity range, the alloy exhibited highly unusual behavior. This behavior consisted of a region where the crack growth rate became essentially independent of the applied stress intensity. The transition in the FCG behavior was related to a change in the observed crack growth mechanisms. In the Paris region, fatigue failure occurred along (111) facets; however, at the lower stress intensities, (001) fatigue failure was observed. A mechanism was proposed, based on barriers to dislocation motion, to explain the changes in the observed FCG behavior. The FCG data were also evaluated in terms of a recently proposed stress intensity parameter, K sub rss. This parameter, based on the resolved shear stresses on the slip planes, quantified the crack driving force as well as the mode I delta K, and at the same time was also able to predict the microscopic crack path under different stress states.

Telesman, Jack↗

Accelerated fatigue crack growth behavior of PWA 1480

An investigation of the fatigue crack growth (FCG) behavior of PWA 1480 single crystal nickel base superalloy was conducted. Typical Paris region behavior was observed above a delta K of 8 MPa sq rt of m. However, below that stress intensity range, the alloy exhibited highly unusual behavior. This behavior consisted of a region where the crack growth rate became essentially independent of the applied stress intensity. The transition in the FCG behavior was related to a change in the observed crack growth mechanisms. In the Paris region, fatigue failure occurred along (111) facets; however, at the lower stress intensities, (001) fatigue failure was observed. A mechanism was proposed, based on barriers to dislocation motion, to explain the changes in the observed FCG behavior. The FCG data were also evaluated in terms of a recently proposed stress intensity parameter, K sub rss. This parameter, based on the resolved shear stresses on the slip planes, quantified the crack driving force as well as the mode I delta K, and at the same time was also able to predict the microscopic crack path under different stress states.

Telesman, Jack↗

EBIC investigation of hydrogenation of crystal defects in EFG solar silicon ribbons

Changes in the contrast and resolution of defect structures in 205 Ohm-cm EFG polysilicon ribbon subjected to annealing and hydrogenation treatments were observed in a JEOL 733 Superprobe scanning electron microscope, using electron beam induced current (EBIC) collected at an A1 Schottky barrier. The Schottky barrier was formed by evaporation of A1 onto the cleaned and polished surface of the ribbon material. Measurement of beam energy, beam current, and the current induced in the Schottky diode enabled observations to be quantified. Exposure to hydrogen plasma increased charge collection efficiency. However, no simple causal relationship between the hydrogenation and charge collection efficiency could be inferred, because the collection efficiency also displayed an unexpected thermal dependence. Good quality intermediate-magnification (1000X-5400X) EBIC micrographs of several specific defect structures were obtained. Comparison of grown-in and stress-induced dislocations after annealing in vacuum at 500 C revealed that stress-induced dislocations are hydrogenated to a much greater degree than grown-in dislocations. The theoretical approximations used to predict EBIC contrast and resolution may not be entirely adequate to describe them under high beam energy and low beam current conditions.

Sullivan, T.↗

Microscopic observations of X-ray and gamma-ray induced decomposition of ammonium perchlorate crystals

The X-ray and gamma-ray induced decomposition of ammonium perchlorate was studied by optical, transmission, and scanning electron microscopy. This material is a commonly used oxidizer in solid propellents which could be employed in deep-space probes, and where they will be subjected to a variety of radiations for as long as ten years. In some respects the radiation-induced damage closely resembles the effects produced by thermal decomposition, but in other respects the results differ markedly. Similar radiation and thermal effects include the following: (1) irregular or ill-defined circular etch pits are formed in both cases; (2) approximately the same size pits are produced; (3) the pit density is similar; (4) the c face is considerably more reactive than the m face; and (5) most importantly, many of the etch pits are aligned in crystallographic directions which are the same for thermal or radiolytic decomposition. Thus, dislocations play an important role in the radiolytic decomposition process.

Herley, P. J.↗