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At least 271 records · Page 15

SPAR VI Technical Report for Experiment 76-22: Directional Solidification of Magnetic Composites

Samples of eutectic Bi/MnBi were directionally solidified during a low-g interval aboard the SPAR 6 flight and in a l-g environment under identical furnace velocity and thermal conditions. The Bi/MnBi eutectic is characterized by a regular rod eutectic whose morphology may be sensitive to thermo-solutal convection and by its components, MnBi, which is ferromagnetic. Morphological analyses on samples show statistically smaller interrod spacings and rod diameters with respect to samples grown under identical solidification furnace conditions in l-g. An adjustment between the interrod spacing, growth velocity, and total undercooling at the solidification interface is proposed. Morphological analyses on samples grown in l-g indicate little difference between results for different growth orientations with respect to the gravity vector. The magnetic properties are significantly affected, however, by the presence of a nonequilibrium magnetic phase and the nonequilibrium phase transforms to the equilibrium ferromagnetic phase during isothermal heat treatment.

Pirich, R. G.↗

Directional solidification of flake and nodular cast iron during KC-135 low-g maneuvers

Alloys solidified in a low-gravity environment can, due to the elimination of sedimentation and convection, form unique and often desirable microstructures. One method of studying the effects of low-gravity (low-g) on alloy solidification was the use of the NASA KC-135 aircraft flying repetitive low-g maneuvers. Each maneuver gives from 20 to 30 seconds of low-g which is between about 0.1 and 0.001 gravity. A directional solidification furnace was used to study the behavior of off eutectic composition case irons in a low-g environment. The solidification interface of hypereutectic flake and spheroidal graphite case irons was slowly advanced through a rod sample, 5 mm in diameter. Controlled solidification was continued through a number of aircraft parabolas. The known solidification rate of the sample was then correlated with accelerometer data to determine the gravity level during solidification for any location of the sample. The thermal gradient and solidification rate were controlled independently. Samples run on the KC-135 aircraft exhibited bands of coarser graphite or of larger nodules usually corresponding to the regions solidified under low-g. Samples containing high phosphorous (used in order to determine the eutectic cell) exhibited larger eutectic cells in the low-g zone, followed by a band of coarser graphite.

Curreri, P. A.↗

The growth of metastable peritectic compounds

The effects of directional solidification processing on the microstructural, compositional, and magnetic properties of high-melting-temperature, commercially important alloys which form from the liquid state via peritectic or eutectic type reactions were determined. Emphasis was placed on ferromagnetic compounds of the commercially important Co-Sm and Al-Mn systems. The primary dendrite spacing for eutectic Sm2Co17/Co scaled with negative square root of V and varied from approximately 50 microns for V 20 cm/h to hundreds of microns for V 10 cm/h. Since the crystal growth mechanism was dendritic rather than cooperative, the assoicated permanent magnet properties were rather poor. Magnetization as a function of sample orientation indicates that the easy axis of magnetization was primarily along the direction of solidification for the eutectic Sm2Co17/Co and peritectic SmCo5/Sm2Co17 compositions. For the Al-Mn case, magnetization and microstructural characterization suggest isotropic, polycrystalling growth for all solidification velocities studied.

Pirich, R. G.↗

Fluoride salts and container materials for thermal energy storage applications in the temperature range 973 to 1400 K

Multicomponent fluoride salt mixtures were characterized for use as latent heat of fusion heat storage materials in advanced solar dynamic space power systems with operating temperatures in the range of 973 to 1400 K. The melting points and eutectic composition for many systems with published phase diagrams were verified, and several new eutectic compositions were identified. Additionally, the heats of fusion of several binary and ternary eutectics and congruently melting intermediate compounds were measured by differential scanning calorimetry. The extent of corrosion of various metals by fluoride melts was estimated from thermodynamic considerations, and equilibrium conditions inside a containment vessel were calculated as functions of the initial moisture content of the salt and free volume above the molten salt. Preliminary experimental data on the corrosion of commercial, high-temperature alloys in LiF-19.5CaF2 and NaF-27CaF2-36MgF2 melts are presented and compared to the thermodynamic predictions.

Misra, Ajay K.↗

Fluoride salts and container materials for thermal energy storage applications in the temperature range 973 - 1400 K

Multicomponent fluoride salt mixtures were characterized for use as latent heat of fusion heat storage materials in advanced solar dynamic space power systems with operating temperatures in the range of 973 to 1400 K. The melting points and eutectic composition for many systems with published phase diagrams were verified, and several new eutectic compositions were identified. Additionally, the heats of fusion of several binary and ternary eutectics and congruently melting intermediate compounds were measured by differential scanning calorimetry. The extent of corrosion of various metals by fluoride melts was estimated from thermodynamic considerations, and equilibrium conditions inside a containment vessel were calculated as functions of the initial moisture content of the salt and free volume above the molten salt. Preliminary experimental data on the corrosion of commercial, high-temperature alloys in LiF-19.5CaF2 and NaF-27CaF2-36MgF2 melts are presented and compared to the thermodynamic predictions.

Misra, Ajay K.↗

Identification of salt-alloy combinations for thermal energy storage applications in advanced solar dynamic power systems

Thermodynamic calculations based on the available data for flouride salt systems reveal that a number of congruently melting compositions and eutectics exist which have the potential to meet the lightweight, high energy storage requirements imposed for advanced solar dynamic systems operating between about 1000 and 1400 K. Compatibility studies to determine suitable containment alloys to be used with NaF-22CaF2-13MgF2, NaF-32CaF2, and NaF-23MgF2 have been conducted at the eutectic temperature + 25 K for each system. For these three NaF-based eutectics, none of the common, commercially available high temperature alloys appear to offer adequate corrosion resistance for a long lifetime; however mild steel, pure nickel and Nb-1Zr could prove useful. These latter materials suggest the possibility that a strong, corrosion resistant, nonrefractory, elevated temperature alloy based on the Ni-Ni3Nb system could be developed.

Whittenberger, J. D.↗

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

The effect of hydrogen on the tensile deformation behavior of PWA 1480 is presented. Tensile tests were interrupted at different plastic strain levels to observe the development of the dislocation structure. Transmission electron microscopy (TEM) foils were cut perpendicular to the tensile axis to allow the deformation of both phases to be simultaneously observed as well as parallel to zone axes (III) to show the superdislocations on their slip planes. Similar to other nickel-base superalloys, hydrogen was detrimental to the room temperature tensile properties of PWA 1480. There was little effect on strength, however the material was severely embrittled. Even without hydrogen, the elongation-to-failure was only approximately 3 percent. The tensile fracture surface was made up primarily of ductile voids with regions of cleavage fracture. These cleavage facets are the eutectic (gamma') in the microstructure. It was shown by quantitative fractography that hydrogen embrittles the eutectic (gamma') and causes the crack path to seek out and fracture through the eutectic (gamma'). There was two to three times the amount of cleavage on the fracture surface of the hydrogen-charged samples than on the surface of the uncharged samples. The effect of hydrogen can also be seen in the dislocation structure. There is a marked tendency for dislocation trapping in the gamma matrix with and without hydrogen at all plastic strain levels. Without hydrogen there is a high dislocation density in the gamma matrix leading to strain exhaustion in this region and failure through the matrix. The dislocation structure at failure with hydrogen is slightly different. The TEM foils cut parallel to zone axes (III) showed dislocations wrapping around gamma precipitates. Zone axes (001) foils show that there is a lower dislocation density in the gamma matrix which can be linked to the effects of hydrogen on the fracture behavior. The primary activity in the gamma precipitates is in the form of superlattice intrinsic stacking faults (SISFs). These faults have also been reported in other ordered alloys and superalloys.

Walston, W. S.↗

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

The room temperature and 300 C tensile behavior of a single crystal superalloy, PWA 1480, has been studied as a function of internal hydrogen concentration and microstructure. Hydrogen is trapped at the porosity and eutectic gamma/gamma in the microstructure, and the effect of these trapping sites on the tensile behavior will be discussed. There is no effect of hydrogen on strength, however, the strain to failure decreases steadily with increasing hydrogen content up to 200 ppm. Cleavage of the eutectic gamma/gamma occurs without hydrogen, but the presence of internal hydrogen causes cracking in the eutectic gamma/gamma at a much earlier stage of deformation leading to a small total strain. In contrast to many superalloys with a high volume fraction of gamma precipitates, there was no evidence of shearing of the gamma, and it was found that at all strains the dislocations are trapped in the gamma matrix. The effect of hydrogen on this behavior and its relation to fracture is described.

Walston, W. S.↗

A Real Time Investigation of Morphological Evolution During Solidification of Different Alloy Systems

Solidification phenomenon which occur at the solid/liquid (s/I) interface play a major role in the determination of structure and hence the technologically important properties of a casting. However, metals being opaque, conclusions related to several important phenomenon such as boundary layer thickness, morphological evolution, and eutectic and cell spacing are deduced from quenching experiments and subsequent post solidification metallographic analysis. Consequently, limited information is obtained about the dynamics of the process. This paper will discuss the recent efforts at the Space Science Laboratory, NASA Marshall Space Flight Center, to view and quantify in-situ and in real time the dynamics of the solidification process and to measure interfacial undercooling. First, a high resolution x-ray transmission microscope (XTM) has been developed to monitor fundamental interfacial phenomena during directional solidification of metals and alloys. The XTM operates in the range of 10-100 KeV and through projection is capable of achieving magnification of up to 16OX. Secondly, an innovative collapsible furnace has been designed to quantify interfacial undercooling by measuring the temperature of a moving s/I interface in reference to a fixed s/l interface. This measurement technique is non-intrusive in nature and is based on the Seebeck principle. In this paper real time results obtained to characterize the dynamics of irregular eutectic spacing will be presented. As an example fiber to lamella or plate transition in the Al-Al2Au eutectic system will be discussed. Further, a resolution limit of 25 micron has permitted viewing in real time morphological instability and cellular growth in Al-Au and Al-Ag systems. Simultaneously, a systematic investigation has been carried out to measure interfacial undercooling for Pb-1 wt.% Sn at and near the marginal stability regime. In conjunction with the XTM observations this study attempts to validate existing relationships between undercooling and growth velocity during plane front growth, marginal stability regime, and stable cellular growth.

Sen, S.↗

Effect of Growth Rate on Elevated Temperature Plastic Flow and Room Temperature Fracture Toughness of Directionally Solidified NiAl-31Cr-3Mo

The eutectic system Ni-33Al-31Cr-3Mo was directionally solidified at rates ranging from 7.6 to 508 mm/h. Samples were examined for microstructure and alloy chemistry, compression tested at 1200 and 1300 K, and subjected to room temperature fracture toughness measurements. Lamellar eutectic grains were formed at 12.7 mm/h; however cellular structures with a radial eutectic pattern developed at faster growth rates. Elevated temperature compression testing between 10(exp -4) to 10(exp -7)/s did not reveal an optimum growth condition, nor did any single growth condition result in a significant fracture toughness advantage. The mechanical behavior, taken together, suggests that Ni-33Al-31Cr-3Mo grown at rates from 25.4 to 254 mm/h will have nominally equivalent properties.

Whittenberger, J. Daniel↗

Triggered Nucleation in Ni60Nb40 Using an Electrostatic Levitator

External triggering of nucleation in an undercooled liquid metal has been performed for the first time in an electrostatically levitated sample of undercooled eutectic Ni60Nb40. With the Electrostatic Levitator (ESL) facility at NASA/MSFC, NiNb alloys were externally nucleated at various undercooling increments. Observation of the resulting microstructure indicates that only one nucleation site is initiated with a trigger if the undercooling is sufficiently high. Well-defined transition zones exist in all the samples. An "anomalous" fine structured eutectic is initially grown from the nucleation point into the undercooled liquid followed by an unexpected variable width transition zone leading to a coarse structured region of dendrites. Our study tends to corroborate the findings of other studies on highly undercooled eutectics regarding a coupled growth zone within which the lamellar structure is formed and outside of which the anomalous is found.

Rathz, T.↗

Directionally Solidified NiAl-Based Alloys Studied for Improved Elevated-Temperature Strength and Room-Temperature Fracture Toughness

Efforts are underway to replace superalloys used in the hot sections of gas turbine engines with materials possessing better mechanical and physical properties. Alloys based on the intermetallic NiAl have demonstrated potential; however, they generally suffer from low fracture resistance (toughness) at room temperature and from poor strength at elevated temperatures. Directional solidification of NiAl alloyed with both Cr and Mo has yielded materials with useful toughness and elevated-temperature strength values. The intermetallic alloy NiAl has been proposed as an advanced material to extend the maximum operational temperature of gas turbine engines by several hundred degrees centigrade. This intermetallic alloy displays a lower density (approximately 30-percent less) and a higher thermal conductivity (4 to 8 times greater) than conventional superalloys as well as good high-temperature oxidation resistance. Unfortunately, unalloyed NiAl has poor elevated temperature strength (approximately 50 MPa at 1027 C) and low room-temperature fracture toughness (about 5 MPa). Directionally solidified NiAl eutectic alloys are known to possess a combination of high elevated-temperature strength and good room-temperature fracture toughness. Research has demonstrated that a NiAl matrix containing a uniform distribution of very thin Cr plates alloyed with Mo possessed both increased fracture toughness and elevated-temperature creep strength. Although attractive properties were obtained, these alloys were formed at low growth rates (greater than 19 mm/hr), which are considered to be economically unviable. Hence, an investigation was warranted of the strength and toughness behavior of NiAl-(Cr,Mo) directionally solidified at faster growth rates. If the mechanical properties did not deteriorate with increased growth rates, directional solidification could offer an economical means to produce NiAl-based alloys commercially for gas turbine engines. An investigation at the NASA Glenn Research Center at Lewis Field was undertaken to study the effect of the directional solidification growth rate on the microstructure, room temperature fracture toughness, and strength at 1027 C of a Ni-33Al-31Cr-3Mo eutectic alloy. The directionally solidified rates varied between 7.6 and 508 millimeters per hour Essentially fault-free, alternating (Cr, Mo)/NiAl lamellar plate microstructures (left photograph) were formed during growth at and below 12.7 mm/hr, whereas cellular microstructures (right photograph) with the (Cr, Mo) phase in a radial spokelike pattern were developed at faster growth rates. The compressive strength at 1027 C continuously increased with increasing growth rate and did not indicate a maxima as was reported for directionally solidified Ni-33Al-34Cr. Surprisingly, samples with the lamellar plate microstructure (left photograph) possessed a room-temperature fracture toughness of approximately 12 MPa(sup square root of m), whereas all the alloys with a cellular microstructure had a toughness of about 17 MPa(sup square root of m). These results are significant since they clearly demonstrate that Ni-33Al-31Cr-3Mo can be directionally solidified at much faster growth rates without any observable deterioration in its mechanical properties. Thus, the potential to produce strong, tough NiAl-based eutectics at commercially acceptable growth rates exists. Additional testing and alloy optimization studies are underway.

Whittenberger, J. Daniel↗

Structures Self-Assembled Through Directional Solidification

Nanotechnology has created a demand for new fabrication methods with an emphasis on simple, low-cost techniques. Directional solidification of eutectics (DSE) is an unconventional approach in comparison to low-temperature biomimetic approaches. A technical challenge for DSE is producing microstructural architectures on the nanometer scale. In both processes, the driving force is the minimization of Gibb's free energy. Selfassembly by biomimetic approaches depends on weak interaction forces between organic molecules to define the architectural structure. The architectural structure for solidification depends on strong chemical bonding between atoms. Constituents partition into atomic-level arrangements at the liquid-solid interface to form polyphase structures, and this atomic-level arrangement at the liquid-solid interface is controlled by atomic diffusion and total undercooling due to composition (diffusion), kinetics, and curvature of the boundary phases. Judicious selection of the materials system and control of the total undercooling are the keys to producing structures on the nanometer scale. The silicon-titanium silicide (Si-TiSi2) eutectic forms a rod structure under isothermal cooling conditions. At the NASA Glenn Research Center, directional solidification was employed along with a thermal gradient to promote uniform rods oriented with the thermal gradient. The preceding photomicrograph shows the typical transverse microstructure of a solidified Si-TiSi2 eutectic composition. The dark and light gray regions are Si and TiSi2, respectively. Preferred rod orientation along the thermal gradient was poor. The ordered TiSi2 rods have a narrow distribution in diameter of 2 to 3 m, as shown. The rod diameter showed a weak dependence on process conditions. Anisotropic etch behavior between different phases provides the opportunity to fabricate structures with high aspect ratios. The photomicrographs show the resulting microstructure after a wet chemical etch and a dry plasma etch. The wet chemical etches the silicon away, exposing the TiSi2 rods, whereas plasma etching preferentially etches the Si-TiSi2 interface to form a crater. The porous architectures are applicable to fabricating microdevices or creating templates for part fabrication. The porous rod structure can serve as a platform for fabricating microplasma devices for propulsion or microheat exchangers and for fabricating microfilters for miniatured chemical reactors. Although more work is required, self-assembly from DSE can have a role in microdevice fabrication.

Dynys, Frederick W.↗

Atomized BaF2-CaF7 for Better-Flowing Plasma-Spray Feedstock

Atomization of a molten mixture of BaF2 and CaF2 has been found to be superior to crushing of bulk solid BaF2- CaF2 as a means of producing eutectic BaF2-CaF2 powder for use as an ingredient of the powder feedstock of a high-temperature solid lubricant material known as PS304. Developed to reduce friction and wear in turbomachines that incorporate foil air bearings, PS304 is applied to metal substrates by plasma spraying. The constituents of PS304 are: a) An alloy of 80 weight percent Ni and 20 weight percent Cr, b) Cr2O3, c) Ag, and d) The BaF2-CaF2 eutectic, specifically, 62 weight percent BaF2 and 38 weight percent CaF2. The superiority of atomization as a means of producing the eutectic BaF2-CaF2 powder lies in (1) the shapes of the BaF2-CaF2 particles produced and (2) the resulting flow properties of the PS304 feedstock powder: The particles produced through crushing are angular, whereas those produced through atomization are more rounded. PS304 feedstock powder containing the more rounded BaF2-CaF2 particles flows more freely and more predictably, as is preferable for plasma spraying.

DellaCorte, Christopher↗

New space processing experiments for the Skylab missions.

The M512 Materials Processing Facility, which is the main item of equipment for the Skylab space manufacturing experiments is described. It is basically an electron-beam welding apparatus, consisting of a battery power supply, a 20-kV electron beam source, and a spherical 40-cm-diam vacuum chamber. It will be used to perform the M551 Metals Melting Experiment, the M552 Exothermic Brazing Experiment, the M553 Sphere Forming Experiment, the M554 Composite Casting Experiment, the M555 Gallium Arsenide Crystal Growth Experiment, the M561 Whisker-Reinforced Composites Experiment, the M562 Indium Antimonide Crystal Growth, Experiment, the M563 Mixed III-V Crystal Growth Experiment, the M564 Alkali Halide Eutectics Experiment, the M565 Silver Grids Melted in Space Experiment, and the M566 Copper-Aluminum Eutectic Experiment. Three apparatus systems designed to broaden the technical scope of the experiments and to gain experience with new experimental techniques are described. These are an electrophoretic separator, an electromagnetic levitation system, and a versatile electric furnace with an electronic control system.

Bredt, J. H.↗

The electrical properties of low-g processed immiscible alloys

When dispersed or mixed immiscibles are solidified on earth, a large amount of separation of the constituents takes place due to differences in densities. However, when the immiscibles are dispersed and solidified in zero-gravity, density separation does not occur, and unique composite solids can be formed with many new and promising electrical properties. By measuring the electrical resistivity and superconducting critical temperature of zero-g processed Ga-Bi samples, it has been found that the electrical properties of such materials are entirely different from the basic constituents and the ground control samples. The finest dispersions are obtained only in a low-gravity environment. Our results indicate that space-processed immiscible materials may form an entirely new class of electronic materials. The interesting electrical properties of directionally solidified Al-Cu eutectic, a two-component alloy consisting of Al and Al2Cu which was processed on Skylab (M566) are briefly reviewed. The electrical resistivity of directionally solidified eutectics with a lamellar structure are highly anisotropic and have been studied both experimentally and theoretically. The local resistivity of the space-processed samples are compared to a ground control sample and to the expected theoretical results.

Otto, G. H.↗

Radial and directional solidification of metallic systems in space

Investigation of the solidification behavior of spherical specimens of Ni-12 wt % Sn and Ni-1 wt % Ag that froze radially from the surface toward the center and cylindrical specimens of Al-33 wt % Cu eutectic that froze directionally under appropriately selected conditions of thermal gradient at the solid-liquid interface and growth rate. Possible effects of vacuum and low gravity conditions, under which the spherical specimens were processed, on observed nucleation and growth phenomena are discussed. A genetic explanation is given of observed microstructures, and the distributions of alloying elements is discussed. In directionally solidified eutectic specimens a comparison is made between statistically evaluated growth defects in Skylab and in ground specimens.

Katamis, T. Z.↗

Metallurgical processing in space

Research in metallurgical processing to study the effects of reduced gravity started with Apollo 14 and advanced with Skylab. Experiments provided specimens for analysis which solidified while constrained and while freely floating, which contained a mixture of normally immiscible materials, demonstrated enhanced capillary flow, solubility and ordered growth of a directionally solidified eutectic. The smaller, equiaxed grain structure obtained in reduced gravity compared to the larger, elongated grains obtained in one gravity indicate a difference in convection due to gravity in constrained solidification. Freely floating nickel alloy specimens showing metallic gas evolution at low pressure and reduced gravity suggest reduced pressure reactions which cannot occur on earth even in high vacuum chambers due to the hydrostatic head in the molten metal. Directionally solidified eutectics showed fewer termination defects when grown in reduced gravity. These are a few of the differences observed due to reduced gravity which could have important consequences on the future of metallurgy. In this paper we attempt to correlate the results of several Skylab solidification experiments.

Mckannan, E. C.↗