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All sourcesNASA NTRSDOE OSTI
NASA NTRS1998

Use of Microgravity to Control the Microstructure of Eutectics

This grant began in June of 1996. Its long term goal is to be able to control the microstructure of directionally solidified eutectic alloys, through an improved understanding of the influence of convection. The primary objective of the present projects is to test hypotheses for the reported influence of microgravity on the microstructure of three fibrous eutectics (MnBi-Bi, InSb-NiSb, Al3Ni-Al). A secondary objective is to determine the influence of convection on the microstructure of other eutectic alloys. Two doctoral students and a masters student supported as a teaching assistant were recruited for this research. Techniques were developed for directional solidification of MnBi-Bi eutectics with periodic application of current pulses to produce an oscillatory freezing rate. Image analysis techniques were developed to obtain the variation in MnBi fiber spacing, which was found to be normally distributed. The mean and standard deviation of fiber spacing were obtained for several freezing conditions. Eighteen ampoules were prepared for use in the gradient freeze furnace QUELD developed at Queen's University for use in microgravity. Nine of these ampoules will be solidified soon at Queen's in a ground-based model. We hope to solidify the other nine in the QUELD that is mounted on the Canadian Microgravity Isolation Mount on MIR. Techniques are being developed for directional solidification of the Al-Si eutectic at different freezing rates, with and without application of accelerated crucible rotation to induce convection. For the first time, theoretical methods are being developed to analyze eutectic solidification with an oscillatory freezing rate. In a classical sharp-interface model, we found that an oscillatory freezing rate increases the deviation of the average interfacial composition from the eutectic, and increases the undercooling of the two phases by different amounts. This would be expected to change the volume fraction solidifying and the fiber spacing. Because of difficulties in tracking the freezing interfaces of the two solid phases, a phase-field model is also being developed. A paper demonstrating application of phase field methods to periodic structures has been submitted for publication.

Wilcox, William R.↗
NASA NTRS1994

Processing and Mechanical Properties of NiAl-Based In-Situ Composites

In-situ composites based on the NiAl-Cr eutectic system were successfully produced by containerless processing and evaluated. The NiAl-Cr alloys had a fibrous microstructure while the NiAl-(Cr,Mo) alloys containing 1 at. percent or more molybdenum exhibited a lamellar structure. The NiAl-28Cr-6Mo eutectic displays promising high temperature strength while still maintaining a reasonable room temperature fracture toughness when compared to other NiAl-based materials. The Laves phase NiAlTa was used to strengthen NiAl and very promising creep strengths were found for the directionally solidified NiAl-NiAlTa eutectic. The eutectic composition was found to be near NiAl-15.5Ta (at. percent) and well aligned microstructures were produced at this composition. An off-eutectic composition of NiAl-14.5Ta was also processed, consisting of NiAl dendrites surrounded by aligned eutectic regions. The room temperature toughness of these two phase alloys was similar to that of polycrystalline NiAl even with the presence of the brittle Laves phase NiAlTa. Polyphase in-situ composites were generated by directional solidification of ternary eutectics. The systems investigated were the Ni-Al-Ta-X (X=Cr, Mo, or V) alloys. Ternary eutectics were found in each of these systems and both the eutectic composition and temperature were determined. Of these ternary eutectics, the one in the NiAl-Ta-Cr system was found to be the most promising. The fracture toughness of the NiAl-(Cr,Al)NiTa-Cr eutectic was intermediate between those of the NiAl-NiAlTa eutectic and the NiAl-Cr eutectic. The creep strength of this ternary eutectic was similar to or greater than that of the NiAl-Cr eutectic.

Johnson, David Ray↗
NASA NTRS1985

Orbital Processing of Aligned Magnetic Composites

Experiments will be conducted on the space shuttle in which aligned, two-phase magnetic composites will be grown by plane front directional solidification. The objectives are to: (1) identify and quantitatively evaluate the influences of gravitationally driven thermo-solutal convection on contained plane front solidification of binary, eutectic, off-eutectic, and peritectic magnetic composites; (2) to evaluate the effectiveness of micro-g processing as a means of damping convection; and (3) to evaluate the uniqueness of micro-g processing relative to the best of terrestrial convection damping.

Larson, D. J.↗
DOE OSTI2021

Microstructure and creep properties of cast near-eutectic Al–Ce–Ni alloys

This study investigates the as-cast and aged microstructures, thermal stability, ambient temperature strengthening, and creep resistance of three ternary Al–Ce–Ni alloys (wt%): near-eutectic Al–10Ce–5Ni (with both eutectic and hypoeutectic regions), hypoeutectic Al-7.5Ce-3.75Ni (with numerous primary Al dendrites), and hypereutectic Al-12.5Ce-6.25Ni (with coarse, blocky primary Al3Ni and Al11Ce3 precipitates and some primary Al dendrites). Depending on the alloy composition and local solidification conditions, the following eutectic morphologies are found: (i) coarse Al–Ce eutectic colonies where Al 11 Ce 3 is in the form of “Chinese script”, (ii) intermingled regions of binary Al–Ce and Al–Ni eutectic colonies, with finer Al 3 Ni and Al 11 Ce 3 fibers, (iii) large ternary eutectic colonies, where the binary Al 3 Ni and Al 11 Ce 3 phases are alternating or intertwining within the individual, fine fibers (diameters of ~60–170 nm, depending on solidification rates), and (iv) ternary eutectic zones (between primary Al dendrites), where fine Al 3 Ni and Al 11 Ce 3 build up a 3D-interconnected network. The high volume fraction of intermetallic phases and extremely fine eutectic spacing/fiber diameter both contribute to high ambient strengthening (higher as-cast microhardness than binary Al–Ce or Al–Ni), and also provide enhanced creep resistance at 300 and 350 °C. Additionally, the alloys are coarsening-resistant up to 425 °C for extended periods, with a gradual decrease in microhardness. The alloys aged at 400 °C to 1050 h show fiber fragmentation and coarsening of the resulting particles, with the faster-diffusing Ni driving more rapid coarsening of the Al 3 Ni particles which engulf finer, more stable Al 11 Ce 3 particles. Severe overaging (performed at 590 °C for 24 h) leads to Al 3 Ni and Al 11 Ce 3 spheroids which remain submicron-sized in eutectic colonies, but micron-sized at colony boundary and at Al dendrite-eutectic interface. Creep resistance at 300 °C of overaged Al–10Ce–5Ni remains substantial, consistent with load-transfer based composite strengthening being an important strengthening mechanism in these alloys, making them excellent candidates for replacement of heavier steel or titanium parts operating under stress up to 300 °C.

36 MATERIALS SCIENCE↗
NASA NTRS1976

Structure-property relationships in eutectic composites

The preparation of a composite material of eutectic composition directly from the molten state is investigated. The manufacture of eutectic composites by unidirectional solidification is reviewed, and it is shown how two-phase composite structures of given relative volume fraction can be produced with a range of particle sizes. Crystallographic relationships and the thermal stability of interfaces in controlled eutectic structures are examined, the mechanical behavior of aligned eutectic microstructures is discussed, and characteristics of eutectic composites having mechanical properties of engineering significance are evaluated. Specific properties of the Ni-Nb eutectic alloy are reviewed to demonstrate the effect of structure control (through directional solidification) on the mechanical response of a eutectic composite. It is noted that unidirectionally solidified eutectic composites possess highly aligned and thermally stable microstructures and also exhibit excellent combinations of strength and ductility to very high temperature levels.

Hertzberg, R. W.↗
NASA NTRS1996

Development and Processing of Nickel Aluminide-Carbide Alloys

With the upper temperature limit of the Ni-based superalloys attained, a new class of materials is required. Intermetallics appear as likely candidates because of their attractive physical properties. With a relatively low density, high thermal conductivity, excellent oxidation resistance, high melting point, and simple crystal structure, nickel aluminide (NiAl) appears to be a potential candidate. However, NiAl is limited in structural applications due to its low room temperature fracture toughness and poor elevated temperature strength. One approach to improving these properties has been through the application of eutectic composites. Researchers have shown that containerless directional solidification of NiAl-based eutectic alloys can provide improvement in both the creep strength and fracture toughness. Although these systems have shown improvements in the mechanical properties, the presence of refractory metals increases the density significantly in some alloys. Lower density systems, such as the carbides, nitrides, and borides, may provide NiAl-based eutectic structure. With little or no information available on these systems, experimental investigation is required. The objective of this research was to locate and develop NiAl-carbide eutectic alloys. Exploratory arc-melts were performed in NiAl-refractory metal-C systems. Refractory metal systems investigated included Co, Cr, Fe, Hf, Mo, Nb, Ta, Ti, W, and Zr. Systems containing carbides with excellent stability (i.e.,HfC, NbC, TaC, TiC, and ZrC) produced large blocky cubic carbides in an NiAl matrix. The carbides appeared to have formed in the liquid state and were randomly distributed throughout the polycrystalline NiAl. The Co, Cr, Fe, Mo, and W systems contained NiAl dendrites with a two-phase interdendritic microconstituent present. Of these systems, the NiAl-Mo-C system had the most promising microstructure for in-situ composites. Three processing techniques were used to evaluate the NiAl-Mo-C system: arc-melting, slow cooling, and containerless directional solidification. Arc-melting provided a wide range of compositions in an economical and simple fashion. The slow cooled ingots provided larger ingots and slower cooling rates than arc-melting. Directional solidification was used to produce in-situ composites consisting of NiAl reinforced with molybdenum carbides.

Newport, Timothy Scott↗
NASA NTRS2017

Solidification and Morphological Evolution of Al-Si Eutectics in Convector-Diffusive Conditions

The Al-Si material system is an important and has been studied for over half century with a focus on industrial applications in high strength and high conductivity alloys. A great deal of researches have been focused on controlling the morphology and hence performance through the addition of small impurities and by processing conditions. Most of the structure-property correlations are based on the post solidified micromorphology and growth conditions. This material system is unique and has been explored for heat spreader, controlling coefficient of expansion by adjusting composition of silicon and in designing composites. The Al-Si system is very interesting system for understanding the dendritic (Al-rich side) eutectic transition. Recently this system has been of great interest because of its applications in designing heat spreader, low temperature flux to grow SiC large substrates and in controlling the coefficient of expansion of Al-based alloys. We have performed extensive experiments to understand eutectic transition and to understand the morphological evolution in presence of impurities. We will discuss the results of dendritic transition into faceted long grains in convector-diffusive conditions. In this presentation we will present morphological transition in presence of carbon impurity and development of novel morphology.

Singh, N. B.↗
DOE OSTI2020

Ultrahigh strength and plasticity in laser rapid solidified Al–Si nanoscale eutectics

As-cast Al–20wt.% Si alloys were processed via laser rapid solidification (LRS) techniques to create eutectic microstructures with nanoscale interconnected, nanotwinned Si fibers. LRS morphologies exhibit higher flow stress, exceeding 800 MPa and uniform plastic deformation above 20% compared to as-cast alloy that fractures at strains below 8% at flow strength of approximately 200 MPa. The strengthening mechanisms of LRS morphologies are interpreted in terms of the interfacial constraints: increase in yield strength as well as strain hardening rate due to nanoscale confined slip in fibrous Al–Si eutectic, and load transfer and eventual plasticity in the nanoscale Si fibers.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Effect of Cooling Rate on Nano-Eutectic Formation in Laser Surface Remelted and Rare Earth Modified Hypereutectic Al-20Si Alloys

Laser Surface Remelting (LSR) was applied to arc-melted Al-20Si-0.2Sr, Al-20Si-0.2Ce, and Al-20Si hypereutectic alloys to refine microstructures. Experiments revealed that microstructures in the melt pool varied from fully eutectic to a mixture of Al dendrites and inter-dendritic eutectic. We calculated cooling rates using the Eagar-Tsai model and correlated cooling rates with characteristic microstructures, revealing that a cooling rate on the order of 104 K/s could lead to maximized fully eutectic microstructure morphology. Due to rapid solidification, the Si composition in the LSR eutectic was measured at 18.2 wt.%, higher than the equilibrium eutectic composition of 12.6 wt.%Si. Compared to Al-20Si, Ce addition had no significant effect on the volume fraction of the fully eutectic structure but refined Si fibers to approximately 30 nm in diameter. Sr addition did not further refine the diameter of eutectic Si fibers compared to Al-20Si but increased the volume fraction of the fully eutectic microstructure morphology. The refinement ratio (φ) of the Si fiber diameter from the bottom of the melt pool to the surface for the three alloys was similar, at around 28%. The established correlation between the cooling rate and the size and morphology of the microstructure within the melt pool will enable tailoring of the microstructure in laser-processed as well as deposited alloys for high strength and plasticity.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Multi-Step Crystallization of Self-Organized Spiral Eutectics

A method for the solidification of metallic alloys involving spiral self-organization is presented as a new strategy for producing large-area chiral patterns with emergent structural and optical properties, with attention to the underlying mechanism and dynamics. This study reports the discovery of a new growth mode for metastable, two-phase spiral patterns from a liquid metal. Crystallization proceeds via a non-classical, two-step pathway consisting of the initial formation of a polytetrahedral seed crystal, followed by ordering of two solid phases that nucleate heterogeneously on the seed and grow in a strongly coupled fashion. Crystallographic defects within the seed provide a template for spiral self-organization. These observations demonstrate the ubiquity of defect-mediated growth in multi-phase materials and establish a pathway toward bottom-up synthesis of chiral materials with an inter-phase spacing comparable to the wavelength of infrared light. Given that liquids often possess polytetrahedral short-range order, our results are applicable to many systems undergoing multi-step crystallization.

36 MATERIALS SCIENCE↗
NASA NTRS2003

Simulating the Effect of Space Vehicle Environments on Directional Solidification of a Binary Alloy

Space microgravity missions are designed to provide a microgravity environment for scientific experiments, but these missions cannot provide a perfect environment, due to vibrations caused by crew activity, on-board experiments, support systems (pumps, fans, etc.), periodic orbital maneuvers, and water dumps. Therefore, it is necessary to predict the impact of these vibrations on space experiments, prior to performing them. Simulations were conducted to study the effect of the vibrations on the directional solidification of a dendritic alloy. Finite element ca!cu!attie?ls were dme with a simd2titcr based on a continuum model of dendritic solidification, using the Fractional Step Method (FSM). The FSM splits the solution of the momentum equation into two steps: the viscous intermediate step, which does not enforce continuity; and the inviscid projection step, which calculates the pressure and enforces continuity. The FSM provides significant computational benefits for predicting flows in a directionally solidified alloy, compared to other methods presently employed, because of the efficiency gains in the uncoupled solution of velocity and pressure. finite differences, arises when the interdendritic liquid reaches the eutectic temperature and concentration. When a node reaches eutectic temperature, it is assumed that the solidification of the eutectic liquid continues at constant temperature until all the eutectic is solidified. With this approach, solidification is not achieved continuously across an element; rather, the element is not considered solidified until the eutectic isotherm overtakes the top nodes. For microgravity simulations, where the convection is driven by shrinkage, it introduces large variations in the fluid velocity. When the eutectic isotherm reaches a node, all the eutectic must be solidified in a short period, causing an abrupt increase in velocity. To overcome this difficulty, we employed a scheme to numerically predict a more accurate value for the rate of change of fraction of liquid as the liquid in an element solidifies. The new method enables us to contrast results of simulations in which the alloy is subjected to no gravity or a steady-state acceleration versus simulations when the alloy is subjected to vibration disturbances; therefore, the effect of vibration disturbances can be assessed more accurately. To assess the impact of these vibration-perturbations, transient accelerometer data from a space shuttle mission are used as inputs for the simulation model. These on-orbit acceleration data were obtained from the Microgravity Science Division at Glenn Research Center (GRC- MSD) and are applied to the buoyancy term of the momentum equation in a simulation of a Pb-5.8 wt. % Sb alloy that solidifies in a thermal gradient of 4000 K/m and a translation velocity of 3 p d s . Figure 2 shows the vertical velocity of a node that begins in the all-liquid region and subsequently solidifies; the vibrations are applied at 5000 seconds in this simulation. An important difficulty, common to all solidification models based on finite elements or 2 The magnitudes of the velocity oscillations that are vibration-induced are very small and acceptable. The biggest concern is whether the concentration of the liquid near the dendrite tips is distorted because of the vibration-induced perturbations. Results for this case show no concentration oscillations present in the all-liquid region.

Westra, D. G.↗
NASA NTRS1975

Directionally solidified pseudo-binary eutectics of Ni-Cr-(Hf, Zr)

A pseudo-binary eutectic, in which the intermetallic Ni7Hf2 reinforces the Ni-Cr solid solution phase, was previously predicted in the Ni-Cr-Hf system by a computer analysis. The experimental determination of pseudo binary eutectic compositions and the directional solidification of the Ni-Cr-Hf, Zr, and Ni-Cr-Zr eutectic alloys are discussed. To determine unknown eutectics, chemical analyses were made of material bled from near eutectic ingots during incipient melting. Nominal compositions in weight percent of Ni-18.6Cr-24.0HF, Ni19.6Cr-12.8Zr-2.8Hf, and Ni-19.2Cr-14.8Zr formed aligned pseudo-binary eutectic structures. The melting points were about 1270 C. The reinforcing intermetallic phases were identified as noncubic (Ni,Cr)7Hf2 and (Ni,Cr)7(Hf,Zr)2, and face centered cubic (Ni,Cr)5Zr. The volume fraction of the reinforcing phases were about 0.5.

Kim, Y. G.↗
NASA NTRS1975

Directionally solidified pseudo-binary eutectics of Ni-Cr-/Hf,Zr/

This report is concerned with the experimental determination of pseudo binary eutectic compositions and the directional solidification of the Ni-Cr-Hf,Zr, and Ni-Cr-Zr eutectic alloys. To determine unknown eutectics, chemical analyses were made of material bled from near eutectic ingots during incipient melting. Nominal compositions in weight per cent of Ni-18.6Cr-24.0Hf, Ni-19.6Cr-12.8Zr-2.8Hf, and Ni-19.2Cr-14.8Zr formed aligned pseudo-binary eutectic structures. The melting points were about 1270 C. The reinforcing intermetallic phases were identified as noncubic (Ni,Cr)7Hf2 and (Ni,Cr)7(Hf,Zr)2, and face centered cubic (Ni,Cr)5Zr. The volume fraction of the reinforcing phases were about 0.5.

Kim, Y. G.↗
DOE OSTI2021

Mechanical Behavior of Al–Al2Cu–Si and Al–Al2Cu Eutectic Alloys

In this study, laser rapid solidification technique was used to refine the microstructure of ternary Al–Cu–Si and binary Al–Cu eutectic alloys to nanoscales. Micropillar compression testing was performed to measure the stress–strain response of the samples with characteristic microstructure in the melt pool regions. The laser-remelted Al–Al2Cu–Si ternary alloy was observed to reach the compressive strength of 1.59 GPa before failure at a strain of 28.5%, which is significantly better than the as-cast alloy with a maximum strength of 0.48 GPa at a failure strain of 4.8%. The laser-remelted Al–Cu binary alloy was observed to reach the compressive strength of 2.07 GPa before failure at a strain of 26.5%, which is significantly better than the as-cast alloy with maximum strength of 0.74 GPa at a failure strain of 3.3%. The enhanced compressive strength and improved compressive plasticity were interpreted in terms of microstructural refinement and hierarchical eutectic morphology.

36 MATERIALS SCIENCE↗
NASA NTRS1987

Directional solidification of Bi-Mn alloys using an applied magnetic field

Off-eutectic compositions of Bi-Mn were directionally solidified in applied transverse magnetic fields up to 3 kG, to determine the effects on thermal and solutal convection. Plane front directional solidification of eutectic and near-eutectic Bi-Mn results in a two-phase rodlike morphology consisting of ferromagnetic MnBi rods in a Bi solid solution matrix. Compositions of either side of the eutectic were studied in growth orientations vertically up and down. Temperature gradient was monitored during growth by means of an in-situ thermocouple. For Bi-rich compositions, the magnetic field appeared to increase mixing as determined from thermal, morphological, chemical, and magnetic analyses. For Mn-rich compositions, morphological and chemical analyses suggest some reduction in mixing due to application of the magnetic force. The capability for carrying out directional solidification of Bi-Mn in high longitudinal magnetic fields was established.

Decarlo, J. L.↗
NASA NTRS1994

Influence of convection on microstructure

The primary motivation for this research was to determine the cause for space processing altering the microstructure of some eutectics, especially the MnBi-Bi eutectic. Four primary hypotheses were to be tested under this current grant: (1) A fibrous microstructure is much more sensitive to convection than a lamellar microstructure, which was assumed in our prior theoretical treatment. (2) An interface with one phase projecting out into the melt is much more sensitive to convection than a planar interface, which was assumed in our prior theoretical treatment. (3) The Soret effect is much more important in the absence of convection and has a sufficiently large influence on microstructure that its action can explain the flight results. (4) The microstructure is much more sensitive to convection when the composition of the bulk melt is off eutectic. These hypotheses were tested. It was concluded that none of these can explain the Grumman flight results. Experiments also were performed on the influence of current pulses on MnBi-Bi microstructure. A thorough review was made of all experimental results on the influence of convection on the fiber spacing in rod eutectics, including results from solidification in space or at high gravity, and use of mechanical stirring or a magnetic field. Contradictory results were noted. The predictions of models for convective influences were compared with the experimental results. Vigorous mechanical stirring appears to coarsen the microstructure by altering the concentration field in front of the freezing interface. Gentle convection is believed to alter the microstructure of a fibrous eutectic only when it causes a fluctuating freezing rate with a system for which the kinetics of fiber branching differs from that for fiber termination. These fluctuations may cause the microstructure to coarsen or to become finer, depending on the relative kinetics of these processes. The microstructure of lamellar eutectics is less sensitive to freezing rate fluctuations and to gentle convection.

Wilcox, William R.↗
NASA NTRS2007

Solidification Behavior of gamma'-Ni3Al Containing Alloys in the Ni-Al-O System

The chemical activities of Al and Ni in gamma(prime)-Ni3Al-containing systems were measured using the multi-cell Knudsen effusion-cell mass spectrometry technique (multi-cell KEMS), over the composition range 8 - 32 at.%Al and temperature range T = 1400 - 1750 K. From these measurements a better understanding of the equilibrium solidification behaviour of gamma(prime)-Ni3Al-containing alloys in the Ni-Al-O system was established. Specifically, these measurements revealed that (1) gamma(prime)-Ni3Al forms via the peritectiod reaction, gamma + Beta (+ A12O3) = gamma (prime) (+ Al2O3), at 1633 +/- 1 K, (2) the {gamma + Beta + Al2O3} phase field is stable over the temperature range 1633 through 1640 K, and (3) equilibrium solidification occurs by the eutectic reaction, L (+ Al2O3) = gamma + Beta (+ Al2O3), at 1640 +/- 1 K and a liquid composition of 24.8 +/- 0.2 at.%Al (at an unknown oxygen content). When projected onto the Ni-Al binary, this behaviour is inconsistent with the current Ni-Al phase diagram and a new diagram is proposed. This new Ni-Al phase diagram explains a number of unusual steady-state solidification structures reported previously and provides a much simpler reaction scheme in the vicinity of the gamma(prime)-Ni3Al phase field.

Copland, Evan↗