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At least 55 records · Page 3

Solidification in immiscible systems: The influence of processing conditions on resulting microstructures

Research carried out over the past two decades in which attempts have been made to produce desirable microstructures in immiscible alloys is reviewed. Factors affecting the formation of desirable microstructures in immiscible alloys are addressed and some of the techniques that have been successful in controlling these factors in order to produce useful structures are discussed. Some of the intended applications of these alloys require a dispersion of one phase in the other, while other applications favor the use of aligned, fibrous microstructures with continuity of both phases. The microstructures obtained in immiscible alloys are often strongly influenced by processing conditions. Perhaps the most well known effect is gravity induced sedimentation of the denser immiscible phase during solidification. This difficulty with sedimentation led to low gravity processing in attempts to produce dispersed microstructures. However, experimentation under low gravity conditions soon revealed that many other factors, including wetting of the crucible walls and surface tension driven flows, often resulted in complete separation and coalescence of the two immiscible phases. The production of aligned fibrous microstructures in hypermonotectic alloys appears to be even more difficult than the formation of a dispersion. Here, in addition to sedimentation and crucible wetting, convective and interfacial instabilities must be considered as well. Calculation of the limits of stability during directional solidification were carried out but require experimental verification.

Andrews, J. Barry↗

Microstructural Development of Directionally Solidified Hg(1-x)Zn(x)Se Alloys

Hg(1-x)Zn(x)Se alloys have been studied as an alternative to HgCdTe for the detection of electromagnetic radiation, because the shorter ZnSe and HgSe bonds were predicted to improve lattice stability. Previous studies showed that optical properties were stable with time and that the microhardness was higher than for HgTe based alloys. However, for this material to be commercially viable, compositional variations must be reduced, and the distribution of defects induced by the growth process must be understood. The basic structural properties of bulk materials were characterized, and dislocation etch pit densities were measured to determine whether the addition of Zn to the HgSe lattice reduced the potential for dislocation formation. Hg(0.9)Zn(0.1)Se alloys were directionally solidified using a modified Bridgman-Stockbarger method and in an applied magnetic field. Radial compositional variations were greatly reduced when solidification occurred in an applied magnetic field. The combination of a convex liquid-solid interface shape and a method for reduced wetting produced boules that were a single crystal after reaching full diameter. Observed surface features indicated ampoule wetting could be eliminated using a graphite getter. Microstructural characteristics were greatly improved over HgCdTe alloys, In six boules, a total of only one twin was observed, and no inclusions were found. A method for polishing and producing dislocation etch pits was developed for these alloys, revealing dislocation etch pit densities one to two orders of magnitude less than HgTe based alloys. A kink in the thermal profile during processing of one boule generated more dislocations than did lattice mismatch due to compositional variations. The results of this investigation indicate this alloy has improved microstructural properties and resistance to dislocation formation compared with similar II-VI alloys, and should be further investigated for the detection of electromagnetic radiation.

Cobb, S. D.↗

Three-Dimensional In Situ Observations of Polycrystalline Microstructure Evolution During Directional Solidification of Transparent Alloys Aboard the ISS and Quantitative Comparison with Numerical Modeling

Cellular/dendritic microstructures formed during solidification have a crucial influence on the mechanical properties of a wide range of structural alloys. By minimizing the amount of gravity-induced convection in the liquid, directional solidification experiments using transparent organic alloys conducted in the DECLIC-DSI onboard the International Space Station have provided unique 3D in situ observations of the spatiotemporal evolution of the solid-liquid interface during the formation of cellular and dendritic microstructures under purely diffusive growth conditions. Those observations have made it possible to perform benchmark quantitative comparisons with the predictions of state-of-the-art phase-field simulations of microstructure formation in 3D on experimentally relevant length and time scales. This talk will report quantitative comparisons between microgravity experiments and phase-field simulations in succinonitrile-camphor alloys of two different compositions, which shed new light on the selection of dendritic array structures, and on roles of macroscopic curvatures and subgrain boundaries between grains with a small misorientation with respect to the temperature gradient in the spatiotemporal evolution of the primary cellular spacing.

Kaihua Ji↗

Melt spinning study

Containerless processing of materials provides an excellent opportunity to study nucleation phenomena and produce unique materials, primarily through the formation of metastable phases and deep undercoolings. Deep undercoolings can be readily achieved in falling drops of molten material. Extended solute solubilities and greatly refined microstructures can also be obtained in containerless processing experiments. The Drop Tube Facility at Marshall Space Flight Center has played an important role in enhancing that area of research. Previous experiments performed in the Drop Tube with refractory metals has shown very interesting microstructural changes associated with deep undercoolings. It is apparent also that the microstructure of the deep undercooled species may be changing due to the release of the latent heat of fusion during recalescence. For scientific purposes, it is important to be able to differentiate between the microstructures of the two types of metallic species. A review of the literature shows that although significant advances have been made with respect to the engineering aspects of rapid solidification phenomena, there is still much to be learned in terms of understanding the basic phenomena. The two major ways in which rapid solidification processing provides improved structures and hence improved properties are: (1) production of refined structures such as fine dendrites and eutectics, and (2) production of new alloy compositions, microstructures, and phases through extended solid solubility, new phase reaction sequences, and the formation of metallic-glass microstructures. The objective of this work has been to determine the optimal methodology required to extract this excess energy without affecting the thermo-physical parameters of the under-cooled melt. In normal containerless processing experiments recalescence occurs as the melt returns toward the melting point in order to solidify. A new type of experiment is sought in which the resultant microstructure of the undercooled species is frozen in without going through the melting point regime and subsequent near equilibrium solidification of the remaining liquid. This experimental approach entails the design of an appropriate melt spinning system which is compatible with Drop Tube operations and processing constraints. That work is the goal of this study.

Workman, Gary L.↗

Utilizing local phase transformation strengthening for nickel-based superalloys

Almost 75 years of research has been devoted to producing superalloys capable of higher operating temperatures in jet turbine engines, and there is an ongoing need to increase operating temperature further. Here, a new disk Nickel-base superalloy is designed to take advantage of strengthening atomic-scale dynamic complexions. This local phase transformation strengthening provides the alloy with a three times improvement in creep strength over similar disk superalloys and comparable strength to a single crystal blade alloy at 760 °C. Ultra-high-resolution chemical mapping reveals that the improvement in creep strength is a result of atomic-scale η (D024) and χ (D019) formation along superlattice stacking faults. To understand these results, the energy differences between the L12 and competing D024 and D019 stacking fault structures and their dependence on composition are computed by density functional theory. This study can help guide researchers to further optimize local phase transformation strengthening mechanisms for alloy development.

Timothy M. Smith↗

Vacuum Plasma Spray of CuCrNb Alloy for Advanced Liquid - Fuel Combustion Chambers

The copper-8 atomic percent chromium-4 atomic percent niobium (CuCrNb) alloy was developed by Glenn Research Center (formally Lewis Research Center) as an improved alloy for combustion chamber liners. In comparison to NARloy-Z, the baseline (as in Space Shuttle Main Engine) alloy for such liners, CuCrNb demonstrates mechanical and thermophysical properties equivalent to NARloy-Z, but at temperatures 100 C to 150 C (180 F to 270 F) higher. Anticipated materials related benefits include decreasing the thrust cell liner weight 5% to 20%, increasing the service life at least two fold over current combustion chamber design, and increasing the safety margins available to designers. By adding an oxidation and thermal barrier coating to the liner, the combustion chamber can operate at even higher temperatures. For all these benefits, however, this alloy cannot be formed using conventional casting and forging methods because of the levels of chromium and niobium, which exceed their solubility limit in copper. Until recently, the only forming process that maintains the required microstructure of CrNb intermetallics is powder metallurgy formation of a billet from powder stock, followed by extrusion. This severely limits its usefulness in structural applications, particularly the complex shapes required for combustion chamber liners. Vacuum plasma spray (VPS) has been demonstrated as a method to form structural articles including small combustion chambers from the CuCrNb alloy. In addition, an oxidation and thermal barrier layer can be formed integrally on the hot wall of the liner that improve performance and extend service life. This paper discusses the metallurgy and thermomechanical properties of VPS formed CuCrNb versus the baseline powder metallurgy process, and the manufacturing of small combustion chamber liners at Marshall Space Flight Center using the VPS process. The benefits to advanced propulsion initiatives of using VPS to fabricate combustion chamber liners while maintaining the superior CuCrNb properties are also presented.

Zimmerman, Frank↗

The microstructure and formation of duplex and black plessite in iron meteorites

Two of the most common plessite structures, duplex and black plessite, in the taenite region of the Windmanstatten pattern of two iron meteorites (Grant and Carlton) are characterized using high-resolution electron microscopy and microanalysis techniques. Two types of gamma precipitates, found in the duplex plessite and black plessite regions, respectively, are identified, and their morphologies are described. The formation of the plessite structure is discussed using the information obtained in this study and results of a parallel investigation of decomposed martensitic Fe-Ni laboratory alloys.

Zhang, J.↗

Three-dimensional in Situ Observations of Polycrystalline Microstructure Evolution During Directional Solidification of Transparent Alloys Aboard the ISS and Quantitative Comparison with Numerical Modeling

Cellular/dendritic microstructures formed during solidification have a crucial influence on the mechanical properties of a wide range of structural alloys. By minimizing the amount of gravity-induced convection in the liquid, directional solidification experiments using transparent organic alloys conducted in the DECLIC-DSI onboard the International Space Station have provided unique 3D in situ observations of the spatiotemporal evolution of the solid-liquid interface during the formation of cellular and dendritic microstructures under purely diffusive growth conditions in polycrystalline samples containing several grains with a small misorientation with respect to the temperature gradient. Those observations have made it possible to perform benchmark quantitative comparisons with the predictions of state-of-the-art phase-field simulations of microstructure formation in 3D on experimentally relevant length and time scales. This talk will report quantitative comparisons between microgravity experiments and phase-field simulations in succinonitrile-camphor alloys of two different compositions that shed new light on the role of subgrain boundaries in the spatiotemporal evolution of the primary cellular spacing and the selection of dendritic array structures.

Kaihua Ji↗

Energy landscape in Ni-Co-Cr and related alloys

Among multi-principal element alloys, the NiCoCr middle-entropy alloy has an outstanding combination of strength and ductility at both low and elevated temperatures. Equiatomic NiCoCr is a single-phase alloy with the face centered cubic (fcc) crystal structure. A low stacking fault energy in the fcc matrix is a cause of a relatively low creep in this alloy. The hexagonal close-packed (hcp) structure differs from the fcc by a stacking of atomic layers. The energy difference between the hcp and fcc structures is known to correlate with the stacking fault energy in the fcc phase. We compute formation and relative structural energies versus composition in the Ni-Co-Cr ternary and related quaternary systems, discuss possibilities of compositional adjustments, and compare theoretical predictions with experiment. We acknowledge funding by NASA’s Aeronautics Research Mission Directorate (ARMD) via Transformational Tools and Technologies (TTT) Project.

NiCoCr↗

NiAl alloys for structural uses

Alloys based on the intermetallic compound NiAl are of technological interest as high temperature structural alloys. These alloys possess a relatively low density, high melting temperature, good thermal conductivity, and (usually) good oxidation resistance. However, NiAl and NiAl-base alloys suffer from poor fracture resistance at low temperatures as well as inadequate creep strength at elevated temperatures. This research program explored macroalloying additions to NiAl-base alloys in order to identify possible alloying and processing routes which promote both low temperature fracture toughness and high temperature strength. Initial results from the study examined the additions of Fe, Co, and Hf on the microstructure, deformation, and fracture resistance of NiAl-based alloys. Of significance were the observations that the presence of the gamma-prime phase, based on Ni3Al, could enhance the fracture resistance if the gamma-prime were present as a continuous grain boundary film or 'necklace'; and the Ni-35Al-20Fe alloy was ductile in ribbon form despite a microstructure consisting solely of the B2 beta phase based on NiAl. The ductility inherent in the Ni-35Al-20Fe alloy was explored further in subsequent studies. Those results confirm the presence of ductility in the Ni-35Al-20Fe alloy after rapid cooling from 750 - 1000 C. However exposure at 550 C caused embrittlement; this was associated with an age-hardening reaction caused by the formation of Fe-rich precipitates. In contrast, to the Ni-35Al-20Fe alloy, exploratory research indicated that compositions in the range of Ni-35Al-12Fe retain the ordered B2 structure of NiAl, are ductile, and do not age-harden or embrittle after thermal exposure. Thus, our recent efforts have focused on the behavior of the Ni-35Al-12Fe alloy. A second parallel effort initiated in this program was to use an alternate processing technique, mechanical alloying, to improve the properties of NiAl-alloys. Mechanical alloying in the conventional sense requires ductile powder particles which, through a cold welding and fracture process, can be dispersion strengthened by submicron-sized oxide particles. Using both the Ni-35Al-Fe alloys to contain approx. 1 v/o Y2O3. Preliminary results indicate that mechanically alloyed and extruded NiAl-Fe + Y2O3 alloys when heat treated to a grain-coarsened condition, exhibit improved creep resistance at 1000 C when compared to NiAl; oxidation resistance comparable to NiAl; and fracture toughness values a factor of three better than NiAl. As a result of the research initiated on this NASA program, a subsequent project with support from Inco Alloys International is underway.

Koss, D. A.↗

Dynamic Instability of Solidification Fronts and Formation of Transverse Layered Structures

A plane front of crystallization in a unidirectional process of solidification of a binary melt or a solution is shown to be unstable with respect to virtual perturbations of the front velocity within some region of physical and operating parameters. This dynamic instability has nothing in common with morphological instability of the front also possible under certain conditions. It gives rise to the origination of a self-oscillating regime of solidification. The oscillations of the front velocity are accompanied by oscillations of other relevant variables, such as the melt concentration and temperature at the front. What is most important is that this provides for a natural explanation of phenomena of the formation of ordered striations commonly observed when producing alloys and withdrawing crystals. A theory of nonlinear instability of the solidification front is developed which also allows for properties of both self-oscillating regimes of solidification and transverse layered structures it allows to be described in an explicit form, without introducing any additional hypotheses and empirical parameters. Apart from other things, the properties are strongly dependent on convective transport originated in consequence of a difference between the densities of the liquid melt and solid alloy. The theory results in a remarkably good agreement with experimental evidence on crystal withdrawal obtained in normal gravity and under space flight conditions. The problem of interplay between modes of the dynamic and morphological types of instability is also discussed. There are parametric regions in which either only one of these types occurs or both of them arise simultaneously.

Buyevich, Yu A.↗

Containerless processing of hypermonotectic and glass forming alloys using the Marshall Space Flight Center 100 meter drop tube facility

Two separate projects were carried out to study alloys whose solidification structures can be strongly influenced by the presence of a container during melting and solidifications. One project involved containerless solidification of hypermonotectic Au35Rh65 alloys. This alloy exhibits liquid immiscibility over a temperature range. It has been suggested that containerless melting might be one solution to the problem of sedimentation in the dispersions of immiscible liquid phases. However, surface tension driven flows could also lead to accumulation of the minority liquid phase at the external surface of a containerlessly melted alloy. The research underway is a first step in determining the influence of containerless, microgravity processing on immiscible alloys. Nickel-niobium alloys were studied using the drop tube facility. One alloy in this system, a Ni60Nb40 alloy, is a good candidate for the formation of a bulk metallic glass. Amorphous alloys of this composition were produced using thin film and mechanical alloying techniques. However, theory indicates that if heterogeneous nucleation can be avoided, it should be possible to produce an amorphous structure in this system using a moderate cooling rate from the melt. The containerless melting and solidification capabilities of the drop tube faciltiy provide ideal conditions for a study of this type. To date, several Ni60Nb40 samples have been levitated, melted and cooled during 4.6 seconds of free fall in the 100 meter drop tube. Structures obtained are discussed.

Andrews, J. B.↗

Boron Arsenide and Boron Phosphide for High Temperature and Luminescent Devices

The crystal growth of boron arsenide and boron phosphide in the form of bulk crystals and epitaxial layers on suitable substrates is discussed. The physical, chemical, and electrical properties of the crystals and epitaxial layers are examined. Bulk crystals of boron arsenide were prepared by the chemical transport technique, and their carrier concentration and Hall mobility were measured. The growth of boron arsenide crystals from high temperature solutions was attempted without success. Bulk crystals of boron phosphide were also prepared by chemical transport and solution growth techniques. Techniques required for the fabrication of boron phosphide devices such as junction shaping, diffusion, and contact formation were investigated. Alloying techniques were developed for the formation of low-resistance ohmic contacts to boron phosphide. Four types of boron phosphide devices were fabricated: (1) metal-insulator-boron phosphide structures, (2) Schottky barriers; (3) boron phosphide-silicon carbide heterojunctions; and (4) p-n homojunctions. Easily visible red electroluminescence was observed from both epitaxial and solution grown p-n junctions.

Chu, T. L.↗

Heats of formation of bcc binary alloys

The method of Bozzolo, Ferrante and Smith is applied for the calculation of alloy energies for bcc elements. The heat of formation of several alloys is computed with the help of the Connolly-Williams method within the tetrahedron approximation. The dependence of the results on the choice of different sets of ordered structures is discussed.

Bozzolo, Guillermo↗

Heats of formation of bcc binary alloys

The method of Bozzolo, Ferrante and Smith is applied for the calculation of alloy energies for bcc elements. The heat of formation of several alloys is computed with the help of the Connolly-Williams method within the tetrahedron approximation. The dependence of the results on the choice of different sets of ordered structures is discussed.

Bozzolo, Guillermo↗

Development and Processing Improvement of Aerospace Aluminum Alloys

This final report, in multiple presentation format, describes a comprehensive multi-tasked contract study to improve the overall property response of selected aerospace alloys, explore further a newly-developed and registered alloy, and correlate the processing, metallurgical structure, and subsequent properties achieved with particular emphasis on the crystallographic orientation texture developed. Modifications to plate processing, specifically hot rolling practices, were evaluated for Al-Li alloys 2195 and 2297, for the recently registered Al-Cu-Ag alloy, 2139, and for the Al-Zn-Mg-Cu alloy, 7050. For all of the alloys evaluated, the processing modifications resulted in significant improvements in mechanical properties. Analyses also resulted in an enhanced understanding of the correlation of processing, crystallographic texture, and mechanical properties.

Lisagor, W. Barry↗

The Features of Self-Assembling Organic Bilayers Important to the Formation of Anisotropic Inorganic Materials in Microgravity Conditions

There is a growing need for inorganic anisotropic particles in a variety of materials science applications. Structural, optical, and electrical properties can be greatly augmented by the fabrication of composite materials with anisotropic microstructures or with anisotropic particles uniformly dispersed in an isotropic matrix. Examples include structural composites, magnetic and optical recording media, photographic film, certain metal and ceramic alloys, and display technologies including flat panel displays. While considerable progress has been made toward developing an understanding of the synthesis of powders composed of monodispersed, spherical particles, these efforts have not been transferred to the synthesis of anisotropic nanoparticles. The major objective of the program is to develop a fundamental understanding of the growth of anisotropic particles at organic templates, with emphasis on the chemical and structural aspects of layered organic assemblies that contribute to the formation of anisotropic inorganic particles.

Talham, Daniel R.↗

Gravitational Effects on Distortion in Sintering

During sintering a powder compact gains strength through low-temperature interparticle bonding, usually induced by solid-state surface diffusion, followed by further strength contributions from high-temperature densification. In cases where a liquid phase forms, sintering densification is accelerated and shape retention is sustained while open pores remain and contribute capillary forces. Unfortunately, sintering densification requires the compact become thermally softened to a point where creep strain rates reach levels near 10(exp -2)/s when the liquid forms. On the other hand, thermal softening of the powder compact substantially reduces the strength at high temperatures. Therefore, the in situ strength evolution during sintering is a primary focus to separate compact densification (as required for high performance) with minimized distortion (as required for net-shaping). With respect to gravitation effects on distortion during sintering there are two points of substantial weakness - prior to significant interparticle bonding and during final pore closure. This research is focused on understanding the competition among interparticle neck growth, densification, thermal softening, grain boundary wetting, capillary effects associated with liquid wetting and residual porosity, and gravity. Most surprising is the apparent role of gravity, where the deviatoric stress acting on the powder structure induces skeletal formation that reduces distortion. In contrast with theory, microgravity samples exhibit more distortion yet fail to fully densify. Results are presented on the experimental concepts supporting an emerging model of sintering strength evolution that enables understanding of both distortion and densification. The experiments have relied on tungsten heavy alloys, various combinations of dihedral angle, pore size, initial porosity, liquid:solid ratio, and heating rates. On Earth, the dominant factor with respect to distortion is the starting body heterogeneity. Current modeling efforts are seeking some means to uniformly predict the distortion based on a starting pore structure heterogeneity parameter. Densification is largely unaffected by the initial pore structure, but distortion is highly variable, suggesting that nonuniform pore closure might be a significant parameter during sintering. With respect to flight experiments, plans include removal of the solid body forces acting on the solid grains, allowing stabilization of the pore structure and examination of the buoyancy effects with regard to distortion. In microgravity there is the surprising result that compacts do not densify, yet distort a factor that is contrary to all current sintering models. Densification without distortion during liquid phase sintering was achieved by manipulating microstructure and its evolution during sintering. Microstructure parameters such as the solid volume fraction, dihedral angle, initial porosity, and pore size were varied to measure densification and distortion behavior during LPS using W-Ni-Cu alloys. Green compacts were formed using ethylene-bis-stearamide as a pore-forming agent with the amount of polymer controlling the initial porosity. Different initial pore sizes were generated by varying the polymer particle size. Dihedral angle was varied by changing the Ni:Cu ratio in the alloys. Finally, the solid volume fraction was adjusted via the tungsten content. Distortion was quantified using profiles determined with a coordinate measuring machine to calculate a distortion parameter. Sintering results showed that solid volume fraction and dihedral angle are the dominant factors on densification and distortion during liquid phase sintering. Distortion decreases with increasing solid volume fraction and dihedral angle, while initial porosity and pore size have no observable effect on distortion at nearly full densification. Various strategies emerge to improve distortion control in liquid phase sintering.

German, Randall M.↗