Investigation of the solidification, structure and properties of eutectic alloys including consideration of properties control
Solidification structure and properties of eutetic alloys
Hertzberg, R. W.↗
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Investigation of the solidification, structure and properties of eutectic alloys including consideration of properties control
Solidification, structure, and properties of eutectic alloys including consideration of properties control
Kraft, R. W.↗
Containerless undercooling and solidification of bulk metastable Nb3Ge alloys
Experiments using containerless undercooling and low-gravity solidification of Nb(1-x)Ge(x) alloys for x=0.13-0.27 have been carried out in a 32-m drop-tube apparatus to study the feasibility of forming metastable Nb3Ge in bulk form. It is found that bulk samples (2-3 mm diam) of Nb-Ge alloys with 18-22% Ge can be undercooled by large amounts (300-500 K) and solidified in a containerless environment. Subsequent quenching of the solidified samples in oil helps preserve the metastable A-15 phase by removing the latent heat of fusion and quickly cooling the samples to a stable temperature below 1000 C. Even at an undercooling of less than 100 K, the superconducting transition temperature of the material is enhanced over the cast material by about 1 K.
Lacy, L. L.↗
Microgravity containerless processing in long drop tubes
Extensive experience in utilizing long drop tubes for studying effects of microgravity on the solidification of alloys was obtained. While some modifications are necessary to improve versatility, the facility proved to be most useful. Both an electron beam furnace and an electromagnetic levitation furnace can be used. The electron beam furnace is used with vacuum environments (0.00001 torr), whereas the levitation furnace is presently used only in inert gas environments (above 100 torr). Experiments are best applied to refractory alloys because of the sensitivity of the detectors now being used to observe solidification. Processing of lower melting point metals and alloys simply cannot be recorded. On the other hand, expected improvements in detector sensitivity will allow experimentation with relatively low melting alloys. In such cases, solidification will occur in flight only if higher inert gas pressure is used (100 to 760 torr) to increase heat loss by convection. Under these conditions microgravity conditions no longer apply. However, as shown by results to date, it is not microgravity as such that is important in drop tube solidification. Instead it is the containerless nature of the process that is significant, leading to large degrees of undercooling before solidification and therefore to unique alloys.
Bayuzick, R. J.↗
Growth of Metastable Peritectic Alloys
Effects of directional solidification on microstructural, compositional, and magnetic properties studied. Two reports describe experiments to determine effects of directional solidification on peritectic alloys. Of particular interest were effects of gravitationally driven convection.
Larson, David J., Jr.↗
Undercooling, Liquid Separation and Solidification of Cu-Co Alloys
Large undercooling can induce not only various solidification pathways, but also a precursor reaction, or liquid separation. This paper deals with the latter effect of undercooling using examples of the Cu-Co system which has a flattened liquidus. Bulk Cu-Co alloys (about 7mm diameter) at compositions ranging from 10 to 90 wt pct Co were highly undercooled using a fluxing technique. Except for Cu-90 wt pct Co, liquid separation was directly observed as undercooling exceeded a critical value depending on the composition. It was also confirmed by a microstructural transition from dendrites to droplets above the critical undercooling. Finally, theoretical calculations regarding the metastable miscibility boundary and maximum droplet radius were made to analyze the experimental results.
Robinson, M. B.↗
Open-source Numerical Modeling of Solidification Cracking Susceptibility: Application to Refractory Alloy Systems
Introduction. Alloys such as aluminum, nickel-base, and austenitic stainless steels are susceptible to solidification cracking during welding and 3D printing. Compositional optimization is one method used to effectively mitigate solidification cracking of those alloy systems. With the surge in hypersonic and in-space propulsion activities, refractory metals (Nb, Mo, Ta, W, and Re) and their alloy derivatives are increasing in importance due to their extreme high melting point and retention of high-temperature strength; however, their chemistry was most typically optimized to promote ductility during mechanical operations such as drawing and forming. Welding of such alloys has been a challenge due to a number of issues including solidification cracking, atmospheric contamination (O, C, and N), as well as a shift in ductile-to-brittle transition to higher temperature following grain growth induced by welding. Compositional optimization of refractory alloys for solidification cracking resistance in particular is desirable as their usage increases with the advent of advanced manufacturing methods such as 3D printing. This work evaluates the effect of compositional variation in refractory metal systems on the solidification cracking susceptibility with the goals of optimizing existing alloys and joining process techniques, and formulating new alloys with increased solidification cracking resistance. Experimental Procedures. A python code was developed in a Jupyter notebook environment (Michael and Sowards, 2023) to facilitate the calculation of crack susceptibility index proposed by Kou (2015). Composition is entered as a single point, or as a 1-D or 2-D array. The notebook calls pycalphad (Otis and Liu, 2017 and Bocklund et al, 2020) to calculate the evolution of fraction solid as a function of temperature (under either Scheil or equilibrium assumptions) and then evaluates steepness of the fraction solid curve near the terminal stage of solidification to predict solidification cracking resistance. Open source thermodynamic databases available at online repositories are used (van de Walle). The process is setup in an automated fashion to generate plots that show variation in solidification cracking susceptibility according to composition on 1-D line plots or 2-D contour plots. The Jupyter notebook and crack susceptibility algorithm was also integrated with a widely used commercial CALPHAD code for validation and alloy exploration. Results and Discussion. The crack susceptibility model was first validated against a series of refractory alloy compositions evaluated in past work which utilized a specialized Varestraint test built inside a vacuum chamber environment (Lessman and Gold, 1971). The alloys tested in the Varestraint apparatus included T-111 (Ta-8W-2Hf), ASTAR-811C (Ta-8W-1Re-0.7Hf-0.025C), FS-85 (Nb-27Ta-10W-1Zr), T-222 (Ta-9.6W-2.4Hf-0.01C), Ta-10W, B-66 (Nb-5Mo-5V-1Zr), and SCb-291 (Nb-10W-10Ta). The initial test of the model showed a strong correlation with empirical Varestraint data, i.e., a Spearman rank correlation between model predictions and hot cracking measurements was observed to be greater than 0.8. Following the validation, a set of refractory metal binary mixtures was investigated to evaluate sensitivity of Nb, Mo, W, and Ta to C, N, and O content. A series of plots were produced that suggest ppmw ranges of C, N, and O where solidification cracking increases significantly and reaches a maximum. Also comparative ranking of each primary refractory metal to each interstitial was produced. For example C produces greater cracking response in Mo whereas O produces greater cracking response in Ta and Nb. Such compositional values have utility in setting limits on pickup of these interstitial elements during welding and printing rather than using a one-size-fits-all approach. Furthermore, the results have use in determining additive powder recycling requirements, which is especially pertinent for refractory metal powders due to their high cost compared to conventional alloys. Another application created thousands of hypothetical alloys within the nominal specified composition range of two widely used refractory alloys C103 (Nb-10Hf-1Ti) and TZM (Mo-0.5Ti-0.1Zr). The cracking index was calculated for the alloys and results were fed into machine learning regression techniques including Multiple Linear Regression, Ridge Regression, and Lasso Regression to determine relative potency each alloying element had on computed solidification cracking index. A series of linear equations were produced that relate composition of C103 and TZM to solidification cracking index. The crack susceptibility of C103 for example is described by an equation of the form: cracking index ~ O + 0.667*C + 0.635*N + 0.00037*Ta – 0.0008*Hf (in wt.%) From that equation, it is clear that O has strong propensity to induce solidification cracking. Interestingly, Hf is shown to reduce calculated cracking response. Finally, realizing the potential of this method to discover new refractory alloy formulations across the period table that have low solidification cracking sensitivity, the code was applied to new untested alloy systems including W-Zr-C, W-Ta-C, and others. Conclusions. In summary, an open source numerical method has been developed using Python code to calculate Kou’s crack susceptibility index. The method was applied to refractory metals which are inherently difficult to study from a weldability testing standpoint since inert shielding gas is not sufficient and welding is typically done in vacuum, especially in light of findings presented here where oxygen has profound influence on solidification cracking. This work revealed the effect of compositional variations on a series of refractory metals and showed the framework defined here will be useful in 1) the development of new alloys that have improved weldability and 3D printability, 2) placing compositional limits on existing alloys, and 3) ensuring adequate controls of manufacturing processes such as 3D printing where powder reuse is critical. Keywords. pycalphad; Python; refractory metals; solidification cracking. References. B. Bocklund et. al. (2020) http://doi.org/10.5281/zenodo.3630657. S. Kou. (2015) https://doi.org/10.1016/j.actamat.2015.01.034. G.G. Lessmann and R.E. Gold. Welding Journal, issue 1, pp. 1-s – 8-s (1971). F.N. Michael and J.W. Sowards. NASA/TM-20230002218 (2023). R. Otis and Z.-K. Liu. (2017) http://doi.org/10.5334/jors.140. A. Van de Wallle et. al. (2018) https://doi.org/10.1016/j.calphad.2018.04.003.
pycalphad↗
Directional solidification and characterization of near eutectic Sm2CO17/Co alloys
The effects of directional solidification processing on the microstructural, compositional, and magnetic properties of near eutectic Co-Sm alloys (about 9 at. pct Sm) have been studied. Initial investigations have been performed at modest thermal gradients in the liquid, G(L) less than 60 C/cm and over a range of furnace (solidification) velocities, V = 0.8 45.4 cm/h. The primary dendrite spacing for near eutectic Sm2Co17/Co scaled with 1/sq rt V and varied from about 50 microns for V greater than or equal to 20 cm/h to hundreds of microns for V less than 10 cm/h, while the rod eutectic diameter and interrod spacing were an order of magnitude smaller. For both dendritic and cooperative growth, the associated permanent magnet properties were rather poor, e.g., remanence less than 4 kG and coercive force less than 1 kOe for the smallest dendrite and rod diameter dimensions encountered, although the magnetic hardness for the rod eutetic was larger than for the dendritic microstructure. Magnetization as a function of sample orientation indicated that the easy axis of magnetization was primarily along the direction of solidification for both ferromagnetic phases.
Pirich, Ronald G.↗
An Implicit Approach to Phase Field Modeling of Solidification for Additively Manufactured Alloys [Slides]
We are leveraging modern algorithms and computational science to provide a route to predictive simulation of microstructure evolution on emerging exascale architectures. We are utilizing the fastest supercomputers in the world for modeling and simulation of microstructure evolution for generation of data under AM conditions. Solidification conditions in AM can be tailored for the reliable design of materials to specific performance requirements. Developing computational tools to further characterize alloys and correlate the processing-structure-properties-performance (PSPP) relationship.
36 MATERIALS SCIENCE↗
Isothermal solidification for high-entropy alloy synthesis
Kinetically trapping the high-temperature states through rapid cooling solidification is widely used for the synthesis of high-entropy alloys (HEAs), especially those with intrinsically immiscible elemental combinations. However, strategies need to be developed to overcome the fundamental limitations of rapid cooling solidification in controlling the crystallinity, structure and morphology of HEAs. Here, in this study, we introduce an isothermal solidification strategy for the synthesis of HEAs by rapidly altering the metal alloy composition through liquid–liquid interface reactions at low temperatures, for example, from 25 °C to 80 °C. We use gallium (Ga)-based metal as the sacrificial reagent and mixing medium. By directing the reactions to the interfaces between the Ga-based liquid metal and an aqueous metal ion solution, the foreign metal ions can be reduced at the interfaces and incorporated into the liquid metal quickly. HEAs with various crystallinity (single crystal, mesocrystal, polycrystal and amorphous), morphology (zero, two and three dimensions) and compositions can be achieved through the isothermal solidification. Ga can be completely consumed, resulting in Ga-free HEAs. If desired, Ga can be one of the metal elements in the final products. In situ liquid phase transmission electron microscopy (TEM) studies and theoretical analysis show the isothermal solidification mechanisms. Our direct observations show the enhanced mixing of liquid metal elements and the solidification process with fluctuating nucleation dynamics. The isothermal solidification marks a powerful strategy for HEA synthesis through an unexplored pathway of kinetically trapping the high-entropy states.
Zhang, Qiubo [Lawrence Berkeley National Laborator↗
Controlled Parametric Forcing During Directional Solidification of a Bulk Organic Alloy Under Microgravity
The response of dendritic microstructures to step-like pulling velocity conditions is investigated using microgravity directional solidification experiments conducted on DECLIC-DSI combined with phase-field simulations. Under a constant pulling velocity of 1.5 µm/s, the evolution toward steady-state growth is characterized in terms of primary spacing, dendrite drift, and tip dynamics. For the first time, side-view observations enabled direct measurement of tip radius and sidebranching frequency. When step-like oscillations of the pulling velocity are imposed, the dendritic array exhibits a strongly period-dependent response: short periods lead to rapid tip adaptation, whereas longer periods induce a phase lag between tip position and morphology, resulting in progressive tip flattening and, above a critical period, interface destabilization and dendrite splitting. Quantitative phase-field simulations, including a realistic thermal field and stochastic noise, reproduce the experimental observations and provide insight into the governing mechanisms, highlighting the role of characteristic relaxation times, sequence-dependent effects, and the irreversible reorganization of the microstructure following splitting.
Microgravity↗
The solidification under zero gravity conditions of binary alloys exhibiting solid state immiscibility
The solidification behavior of gold-silicon alloys containing up to 25 at. % silicon was studied, and a mathematical model of gravity segregation during solidification was developed. A background of knowledge is provided which can be used in the design of zero gravity solidification experiments to be carried out in the 300-ft drop tower, in Aerobee rockets and in future space missions. Such experiments are needed to develop the basic scientific knowledge required for the design of economically viable space manufacturing processes. Some preliminary zero gravity experiments were carried out on a gold-25 at. % silicon alloy using the drop tower facility.
Johnson, A. A.↗
Low-Gravity Alloy Studies on Aircraft
Controlled solidification continued through many dives. Since each dive gives 20 to 30 seconds in which gravity is 0.001 to 0.1 its normal value, and aircraft may make about ten low-gravity maneuvers in mission, technique allows substantial time to conduct a low-gravity experiment. In directional solidification, liquid/solid interface advanced slowly through rod of sample alloy. Solidification continues during several aircraft maneuvers. Known solidification rate of sample correlated with accelerometer data to find gravity value during solidification for any point in sample. Thermal gradient and solidification rate controlled independently.
Curreri, P. A.↗
Containerless processing and rapid solidification of Nb-Si alloys in the niobium-rich eutectic range
Containerless processing and rapid solidification techniques were used to process Nb-Si alloys in the Nb-rich eutectic range. Electromagnetically levitated drops were melted and subsequently splat-quenched from different temperatures. A variety of eutectic morphologies was obtained as a function of the degree of superheating or undercooling of the drops prior to splatting. Metallic glass was observed only in drops quenched from above the melting temperature. Microstructures of splats deeply undercooled prior to quenching were very fine and uniform. These results are discussed in terms of classic nucleation theory concepts and the expected heat evolution at different regions of the splat during the rapid quenching process. The locations of the coupled-zone boundaries for the alpha-Nb + Nb3Si eutectic are also suggested.
Hofmeister, W. H.↗
Investigation of compositional segregation during unidirectional solidification of solid solution semiconducting alloys
Compositional segregation of solid solution semiconducting alloys in the radial direction during unidirectional solidification was investigated by calculating the effect of a curved solid liquid interface on solute concentration at the interface on the solid. The formulation is similar to that given by Coriell, Boisvert, Rehm, and Sekerka except that a more realistic cylindrical coordinate system which is moving with the interface is used. Analytical results were obtained for very small and very large values of beta with beta = VR/D, where V is the velocity of solidification, R the radius of the specimen, and D the diffusivity of solute in the liquid. For both very small and very large beta, the solute concentration at the interface in the solid C(si) approaches C(o) (original solute concentration) i.e., the deviation is minimal. The maximum deviation of C(si) from C(o) occurs for some intermediate value of beta.
Wang, J. C.↗
Influence of low-gravity solidification on heterogeneous nucleation in stable iron-carbon alloys
The effect of gravity on the processes of nucleation and growth of Fe-C alloys during directional solidification was investigated in experiments in which inoculated and uninoculated samples of an alloy of the gray iron type were solidified on ground (1 g) and under the low-gravity (low-g) and high-gravity (high-g) conditions obtained by aircraft parabolic flights. It was found that a higher number of grains was obtained during solidification in high-g condition, due to higher convection in high-g. It was demonstrated that grain multiplication due to convection can contribute up to 23 percent of the total number of grains resulting from heterogeneous nucleation of uninoculated samples. For the case of inoculated samples, it was found that the contribution of the convection-induced nucleation can be as high as 30 percent, but can be zero at very low or very high grain numbers.
Tian, Huameng↗
An evaluation of the benefits of utilizing rapid solidification for development of 2XXX (Al-Cu-Mg) alloys
The advantages of rapid solidification processing over ingot metallurgy processing in the development of 2XXX aluminum alloy compositions were evaluated using a similarly processed ingot metallurgy (IM) control alloy. The powder metallurgy (PM) alloy extrusions showed a reduced age-hardening response in comparison with similar IM compositions, with higher tensile properties for naturally aged extrusions but lower properties for artificially aged ones. However, the tensile properties of naturally and artificially aged PM alloy extrusions based on a version of IM 2034 alloy, but containing 0.6 weight percent zirconium, were comparable to those of the IM control extrusions and had significantly superior combinations of strength and toughness. The tensile properties of this PM alloy showed even greater advantage in 6.4-mm (0.25-in.) and 1.8-mm (0.070-in.) plate and sheet, the yield strength being about 68 MPa (10 ksi) greater than reported values for the IM 2034 alloy sheet. An artificially aged PM alloy based on 2219 alloy also showed a strength and strength-toughness combination comparable to those of the PM Al-Cu-Mg-Zr alloy, substantially outperforming the IM 2219 alloy. These results show that rapid solidification offers the flexibility needed to modify conventional IM compositions to produce new alloy compositions with superior mechanical properties.
Paris, H. G.↗
Investigation of the solidification, structure and properties of eutectic alloys including consideration of properties control Second semiannual progress report
Solidification, structure, and mechanical and physical properties of controlled eutectic alloys
PHYSICAL PROPERTY↗