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At least 19 records

Secondary arm coarsening and microsegregation in superalloy PWA-1480 single crystals: Effect of low gravity

Single crystal specimens of nickel base superalloy PWA-1480 were directionally solidified on ground and during low gravity (20 sec) and high gravity (90 sec) parabolic maneuver of KC-135 aircraft. Thermal profiles were measured during solidification by two in-situ thermocouples positioned along the sample length. The samples were quenched during either high or low gravity cycles so as to freeze the structures of the mushy zone developing under different gravity levels. Microsegregation was measured by examining the solutal profiles on several transverse cross-sections across primary dendrites along their length in the quenched mushy zone. Effect of gravity level on secondary arm coarsening kinetics and microsegregation have been investigated. The results indicate that there is no appreciable difference in the microsegregation and coarsening kinetics behavior in the specimens grown under high or low gravity. This suggests that short duration changes in gravity/levels (0.02 to 1.7 g) do not influence convection in the interdendritic region. Examination of the role of natural convection, in the melt near the primary dendrite tips, on secondary arm spacings requires low gravity periods longer than presently available on KC-135. Secondary arm coarsening kinetics show a reasonable fit with the predictions from a simple analytical model proposed by Kirkwood for a binary alloy.

Vijayakumar, M.↗

Influence of gravity-free solidification on microsegregation

Single crystalline germanium has been grown for the first time in space aboard Skylab Mission No. 2. The crystal growth experiment, designed to characterize the influence of gravity-free solidification on microsegregation of a semiconductor material, contained three crystals. One was doped with Ga; the second with Sb; and the third with B. Portions of the germanium crystals were remelted and subsequently resolidified at 5 microns per second under controlled conditions by the gradient freeze technique. Detailed spreading resistance measurements made on the Ga doped Ge crystals indicate that microsegregation in space is reduced by two to five-fold in the bulk and eight-fold near the surface, while macrosegregation in space is reduced by six-fold in the bulk. The effective segregation coefficient for Ga in Ge was analyzed extensively and was found to be larger for space solidification. This has the implication that the solute boundary layer at the growth interface in space is correspondingly thinner. The solidification interface is significantly smoother and is found to be initially convex toward the melt in space. A convective mixing model has been advanced to explain the absence of gravity on convective mixing and solute segregation during solidification.

Yue, J. T.↗

Dentritic morphology and microsegregation in directionally solidified superalloy, PWA-1480, single crystal: Effect of gravity; center director's discretionary fund report

Primary dendrite spacings, secondary dendrite spacings, and microsegregation have been examined in PWA-1480 single crystal specimens which were directionally solidified during parabolic maneuvers on the KC-135 aircraft. Experimentally observed growth rate and thermal gradient dependence of primary dendrite spacings are in good agreement with predictions from dendrite growth models for binary alloys. Secondary dendrite coarsening kinetics show a reasonable fit with the predictions from an analytical model proposed by Kirkwood for a binary alloy. The partition coefficients of tantalum, titanium, and aluminum are observed to be less than unity, while that for tungsten and cobalt are greater than unity. This is qualitatively similar to the nickel base binaries. Microsegregation profiles experimentally observed for PWA-1480 superalloy show a good fit with Bower, Brody, and Flemings model developed for binary alloys. Transitions in gravity levels do not appear to affect primary dendrite spacings. A trend of decreased secondary arm spacings with transition from high gravity to the low gravity period was observed at a growth speed of 0.023 cm s(exp -1). However, definite conclusions can only be drawn by experiments at lower growth speeds which make it possible to examine the side-branch coarsening kinetics over a longer duration. Such experiments, not possible due to the insufficient low-gravity time of the KC-135, may be carried out in the low-gravity environment of space.

Tewari, S. N.↗

Enhancing microsegregation during rapid directional solidification through ternary microalloying

The nano-cellular dendritic microstructure formed during rapid directional solidification in powder bed fusion additive manufacturing creates unique properties such as simultaneous improvement in strength and ductility. However, process control of microsegregation features remains challenging due to low sensitivity of critical solidification mechanisms to process parameters. This study leverages microalloying to achieve large changes in dendrite composition, microstructure, and interdendritic zone width during laser powder bed fusion without modifying process parameters. CALPHAD simulations predict that the addition of Zr significantly steepens the solidus line of the dilute Cu-Cr alloy system, leading to enhanced Cr rejection into the melt and greater than 95% reduction in solubility of Cr in the solidified Cu matrix. Experimental validation using time-of-flight secondary ion mass spectrometry and Kelvin probe force microscopy reveals that the ternary alloy containing 0.01 wt% Zr exhibited wider interdendritic regions compared to the binary, a significantly higher number of Cr-rich particles within interdendritic regions, near-complete ejection of oxygen impurities from the matrix, and greater nanoscale work function contrast. These features indicate more aggressive Cr segregation in the presence of Zr and a purer Cu matrix and provide a potentially robust method for engineering the nano-cellular dendritic solidification microstructure.

CALPHAD↗

Influence of Molybdenum on Rapid Solidification Microstructure and Microsegregation in Primary Ferrite Solidified Stainless Steel

Due to the widespread use and familiarity of austenitic stainless steels in many industries these alloys are often the first materials used when adapting new processing techniques. The rapid cooling and solidification rates that occur during fusion based additive manufacturing processes like powder bed fusion cause a fundamental shift in the solidification behavior of the material. While the effects that Cr and Ni have on the microstructure have been fairly well documented across a range of solidification conditions, the impact of alloying elements like Mo are not as well understood at rapid solidification rates. For this study, four custom stainless steel alloy feedstocks were made with targeted modification of the Cr and Mo concentrations to maintain a constant Cr/Ni eq ratio of ~1.7. Two-piston splat quenching was used to produce rapidly solidified samples and the solidification mode, phase, and cell size were investigated. Solidification rates were estimated to be between 0.4 and 1.5m/s. A comparison of the microsegregation and partitioning behavior of Cr, Ni and Mo in ferrite solidified material was also performed for the different alloy compositions. Variations of the Mo concentration between each feedstock showed no measurable influence on the solidification/cooling rates, solidification morphology, or the partitioning of Mo. Furthermore, higher concentrations of Mo were found to significantly increase the amount of ferrite phase in the microstructure by suppressing the ferrite to austenite massive transformation.

36 MATERIALS SCIENCE↗

Effects of Remelting Current on Structure, Composition, Microsegregation, and Inclusions in Inconel 718 Electroslag Remelting Ingots

The macro- and microstructures, chemical compositions, microsegregations, and nonmetallic inclusion characteristics at different positions of the as-cast IN718 ingots produced by a laboratory-scale electroslag remelting (ESR) furnace under four remelting currents (150, 200, 250, and 300 A) were compared and investigated comprehensively. The results indicate that the average melting rate increases with the increasing remelting current, and the molten pool tends to be deeper. Thus, at the same position of the ESR ingots, the volume fraction of the segregated phase, the degree of elemental segregation, and the secondary dendrite arm spacing have the same tendency to increase with the increasing remelting current and show an increasing trend from the bottom to the top along the height of each ingot. If the current is set relatively low, the oxygen and nitrogen levels in the ingots increase, the conditions that make the contents and distributions of Al and Ti become unstable. In addition, the major nonmetallic inclusions in the IN718 ESR ingots are MgO·Al{sub 2}O{sub 3} complex oxide inclusions with a three-layer structure and (Nb,Ti)N nitrides. The volume fractions and mean equivalent diameters display a downward trend with the increasing remelting current. The size and quantity of these inclusions are always larger in the upper portions of the ingots than those in the lower portions.

36 MATERIALS SCIENCE↗

Microsegregation in directionally solidified Pb-8.4 at. pct Au alloy

The dependence of microsegregation behavior on growth rate and thermal gradient has been examined in a Pb-8.4 at. pct Au alloy material partially directionally solidified and quenched. The composition of the quenched 'liquid' at the dendrite tip (Ct), that of the eutectic-like solid phase freezing from the interdendritic liquid at the base of dendrite (Cse), the volume fraction of this eutectic-like region (fe), and solute profiles in the interdendritic quenched liquid and ahead of the dendrite have been measured. Two dendritic growth models for solidification of a binary alloy melt in a positive thermal gradient at the liquid-solid interface, one for dendrites with 'minimum undercooled dendrite tip' and the other for an Ivantsov type of dendrite with 'marginally stable tip', have been examined for a quantitative comparison with measured values of Ct, Cse, and fe. Convection in the melt, possibly due to horizontal density gradients, is found to be a serious limitation for theoretical understanding of the observed experimental behavior and meaningful comparison of theories.

Tewari, S. N.↗

Microsegregation during directional solidification

During the directional solidification of alloys, solute inhomogeneities transverse to the growth direction arise due to morphological instabilities (leading to cellular or dendritic growth) and/or due to convection in the melt. In the absence of convection, the conditions for the onset of morphological instability are given by the linear stability analysis of Mullins and Sekerka. For ordinary solidification rates, the predictions of linear stability analysis are similar to the constitutional supercooling criterion. However, at very rapid solidification rates, linear stability analysis predicts a vast increase in stabilization in comparison to constitutional supercooling.

Coriell, S. R.↗

Quantitative analysis of the effects of vertical magnetic fields on microsegregation in Te-doped LEC GaAs

Using near-IR transmission microscopy with computational absorption analysis, the effects of axial magnetic fields on micro- and macrosegregation during LP-LEC growth of GaAs were quantitatively investigated with a spatial resolution approaching 2 microns. Segregation inhomogeneities exceeding one order of magnitude are found to be related to fluid dynamics of the melt. The applicability of the BPS theory as well as the nonapplicability of the Cochran analysis are established.

Carlson, D. J.↗

Microstructural modification of additively manufactured metals by electropulsing

Additive manufacturing (AM) promises rapid development cycles and fabrication of ready-to-use, geometrically-complex parts. The metallic parts produced by AM often contain highly non-equilibrium microstructures, e.g. chemical microsegregation and residual dislocation networks. While such microstructures can enhance some material properties, they are often undesirable. Many AM parts are thus heat-treated after fabrication, a process that significantly slows production. This study investigated if electropulsing, the process of sending high-current-density electrical pulses through a metallic part, could be used to modify the microstructures of AM 316 L stainless steel (SS) and AlSi10Mg parts fabricated by selective laser melting (SLM) more rapidly than thermal annealing. Electropulsing has shown promise as a rapid postprocessing method for materials fabricated using conventional methods, e.g. casting and rolling, but has never been applied to AM materials. For both the materials used in this study, as-fabricated SLM parts contained significant chemical heterogeneity, either chemical microsegregation (316 L SS) or a cellular interdendritic phase (AlSi10Mg). In both cases, annealing times on the order of hours at high homologous temperatures are necessary for homogenization. Using electropulsing, chemical microsegregation was eliminated in 316 L SS samples after 10, 16 ms electrical pulses. In AlSi10Mg parts, electropulsing produced spheroidized Si-rich particles after as few as 15, 16 ms electrical pulses with a corresponding increase in ductility. Finally, this study demonstrated that electropulsing can be used to modify the microstructures of AM metals.

36 MATERIALS SCIENCE↗

Uncovering grain and subgrain microstructure at the scale of additive manufacturing melt tracks with a scalable cellular automaton solidification model

Metal additive manufacturing, characterized by rapid solidification, yields refined grains with a distinctive cellular subgrain microstructure that plays a pivotal role in determining material properties. Due to the significant computational expense demanded to simulate the required physics with submicron spatial resolution, their numerical simulations have been limited to proof-of-concept studies to either 2D or small subregions of a melt pool. In this study, an open-source, scalable, solidification code, muMatScale, based on the cellular automaton method, has been developed to predict the grain and the underlying subgrain microstructure over an entire melt pool. The model incorporates flexible parallelization schemes, utilizing MPI and OpenMP GPU Offloading, in addition to appropriate multi-physics specific to non-equilibrium rapid solidification in AM. The impact of nucleation parameters on grain microstructures was investigated with a focus on grain size variations and morphology transitions. With selected nucleation parameters, the simulation predicted the grain size, subgrain morphology, crystallographic orientation, and microsegregation aligned with experimental measurements. The model demonstrates that epitaxial grain growth is a dominant factor at the melt pool boundary, influencing grain size variation under different grain sizes in the build plate while maintaining consistent primary dendrite arm spacing under identical thermal conditions. Here, the highly efficient numerical model enables large-scale simulations with a spatial resolution of 100 nm or less, unveiling unprecedented insights into thermal and solutal diffusion driven grain growth, and the subgrains with microsegregation within grains in 3D across scales. muMatScale will enable the linking of submicron length-scale microstructure to part-level material behavior by investigating fundamental solidification problems at the intercellular scale in many-track and many-layer builds.

36 MATERIALS SCIENCE↗

Microstructural development in DED stainless steels: applying welding models to elucidate the impact of processing and alloy composition

Austenitic stainless steel microstructures produced by directed energy deposition (DED)are analogous to those developed during welding, particularly high energy density welding. To better understand microstructural development during DED, theories of microstructural evolution,which have been established to contextualize weld microstructures, are applied in this study to microstructural development in DED austenitic stainless steels. Phenomenological welding models that describe the development of oxide inclusions, compositional microsegregation, ferrite,matrix austenite grains, and dislocation substructures are utilized to clarify microstructural evolution during deposition of austenitic stainless steels. Two different alloys, 304L and 316L, arecompared to demonstrate the broad applicability of this framework for understanding microstmctural development during the DED process. Despite differences in grain morphology and solidification mode for these two alloys (which can be attributed to compositional differences),similar tensile properties are achieved. It is the fine-scale compositional segregation and dislocation structures that ultimately determine the strength of these materials. The evolution of microsegregation and dislocation structures is shown to be dependent on the rapid solidification and thermomechanical history of the DED processing method and not the composition of the starting material.

36 MATERIALS SCIENCE↗