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At least 703 records · Page 39

Direct Observation of Pore Formation and Bubble Mobility during Controlled Melting and Resolidification in Microgravity

Detailed studies on the controlled melting and subsequent re-solidification of succinonitrile were conducted in the microgravity environment aboard the International Space Station (ISS) using the PFMI apparatus (Pore Formation and Mobility Investigation) located in the ISS glovebox facility (GBX). Samples were initially prepared on ground by filling glass tubes, 1 cm ID and approximately 30 cm in length, with pure succinonitrile (SCN) under 450 millibar of nitrogen. During Space processing, experimental parameters like temperature gradient and translation speed, for melting and solidification, were remotely monitored and controlled from the ground Telescience Center (TSC) at the Marshall Space Flight Center. Real time visualization during controlled melting revealed bubbles of different sizes initiating at the solid/liquid interface, and traveling up the temperature gradient ahead of them. Subsequent controlled re-solidification of the SCN revealed the details of porosity formation and evolution. A preliminary analysis of the melt back and re- solidification and its implications to future microgravity materials processing is presented and discussed.

Grugel, Richard N.↗

Grain Structure Evolution in Fe-6Si During Directed Energy Deposition

The purpose of this study is to explore the effect of additive manufacturing (AM) process variables on the grain structure of Fe-6Si, a soft-magnetic alloy used in electrical machine and grid applications. Samples were fabricated with laser engineered net shaping (LENS) with varying inter-pass timing and numbers of unidirectional passes. Here the results show that the grain structure was affected by both solidification and solid-state grain growth mechanisms. A model of the LENS process suggests that, although shorter inter-pass times encourage greater nucleation of new grains and therefore grain refinement during solidification, these conditions also help maintain high solid-state temperatures that allow for grain boundary motion to keep pace with the build rate. Grains formed under these conditions may span multiple layers, and the high-temperature gradient promotes directional growth. This new understanding of these microstructure evolution mechanisms will aid in using process conditions to control the competition between solidification and solid-state grain growth to create grain structures that may not be possible with conventional processing.

36 MATERIALS SCIENCE↗

In-Operando Study of Shape Retention and Microstructure Development in a Hydrolyzing Sol–Gel Ink during 3D-Printing

3D printing of amorphous and crystalline ceramics is of paramount importance for the fabrication of a wide range of devices with applications across different technology fields. Printed ceramics are remarkably enabled by the sol-gel synthesis method in conjunction with continuous filament direct ink writing. During printing, multiple processes contribute to the evolution of inks including shape retention, chemical conversion, solidification, and microstructure formation. Traditionally, depending on the ink composition and printing environment, several mechanisms have been associated with the shape retention and solidification of 3D printed structures: gelation, rapid solvent evaporation, energy-driven phase transformation, and chemical-driven phase transformation. Understanding the fundamental differences between these mechanisms becomes key since they strongly influence the spatiotemporal evolution of the materials, as the out-of-equilibrium processes inherent to the extrusion, relaxation, and solidification of printed materials have significant effects on the materials properties. Herein, we investigate the shape retention mechanism and the hydrolysis-induced material conversion and microstructure formation during the 3D printing of a water reactive sol-gel ink that transforms into titanium dioxide-based ceramic. This study aims at identifying characteristic mechanisms associated with the material transformation, establishing connections between the microstructure development and the timescales associated with solidification under operando 3D-printing conditions. The investigation of this material's out-of-equilibrium pathways under processing conditions is enabled by time-resolved coherent X-ray scattering, providing simultaneous access to temporospatially resolved microstructural and dynamics information. Furthermore, we explore X-ray speckle tracking as a tool to resolve deformations of the microstructure in a printed filament associated with the deposition of consecutive filaments. Through this work, we aim at providing a fundamental understanding of the relationships behind these transformative processes in 3D printing and their timescales as the basis for achieving unprecedented control over printed materials microstructure.

36 MATERIALS SCIENCE↗

Droplet Growth in Undercooled Cu-Co Alloys

High undercooling usually leads to the refinement of microstructures, while an opposite tendency occurs in liquid immiscible alloys. In the Cu-Co system, there is a metastable liquid miscibility gap which may allow the study of droplet nucleation and growth by undercooling experiments. In the present work, two alloys of Cu50Co50 and Cu68Co32 (atomic) were undercooled using a melt fluxing technique in which the liquid separation temperature could be directly measured. It was observed that after separation the resultant melts were further undercooled by 315 K prior to solidification. The relationship between the largest droplet radius and undercooling was found to exhibit three regimes: a power law growth, linear growth, and saturation stage. In addition to dendrites and droplet-like morphology reported previously, an interconnected structure was formed for the Cu50Co50 alloy at intermediate undercooling. It played a crucial role in droplet coarsening at high undercooling.

Robinson, Michael B.↗

Interface morphology and dislocation-mediated processes during rapid solidification of thin films

Rapid solidification experiments have, in recent years, revealed a wealth of new microstructural phenomena that suggest a strong connection between the kinetics of solidification and the crystalline structures that emerge as a result. In this work, we investigate the interplay between interface morphology and defect-mediated processes during rapid solidification conditions using a Phase Field Crystal (PFC) model, enabling us to simultaneously and efficiently explore the physics of solidification and elasto-plasticity in the formalism of a single-field theory. We predict that there are two mechanisms by which dislocations emitted directly from the solid–liquid interface induce orientation gradients as well as the formation of subgrain boundaries within a single solidifying cell. We relate these mechanisms to the morphology of the moving solid–liquid interface and identify a suitable control parameter in the PFC model with which we can go between said morphologies by effectively changing the relative strength of the capillary length and kinetic coefficients of the solid–liquid interface. Thus, we are able to provide mechanistic explanations for several microstructural features (with an emphasis on orientation gradients and subgrain boundaries) observed during the rapid solidification of pure materials. We also provide a simple explanation for the formation of “jagged” subgrain boundaries, which is consistent with our experimental observations in rapidly solidified samples of Aluminum, whose mechanisms have thus far been unknown.

Interface morphology↗

Microstructural evolution, defect mitigation, and precipitation behavior in AA6061 via laser powder bed fusion with high-temperature substrate heating

Defects, particularly solidification cracking, remain persistent challenges in the laser powder bed fusion (LPBF) processing of AA6061 aluminum alloy. This study systematically investigates defect mitigation, microstructural evolution, and mechanical properties associated with high-temperature substrate preheating at 500 °C. Comprehensive microstructural analyses, including characterization of defects, grain structures, and precipitation behavior, were performed on samples in both as-built and T6 heat-treated states. Elevated preheating substantially reduced solidification cracking across a wide processing window, while demonstrating decreased crack sensitivity to laser parameters. Columnar cracks along the build direction were observed despite substrate preheating. Lack-of-fusion and keyhole porosity were effectively eliminated, though gas-induced microporosity persisted at higher powers. In-depth characterization of two distinct laser power and speed conditions confirmed the formation of micron-sized, non-coherent Mg 2 Si precipitates under heated substrate conditions, alongside α-AlFeCrMnSi intermetallic phases indicative of in-situ thermal effects during fabrication. Subsequent T6 heat treatment revealed the formation of fine, coherent needle-shaped β″ strengthening precipitates. Despite substantial differences in processing parameters, comparable mechanical properties were measured in the as-built samples (∼52 MPa yield strength, ∼130 MPa tensile strength), primarily due to reduced strain hardening effects and consistent precipitation characteristics. Meanwhile, the T6 heat treatment led to significant improvement in properties, enhancing yield strength by over 400%, aligning closely with the performance of conventional wrought AA6061-T6. These findings underscore that high-temperature substrate preheating offers an effective means to suppress cracks, control precipitation, and enhance mechanical performance in LPBF-processed AA6061.

36 MATERIALS SCIENCE↗

Magnetic Field Suppression of Flow in Semiconductor Melt

One of the most promising approaches for the reduction of convection during the crystal growth of conductive melts (semiconductor crystals) is the application of magnetic fields. Current technology allows the experimentation with very intense static fields (up to 80 KGauss) for which nearly convection free results are expected from simple scaling analysis in stabilized systems (vertical Bridgman method with axial magnetic field). However, controversial experimental results were obtained. The computational methods are, therefore, a fundamental tool in the understanding of the phenomena accounting during the solidification of semiconductor materials. Moreover, effects like the bending of the isomagnetic lines, different aspect ratios and misalignments between the direction of the gravity and magnetic field vectors can not be analyzed with analytical methods. The earliest numerical results showed controversial conclusions and are not able to explain the experimental results. Although the generated flows are extremely low, the computational task is a complicated because of the thin boundary layers. That is one of the reasons for the discrepancy in the results that numerical studies reported. Modeling of these magnetically damped crystal growth experiments requires advanced numerical methods. We used, for comparison, three different approaches to obtain the solution of the problem of thermal convection flows: (1) Spectral method in spectral superelement implementation, (2) Finite element method with regularization for boundary layers, (3) Multiquadric method, a novel method with global radial basis functions, that is proven to have exponential convergence. The results obtained by these three methods are presented for a wide region of Rayleigh and Hartman numbers. Comparison and discussion of accuracy, efficiency, reliability and agreement with experimental results will be presented as well.

Fedoseyev, A. I.↗

3D Characterization of the Columnar-to-Equiaxed Transition in Additively Manufactured Inconel 718

Additive manufacturing (AM) provides enormous processing flexibility, enabling novel part geometries and optimized designs. Access to a local heat source further permits the potential for local microstructure control on the scale of individual melt pools, which can enable local control of part properties. In order to design tailored processing strategies for target microstructures, models predicting the columnar-to-equiaxed transition must be extended to the high solidification velocities and complex thermal histories present in AM. Here, we combine 3D characterization with advanced modeling techniques to develop a more complete understanding of the solidification process and evolution of microstructure during electron beam melting (EBM) of Inconel 718. Full calibration of existing microstructure prediction models demonstrates the differences between AM processes and more conventional welding techniques, underlying the need for accurate determination of key parameters that can only be measured directly in 3D. The ability to combine multisensor data in a consistent 3D framework via data fusion algorithms is essential to fully leverage these advanced characterization approaches. Thermal modeling provides insight on microstructure development within isolated solidification events and demonstrates the role of Marangoni effects on controlling solidification behavior.

Polonsky, Andrew↗

Reduced gravity favors columnar crystal growth

In zero gravity, alined columnar microstructures form at expense of equiaxed growth. Preferential crystal growth occurs in solidification chamber consisting of semicylindrical copper chill block brazed to stainless steel top plate. Method is best utilized in castings where directional dependence of physical properties is beneficial, as in turbine blades.

Kattamis, T. Z.↗

Evolution of dislocations during the rapid solidification in additive manufacturing

Materials processed by fusion-based additive manufacturing (AM) typically exhibit relatively high dislocation densities, along with cellular structures and elemental segregation. This representative structural feature significantly influences material performance; however, post-mortem microstructure characterizations of AM materials cannot capture the dynamic evolution of dislocations during the manufacturing process, thereby offering limited mechanism-based guidance for further advancing AM techniques and facilitating the qualification and certification of AM products. In this study, we conduct operando high-energy synchrotron X-ray diffraction experiments on wire-laser directed energy deposition of 316 L stainless steel. Through a unique configuration, our operando synchrotron experiments semi-quantitatively probe the dislocation density in solid phases and their dynamic changes during solidification and subsequent cooling. By integrating this advanced synchrotron technique with multi-physics simulation, in-situ neutron diffraction, and multi-scale electron microscopy characterization, our mechanistic study aims to elucidate the effects of rapid cooling and subsequent thermal cycling on the dislocation generation and evolution.

36 MATERIALS SCIENCE↗

Effects of Traveling Magnetic Field on Dynamics of Solidification

The Lorentz body force induced in electrically conducting fluids can be utilized for a number of materials processing technologies. An application of strong static magnetic fields can be beneficial for damping convection present during solidification. On the other hand, alternating magnetic fields can be used to reduce as well as to enhance convection. However, only special types of time dependent magnetic fields can induce a non-zero time averaged Lorentz force needed for convection control. One example is the rotating magnetic field. This field configuration induces a swirling flow in circular containers. Another example of a magnetic field configuration is the traveling magnetic field (TMF). It utilizes axisymmetric magnetostatic waves. This type of field induces an axial recirculating flow that can be advantageous for controlling axial mass transport, such as during solidification in long cylindrical tubes. Incidentally, this is the common geometry for crystal growth research. The Lorentz force induced by TMF can potentially counter-balance the buoyancy force, diminishing natural convection, or even setting up the flow in reverse direction. Crystal growth process in presence of TMF can be then significantly modified. Such properties as the growth rate, interface shape and macro segregation can be affected and optimized. Melt homogenization is the other potential application of TMF. It is a necessary step prior to solidification. TMF can be attractive for this purpose, as it induces a basic flow along the axis of the ampoule. TMF can be a practical alloy mixing method especially suited for solidification research in space. In the theoretical part of this work, calculations of the induced Lorentz force in the whole frequency range have been completed. The basic flow characteristics for the finite cylinder geometry are completed and first results on stability analysis for higher Reynolds numbers are obtained. A theoretical model for TMF mixing is also developed. In the experimental part, measurements of flow induced by TMF in a column of mercury (Hg) are presented. Also, an alloy mixing of Bi-Sn of the eutectic composition is demonstrated. A traveling magnetic field of 4mT at 3kHz applied for 120 minutes is found to be sufficient to homogenize an alloy enclosed in a 1cm diameter and 12 cm long tube.

Source record↗

Alloy and structural optimization of a directionally solidified lamellar eutectic alloy

Mechanical property characterization tests of a directionally solidified Ni-20 percent Cb-2.5 percent Al-6 percent Cr cellular eutectic turbine blade alloy demonstrated excellent long time creep stability and indicated intermediate temperature transverse tensile ductility and shear strength to be somewhat low for turbine blade applications. Alloy and structural optimization significantly improves these off-axis properties with no loss of longitudinal creep strength or stability. The optimized alloy-structure combination is a carbon modified Ni-20.1 percent Cb-2.5 percent Al-6.0 percent Cr-0.06 percent C composition processed under conditions producing plane front solidification and a fully-lamellar microstructure. With current processing technology, this alloy exhibits a creep-rupture advantage of 39 C over the best available nickel base superalloy, directionally solidified MAR M200+ Hf. While improved by about 20 percent, shear strength of the optimized alloy remains well below typical superalloy values.

Sheffler, K. D.↗

Effect Of Solidification Speed On Fatigue Properties

Fast solidification increases fatigue life, but failure distribution becomes less predictable. Report describes effects of rate of solidification on nickel-based super-alloy MAR-M246(Hf) used in turbine blades. Based on experiments in which specimens directionally solidified at 5 cm/h and 30 cm/h, then tested for high cycle fatigue. Specimens also inspected by energy-dispersive x-ray (EDX) analysis and optical and electron microscopy.

Mccay, M. H.↗

Dendritic solidification of alloys in low gravity

The effect of low gravity during solidification on primary and secondary dendrite spacings is investigated. Dendritic spacing data for iron-carbon-type alloys and superalloys which were directionally solidified during aircraft low-g trajectories are examined. The low-g data data are compared with data for metal model materials and binary alloys, and theoretical models to explain the dendritic spacing are considered.

Curreri, P. A.↗

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.↗

Overview of NASA's Microgravity Materials Research Program

The NASA microgravity materials program is dedicated to conducting microgravity experiments and related modeling efforts that will help us understand the processes associated with the formation of materials. This knowledge will help improve ground based industrial production of such materials. The currently funded investigations include research on the distribution of dopants and formation of defects in semiconductors, transitions between columnar and dendritic grain morphology, coarsening of phase boundaries, competition between thermally and kinetically favored phases, and the formation of glassy vs. crystalline material. NASA microgravity materials science investigators are selected for funding either through a proposal in response to a NASA Research Announcement or by participation in a team proposing to a foreign agency research announcement. In the latter case, a US investigator participating in a successful proposal to a foreign agency can then apply to NASA for funding of an unsolicited proposal. The program relies on cooperation with other aerospace partners from around the world. The ISS facilities used for these investigations are provided primarily by partnering with foreign agencies and in most cases the US investigators are working as a part of a larger team studying a specific area of materials science. The following facilities are to be utilized for the initial investigations. The ESA provided Low Gradient Facility and the Solidification and Quench Inserts to the Materials Research Rack/Materials Science Laboratory are to be used primarily for creating bulk samples that are directionally solidified or quenched from a high temperature melt. The CNES provided DECLIC facility is used to observe morphological development in transparent materials. The ESA provided Electro-Magnetic Levitator (EML) is designed to levitate, melt and then cool samples in order to study nucleation behavior. The facility provides conditions in which nucleation of the solid is not triggered from the wall and in which fluid flows in the sample can be controlled and manipulated. These conditions allow scientists ideal conditions for understanding the relative amounts and distribution of different phases that form in the solid. Finally, the Coarsening of Solid Liquid Melts hardware allows quenching of low temperature samples in the Microgravity Science Glovebox.

Downey, James Patton↗

Eutectic superalloys strengthened by sigma, Ni3CB lamellae and gamma prime, Ni3Al precipitates

By means of a screening and solidification optimization study of certain alloys located on the gamma-sigma liquidus surface within the Ni-Cb-Cr-Al system, alloys with high temperature properties superior to those of all known superalloys were defined. One alloy, Ni - 19.7w/o Cb - 6.0w/o Cr - 2.5w/o Al, directionally solidified at 3 cm/hr met or exceeded each program goal. A second alloy, Ni-21.75 w/o Cb-2.55 w/o Al, although deficient in its inherent oxidation resistance, met the other program goals and combined a remarkable insensitivity of composite microstructure to solidification parameters with excellent low temperature toughness. This investigation demonstrated that useful properties for gas turbine airfoil application have been achieved by reinforcing a strong and tough gamma solid solution matrix containing precipitated gamma prime by a lamellar intermetallic compound Ni3 Cb having greater strength at elevated temperature.

Lemkey, F. D.↗

A Solid Case for Microgravity Processing

Solidification of metals, particularly alloys, is a complicated process. At some sufficiently high temperature, the components comprising an alloy fully mix, producing a single homogeneous liquid. Unfortunately, after this liquid is cast into a mold and allowed to freeze, the resulting solid is usually very inhomogeneous. In most cases the first solid to "freeze out" of the liquid has a composition very close to one of the pure metals. This initially solidifying metal usually comprises microscopic, pine-tree shaped components, collectively referred to as a dendritic array, whose distribution, alignment, and scale directly influence a materials strength and docility. During dendrite growth the adjacent liquid becomes enriched, and consequently, solidifies a much lower temperature and considerably later time. Thus, in the course of solidification, both the solid and the enriched liquid can have compositions (and local temperatures) significantly different from those of the bulk liquid. Different compositions and temperatures imply different densities that, in Earth's gravity, induce motion in the liquid. Such motion promotes formation of a casting that is denser at the bottom and lighter at the top. This condition known as macrosegregation, precludes optimized, uniform material properties.

Grugel, Richard N.↗