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Microstructural changes enhance properties of alloys. Major feature of process is rapid quenching of alloys or intermetallic compounds from liquid to solid state at cooling rates of 10 to the 6th power C/s.
Recent improvements in the resolution of the X-ray Transmission Microscope (XTM) for Solidification Studies provide microstructure feature detectability down to 5 micrometers during solidification. This presentation will show the recent results from observations made in real-time of the solid-liquid interfacial morphologies of the Al-CuAI2 eutectic alloy. Lamellar dimensions and spacings, transitions of morphology caused by growth rate changes, and eutectic grain structures are open to measurements. A unique vantage point viewing the face of the interface isotherm is possible for the first time with the XTM due to its infinite depth of field. A video of the solid-liquid interfaces seen in-situ and in real-time will be shown.
Uniform microstructural development during solidification of immiscible liquids on Earth is hampered by inherent density differences between the phases. Microgravity processing minimizes settling but segregation still occurs due to gravity independent wetting and coalescence phenomena. Experiments with the transparent organic, metal analogue, succinonitrile-glycerol system were conducted in conjunction with applied ultrasonic energy. The processing parameters associated with this technique have been evaluated in view of optimizing dispersion uniformity. Experimental results to evaluate microstructural phase distributions, based on other liquid-liquid immiscibility systems, will also be presented.
Uniform microstructural distribution during solidification of immiscible liquids (e.g., oil and water; aluminum and lead) on Earth is hampered by inherent density differences between the phases. Microgravity processing minimizes settling but segregation still occurs due to gravity independent wetting and coalescence phenomena. Experiments with the transparent organic, metal analogue, succinonitrile-glycerol system were conducted in conjunction with applied ultrasonic energy. The processing parameters associated with this technique have been evaluated in view of optimizing dispersion uniformity. Characterization of the experimental results in terms of a modeling effort will also be presented,
In order to identify the possible hierarchy of microstructural pathways and transitions, a systematic evaluation of the microstructural evolution in undercooled Fe-Ni alloys was performed on uniformly processed samples covering seven orders of magnitude in volume. At appropriate undercooling levels, alternate solidification pathways become thermodynamically possible and metastable product structures can result from the operation of competitive solidification kinetics. For thermal history evaluation, a heat flow analysis was applied and tested with large Fe-Ni alloy particles (1 to 3 mm) to assess undercooling potential. Alloy powders (10 to 150 microns), with large liquid undercoolings, were studied under the same composition and processing conditions to evaluate the solidification kinetics and microstructural evolution, including fcc/bcc phase selection and the thermal stability of a retained metastable bcc phase. The identification of microstructural transitions with controlled variations in sample size and composition during containerless solidification processing was used to develop a microstructure map which delineates regimes of structural evolutions and provides a unified analysis of experimental observations in the Fe-Ni system.
The unidirectional solidification methods are zone melting, crystal pulling, Bridgemen, and slow cooling. In order to obtain excellent properties (such as transparency), pores, voids and cracks must be avoided, and elimination of such defects is described.
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The effects of gravity on the microstructure of directionally solidified near-eutectic cast irons are studied, using a Bridgman-type automatic directional solidification furnace aboard a NASA KC-135 aircraft which flies parabolic arcs and generates alternating periods of low-g (0.01 to 0.001 g, 30 seconds long) and high-g (1.8 g, 1.5 minutes long). Results show a refinement of the interlamellar spacing of the eutectic during low-g processing of metastable Fe-C eutectic alloys. Low-g processing of stable Fe-C-Si eutectic alloys (lamellar or spheroidal graphic) results in a coarsening of the eutectic grain structure. Secondary dendrite arm spacing of austenite increases in low-g and decreases in high-g. The effectiveness of low-gravity in the removal of buoyancy-driven graphite phase segregation is demonstrated.
The influence was studied of convection during directional solidification on the resulting microstructure of eutectics, specifically lead/tin and manganese/bismuth. A theory was developed for the influence of convection on the microstructure of lamellar and fibrous eutectics, through the effect of convection on the concentration field in the melt in front of the growing eutectic. While the theory agrees with the experimental spin-up spin-down results, it predicts that the weak convection expected due to buoyancy will not produce a measurable change in eutectic microstructure. Thus, this theory does not explain the two fold decrease in MnBi fiber size and spacing observed when MnBi-Bi is solidified in space or on Earth with a magnetic field applied. Attention was turned to the morphology of the MnBi-Bi interface and to the generation of freezing rate fluctuations by convection. Decanting the melt during solidification of MnBi-Bi eutectic showed that the MnBi phase projects into the melt ahead of the Bi matrix. Temperature measurements in a Bi melt in the vertical Bridgman-Stockbarger configuration showed temperature variations of up to 25 C. Conclusions are drawn and discussed.
The objective of the research is to quantitatively determine and understand the fundamental mechanisms that control the microstructural evolution during solidification of an assemblage of equiaxed dendritic crystals. A microgravity experiment will be conducted to obtain benchmark data on the transient growth and interaction of up to four equiaxed crystals of a pure and transparent metal analog (succinonitrile, SCN) under strictly diffusion dominated conditions. Of interest in the experiment are the transient evolution of the primary and secondary dendrite tip speeds, the dendrite morphology (i.e., tip radii, branch spacings, etc.) and solid fraction, the tip selection criterion, and the temperature field in the melt for a range of initial supercoolings and, thus, interaction "strengths" between the crystals. The experiment thus extends the microgravity measurements of Glicksman and coworkers for steady growth of a single dendrite [Isothermal Dendritic Growth Experiment (IDGE), first flown on USMP-2] to a case where growth transients are introduced due to thermal interactions between neighboring dendrites - a situation more close to actual casting conditions. Corresponding earth-based experiments will be conducted to ascertain the influence of melt convection. The experiments are supported by a variety of analytical models and numerical simulations. The data will primarily be used to develop and test theories of transient dendritic growth and the solidification of multiple interacting equiaxed crystals in a supercooled melt.
Gravity driven separation precludes uniform microstructural development during controlled directional solidification (DS) processing of hypermonotectic alloys. It is well established that liquid/liquid suspensions, in which the respective components are immiscible and have significant density differences, can be established and maintained by utilizing ultrasound. A historical introduction to this work is presented with the intent of establishing the basis for applying the phenomena to promote microstructural uniformity during controlled directional solidification processing of immiscible mixtures. Experimental work based on transparent organics, as well as salt systems, will be presented in view of the processing parameters.
There are many metal alloy systems that separate into two different liquids upon cooling from a higher temperature. Uniform microstructural development during solidification of these immiscible liquids on Earth is hampered by inherent density differences between the phases. Microgravity processing minimizes settling but segregation still occurs due to gravity independent wetting and coalescence phenomena. Experiments with the transparent organic, metal analogue, succinonitrile-glycerol system were conducted in conjunction with applied ultrasonic energy. The processing parameters associated with this technique have been evaluated in view of optimizing dispersion uniformity. Characterization of the experimental results in terms of an initial modeling effort will also be presented.
There are many metal alloy systems that separate into two different liquids upon cooling from a higher temperature. Uniform microstructural development during solidification of these immiscible liquids on Earth is hampered by inherent density differences between the phases. Microgravity processing minimizes settling but segregation still occurs due to gravity independent wetting and coalescence phenomena. Experiments with the transparent organic, metal analogue, succinonitrile-glycerol system were conducted in conjunction with applied ultrasonic energy. The processing parameters associated with this technique have been evaluated in view of optimizing dispersion uniformity. Characterization of the experimental results in terms of an initial modeling effort will also be presented.
The enhanced control over microstructural evolution inherent in rapid solidification processing techniques are exploited to create novel ceramic magnetic materials. The great sensitivity of magnetic properties to local structure provides a powerful probe both for the study of structure and of microscopic solidification mechanisms. The first system studied is the SrO-Fe2O3 binary, which contains the commercially important hard magnetic compound strontium hexaferrite. The products were analyzed by transmission electron microscopy, Mossbauer spectroscopy, magnetic measurements, and differential thermal analysis. As-quenched ribbons contain high concentrations of super-paramagnetic particles, 80 to 250 Angstroms in diameter, in a glassy matrix. This suggests the possibility of crystallizing monodomain strontium hexaferrite during subsequent heat treatment, with a resulting increase in coercivity over conventionally processed ferrite magnets. That magnetic properties can be controlled in solidification processing by varying the quench rate is demonstrated.
The use of directional solidification to produce aligned or magnetic microstructures for the MnAl alloy and the effect of annealing on the bulk magnetic properties of the alloy are investigated. The phase composition, cylindrically shaped magnetization, and room-temperature magnetization of the samples are analyzed. The microstructure of a directionally solidified Al-Mn alloy is characterized by a two-phase structure consisting of randomly-oriented Al-rich fibers of about 40 at. pct Al dispersed in a textureless matrix of about 50 at. pct Al; the matrix phase contains at least 50 wt pct of the metastable and ferrimagnetic tau-phase, and the Al-rich fibers as a precipitated Cr5Al8-type Al-Mn phase. Significant macrosegregation for the thermally stable growth-up orientation is detected. The data reveal that the annealing enhances the cell-like microstructure observed transverse of the solidification direction and increases remanent magnetization and intrinsic coercivity.
This article investigates the fabrication of defect-free Rockit® 606, a high‑carbon, vanadium- and chromium-enriched precipitation-hardening martensitic steel coating, using high-speed laser cladding (HSLC). Compared to conventional laser cladding, HSLC offers higher deposition efficiency, improved coating quality, minimal thermal distortion, and a reduced heat-affected zone. Various HSLC parameters—including laser power, travel speed, powder feed rate, and overlap distance—were optimized to achieve superior coating properties. Microstructural analysis revealed solidification cracks in coatings deposited on carburized steel, regardless of processing parameters. However, preheating the substrate to 250 °C effectively eliminated cracking by reducing thermal gradients. The coatings exhibited a columnar dendritic microstructure, with coarser dendrites near the substrate and finer dendrites towards the surface. Hardness measurements confirmed that all coatings significantly exceeded the industry-specified threshold of 60 HRC, with preheating having minimal effect on overall hardness distribution. Reciprocating sliding wear tests demonstrated a substantial improvement in wear resistance for the defect-free HSLC coatings compared to baseline carburized steel. These findings underscore the potential of HSLC for producing high-performance, wear-resistant coatings suitable for industrial applications.
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.
There are innumerable two-component systems in which two very different liquid phases co-exist in equilibrium over a range of temperature and composition, e.g., oil and water, salt fluxes and solders, aluminum and lead. Often it is of practical concern to fabricate a solid component consisting of a uniform dispersion of one phase in the other. Unfortunately, uniform microstructural development during solidification of two immiscible liquids is hampered by inherent, often large, density differences between the phases that lead to severe segregation. Uniformity is also compromised by preferential wetting and coalescence phenomena. It is, however, well known that ultrasonic energy can initiate and maintain a fine liquid-liquid dispersion. The work presented here extends that observation by application of ultrasonic energy to promote uniform phase incorporation during controlled directional solidification. To this end experiments with the transparent organic, immiscible, succinonitrile-glycerol system were conducted and the numerous processing parameters associated with this technique were evaluated in view of optimizing dispersion uniformity. In view of the initial experimental results a model that predicts the dispersed liquid droplet size as a function of material properties, sample geometry, and applied energy has been developed. In the mathematical model we consider the ultrasonic field in an experimental ampoule of length L and diameter D induced by a probe having a vibration frequency of f=2OKhz (circular frequency omega = 2 pi f). The amplitude is adjustable from A=65 to 13Omicrons. The probe tip diameter is d, the liquid has a density of p, in which the speed of sound and surface tension are, respectively, c and sigma. The mathematical model and numerical investigation for the experiments [1] is done using the following assumptions: (i) The droplet size is small in comparison to the sound wave length; (ii) The forces between droplets are neglected (relative concentration is small); (iii) The droplet is stable if the kinetic energy, E(sub K), of the liquid motion due to ultrasonic field influence is less then the binding energy, E(sub S), due to the surface tension (it is easy to show that the surface energy of two droplets resulting from one is larger by about a factor of two.); (iv) The stability limit is characterized by E(sub S) to approx. E(sub K).