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At least 595 records · Page 33

Experimental observation of the influence of furnace temperature profile on convection and segregation in the vertical Bridgman crystal growth technique

Azulene-doped naphthalene was directionally solidified during the vertical Bridgman-Stockbarger technique. Doping homogeneity and convection were determined as a function of the temperature profile in the furnace and the freezing rate. Convection velocities were two orders of magnitude lower when the temperature increased with height. Rarely was the convection pattern axisymmetric, even though the temperature varied less than 0.1 K around the circumference of the growth ampoule. Correspondingly the cross sectional variation in azulene concentration tended to be asymmetric, especially when the temperature increased with height. This cross sectional variation changed dramatically along the ingot, reflecting changes in convection presumably due to the decreasing height of the melt. Although there was large scatter and irreproducibility in the cross sectional variation in doping, this variation tended to be least when the growth rate was low and the convection was vigorous. It is expected that compositional variations would also be small at high growth rates with weak convection and flat interfaces, although this was not investigated in the present experiments. Neither rotation of the ampoule nor deliberate introduction of thermal asymmetries during solidification had a significant influence on cross sectional variations in doping. It is predicted that slow directional solidification under microgravity conditions could produce greater inhomogeneities than on Earth. Combined use of microgravity and magnetic fields would be required to achieve homogeneity when it is necessary to freeze slowly in order to avoid constitutional supercooling.

Neugebauer, G. T.↗

Microstructural Characterization of a Directionally-Solidified Ni-33 (at. %)Al-31Cr-3Mo Eutectic Alloy as a Function of Withdrawal Rate

The Ni-33 (at. %)Al-3lCr-3Mo eutectic alloy was directionally-solidified (DS) at different rates, V(sub I), varying between 2.5 to 508 mm/ h. Detailed qualitative and quantitative metallographic and chemical analyses were conducted on the directionally-solidified rods. The microstructures consisted of eutectic colonies with parallel lamellar NiAl/(Cr,Mo) plates for solidification rates at and below 12.7 mm/ h. Cellular eutectic microstructures were observed at higher solidification rates, where the plates exhibited a radial pattern. The microstructures were demonstrated to be fairly uniform throughout a 100 mm length of the DS zone by quantitative metallography. The average cell size, bar-d, decreased with increasing growth rate to a value of 125 microns at 508 mm/ h according to the relation bar-d (microns) approx. = 465 V(sup -0.22, sub I), where V(sub I) is in mm/ h. Both the average NiAl plate thickness, bar-Delta(sub NiAl), and the interlamellar spacing, bar-lambda, were observed to be constant for V(sub I) less than or = 50.8 mm/ h but decreased with increasing growth rate above this value as 0.93 bar-Delta(sub NiAl)(microns) = 61.2 V(sup -0.93, sub I) and bar-lambda (microns) = 47.7 V(sup -0.64, sub I), respectively. The present results are detailed on a microstructural map. Keywords Optical microscopy, microstructure, compounds intermetallic, directional solidification

Raj, S. V.↗

An operando synchrotron study on the effect of wire melting state on solidification microstructures of Inconel 718 in wire-laser directed energy deposition

Directed energy deposition (DED) with a coaxial wire-laser configuration has gained significant attention in recent years for the production of large-scale metallic components because of its low directional dependence, fast deposition rate, high feedstock efficiency, and low manufacturing costs. This work studies the coaxial wire-laser DED process of Inconel 718 alloy under a stable deposition condition with a relatively low input volumetric energy density (55.5J/mm 3 ). Post characterization reveals a cluster of refined grains at the center-bottom region of the as-printed track. Operando high-energy synchrotron X-ray experiments and multi-physics modeling are applied innovatively to study the fundamental mechanism responsible for the formation of this microstructure. The X-ray diffraction experiment provides direct evidence, which is supported by the simulation, that the feeding wire can reach the melt pool bottom and release solid particles (primarily carbides) near the mushy zone owing to insufficient melting. Consequently, these sub-micron sized particles suppress the growth of large columnar grains and cause the formation of unique microstructural heterogeneity. In conclusion, this discovery offers new opportunities for tailoring the solidification microstructure by controlling the melting state of the feedstock wire in DED process, in addition to commonly known factors such as the thermal gradient and solidification velocity.

42 ENGINEERING↗

Determination of Systems Suitable for Study as Monotectic Binary Metallic Alloy Solidification Models

Succinonitrile-water and diethylene glycol-ethyl salicylate are two transparent systems which have been studied as monotectic binary metallic alloy solidification models. Being transparent, these systems allow for the direct observations of phase transformations and solidification reactions. The objective was to develop a screening technique to find systems of interest and then experimentally measure those systems. The succinonitrile-water system was used to check the procedures. To simulate the phase diagram of the system, two computer programs which determine solid-liquid and liquid-liquid equilibria were obtained. These programs use the UNIFAC method to determine activity coefficients and together with several other programs were used to predict the phase diagram. An experimental apparatus was developed and the succinonitrile-water phase diagram measured. The diagram was compared to both the simulation and literature data. Substantial differences were found in the comparisons which serve to demonstrate the need for this procedure.

Smith, J. E., Jr.↗

Reproducible Crystal Growth Experiments in Microgravity Science Glovebox at the International Space Station (SUBSA Investigation)

Solidification Using a Baffle in Sealed Ampoules (SUBSA) is the first investigation conducted in the Microgravity Science Glovebox (MSG) Facility at the International Space Station (ISS) Alpha. 8 single crystals of InSb, doped with Te and Zn, were directionally solidified in microgravity. The experiments were conducted in a furnace with a transparent gradient section, and a video camera, sending images to the earth. The real time images (i) helped seeding, (ii) allowed a direct measurement of the solidification rate. The post-flight characterization of the crystals includes: computed x-ray tomography, Secondary Ion Mass Spectroscopy (SIMS), Hall measurements, Atomic Absorption (AA), and 4 point probe analysis. For the first time in microgravity, several crystals having nearly identical initial transients were grown. Reproducible initial transients were obtained with Te-doped InSb. Furthermore, the diffusion controlled end-transient was demonstrated experimentally (SUBSA 02). From the initial transients, the diffusivity of Te and Zn in InSb was determined.

Ostrogorsky, A.↗

Solidification processing of monotectic alloy matrix composites

Directionally solidified aluminum-indium alloys of the monotectic composition were found to form an in situ rod composite which obeys a lambda exp 2 R = constant relation. The experimental data shows good agreement with previously reported results. A theoretical boundary between cellular and dendritic growth conditions was derived and compared with experiments. The unique wetting characteristics of the monotectic alloys can be utilized to tailor the interface structure in metal matrix composites. Metal matrix composites with monotectic and hypermonotectic Al-In matrices were made by pressure infiltration, remelted and directionally solidified to observe the wetting characteristics of the alloys as well as the effect on structure of solidification in the constrained field of the fiber interstices. Models for monotectic growth are modified to take into account solidification in these constrained fields.

Frier, Nancy L.↗

Tailoring material microstructure and property in wire-laser directed energy deposition through a wiggle deposition strategy

Developing effective strategies to directly control material microstructure, property, and anisotropy is an active research area in metal additive manufacturing. This work develops a wiggle deposition pattern for wire-laser directed energy deposition (DED) of 316L stainless steel (SS) to modify the solidification texture, particularly in the building direction, in as-deposited samples. Through multi-physics simulation, operando near-infrared imaging, and synchrotron x-ray characterization, it is found that the wiggle deposition strategy induces highly dynamic melt flow and oscillating thermal gradient in the melt pool, which is responsible for the variation of preferable grain growth direction and crystallographic texture in the sample. The specific texture reduces the anisotropy in the tensile strength of as-printed 316L SS samples cut along different directions. Also, it largely increases the ductility along the build direction. Crystal plasticity simulation is performed to correlate the sample texture with mechanical property. In conclusion, this work offers a unique approach for tailoring local properties through the control of melt pool instability by applying different tool paths.

36 MATERIALS SCIENCE↗

Materials for advanced rocket engine turbopump turbine blades

A study program was conducted to identify those materials that will provide the greatest benefits as turbine blades for advanced liquid propellant rocket engine turbines and to prepare technology plans for the development of those materials for use in the 1990 through 1995 period. The candidate materials were selected from six classes of materials: single-crystal (SC) superalloys, oxide dispersion-strengthened (ODS) superalloys, rapid solidification processed (RSP) superalloys, directionally solidified eutectic (DSE) superalloys, fiber-reinforced superalloy (FRS) composites, and ceramics. Properties of materials from the six classes were compiled and evaluated and property improvements were projected approximately 5 years into the future for advanced versions of materials in each of the six classes.

Chandler, W. T.↗

Experiments with the low melting indium-bismuth alloy system

The following is a laboratory experiment designed to create an interest in and to further understanding of materials science. The primary audience for this material is the junior high school or middle school science student having no previous familiarity with the material, other than some knowledge of temperature and the concepts of atoms, elements, compounds, and chemical reactions. The objective of the experiment is to investigate the indium-bismuth alloy system. Near the eutectic composition, the liquidus is well below the boiling point of water, allowing simple, minimal hazard casting experiments. Such phenomena as metal oxidation, formation of intermetallic compound crystals, and an unusual volume increase during solidification could all be directly observed. A key concept for students to absorb is that properties of an alloy (melting point, mechanical behavior) may not correlate with simple interpolation of properties of the pure components. Discussion of other low melting metals and alloys leads to consideration of environmental and toxicity issues, as well as providing some historical context. Wetting behavior can also be explored.

Krepski, Richard P.↗

Evaluation of the MICAST #2-12 AI-7wt%Si Sample Directionally Solidified Aboard the International Space Station

The US team of the European led "MIcrostructure Formation in CASTing of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions" (MICAST) program recently received a third Aluminum - 7wt% silicon alloy that was processed in the microgravity environment aboard the International Space Station. The sample, designated MICAST#2-12, was directionally solidified in the Solidification with Quench Furnace (SQF) at a constant rate of 40micometers/s through an imposed temperature gradient of 31K/cm. Procedures taken to evaluate the state of the sample prior to sectioning for metallographic analysis are reviewed and rational for measuring the microstructural constituents, in particular the primary dendrite arm spacing (Lambda (sub1)), is given. The data are presented, put in context with the earlier samples, and evaluated in view of a relevant theoretical model.

Tewari, Surendra N.↗

Formation of a metastable ferromagnetic tau phase during containerless melt processing and rapid quenching in Mn-Al-C alloys

Solidification of selected Mn-Al-C alloys during containerless levitation and rapid quenching has yielded the first report for a ferromagnetic metastable tau phase formed directly from the melt. Complete solidification to tau phase was interrupted by the competitive evolution of an equilibrium epsilon phase during recalescence. The amount of undercooling required to produce the metastable ferromagnetic tau phase in a Mn(0.55)Al(0.433)C(0.017) alloy during solidification was estimated as approximately 470 K based on differential thermal analysis results. When the alloy carbon content was increased to 3.4 at. pct, transition in structure development occurred so that the samples exhibited gamma 2 phase formation as well as tau and epsilon phases.

Kim, Y. J.↗

Experiments and simulations on solidification microstructure for Inconel 718 in powder bed fusion electron beam additive manufacturing

Previous research on the powder bed fusion electron beam additive manufacturing of Inconel 718 has established a definite correlation between the processing conditions and the solidification microstructure of components. However, the direct role of physical phenomena such as fluid flow and vaporization on determining the solidification morphology have not been investigated quantitatively. In this work, we investigate the transient and spatial evolution of the fusion zone geometry, temperature gradients, and solidification growth rates during pulsed electron beam melting of the powder bed with a focus on the role of key physical phenomena. The effect of spot density during pulsing, which relates to the amount of heating of the build area during processing, on the columnar-to-equiaxed transition of the solidification structure was studied both experimentally and theoretically. Predictions and the evaluation of the role of heat transfer and fluid flow were established using existing solidification theories combined with transient, three-dimensional numerical heat transfer and fluid flow modeling. Metallurgical characteristics of the alloy’s solidification are extracted from the transient temperature fields, and microstructure is predicted and validated using optical images and electron backscattered diffraction data from the experimental results. Simulations show that the pure liquid region solidified quickly, creating a large two-phase, mushy region that exists during the majority of solidification. While conductive heat transfer dominates in the mushy region, both the pool geometry and the solidification parameters are affected by convective heat transfer. Lastly, increased spot density during processing is shown to increase the time of solidification, lowering temperature gradients and increasing the probability of equiaxed grain formation.

36 MATERIALS SCIENCE↗

A new furnace for high gradient directional growth

A new design furnace for high gradient solidification of in-situ composites is presented. Its essential feature is the direct addition of heat to one side of a thin, pancake-like layer of liquid, and continuous withdrawal of a solid crystal from the other side. Liquid in the thin layer is continuously replenished by solid or liquid feed, and the thinness of the layer permits a large heat throughput with a high temperature gradient without excessive metal superheat. The commercial advantages of this design are improved process efficiency in scale-up, lower melt temperatures, and control of interface morphology by adjusting heater position and temperature. The furnace was tested on Sn-Pb and Al-Cu alloys, obtaining 100C/mm gradients for 6 mm specimens of Al-31.5 % Cu alloy.

Flemings, M. C.↗

Characterization of Titanium Alloys Produced by Electron Beam Directed Energy Deposition

Functionally graded materials offer the potential to improve structural efficiency by allowing the material composition and/or microstructural features to spatially vary within a component. Additive manufacturing techniques enable the fabrication of such graded materials and structures. While examining several titanium alloys, this paper focuses on Ti-8Al-1Er as it has a unique microstructure that is only feasible when produced by rapid solidification methods like electron beam directed energy deposition, an additive manufacturing process. The results show that, when mixed, Ti-8Al-1Er and commercially-pure titanium uniformly mix at various ratios and the resultant static tensile properties of the mixed alloys behave according to rule-of-mixtures. At discontinuous interfaces between Ti-8Al-1Er and commercially-pure titanium, the crack growth behavior progresses smoothly across the discontinuity as the crack transitions from one crack growth regime into another. Studies on monolithic samples shows the mechanisms of damage in the Ti-8Al-1Er; specifically, that strain localization occurs near grain boundaries of high mis-orientation on the microscale and that twinning and dislocation density is concentrated near erbia-strengthening particles (Er2O3) on the nanoscale.

Newman, John A.↗

Transparent Analogs for Alloy Phase Studies

Report describes experiments to add information to data base supporting use of transparent, partially miscible liquids and solids as analogs in studies of alloy solidification. Behavior of these materials observed directly while they undergo liquid/liquid and liquid/solid phase transformations. Light-scattering techniques used to determine phase boundaries. Transparent analogs allow observation of both solidification patterns and processes leading to those patterns, whereas metal alloys require tedious post-solidification metallographic analyses because processes not generally observed. Experiments with transparent substances safer and cheaper since conducted at much lower temperatures.

Frazier, D. O.↗

High fidelity model of directed energy deposition: Laser-powder-melt pool interaction and effect of laser beam profile on solidification microstructure

Metal additive manufacturing technologies keep receiving a great deal of interest as well as strong requests to develop methods to link the process science to printed parts performance and understand how to overcome inherent limitations. Here, a high-fidelity model based on the multiphysics ALE3D code was developed to reproduce the directed energy deposition process down to the powder scale. This includes resolving the laser-powder-melt pool interactions (powder impingement and incorporation into melt pool, hydrodynamics flow condition and laser absorption inefficiencies) as well as the resulting solidification microstructure. This micrometer scale digital twin captured the effect of powder incorporation process and powder flow rate on porosity. Furthermore, it was used to explore how a ring laser beam profile instead of the standard Gaussian laser profile could decrease the thermal gradient along the solidification front in the melt pool, which in turn can increase propensity for more desirable equiaxed grains.

36 MATERIALS SCIENCE↗

Dendritic deformation modes in additive manufacturing revealed by operando x-ray diffraction

Abstract Dynamic solidification behavior during metal additive manufacturing directly influences the as-built microstructure, defects, and mechanical properties of printed parts. How the formation of these features is driven by temperature variation (e.g., thermal gradient magnitude and solidification front velocity) has been studied extensively in metal additive manufacturing, with synchrotron x-ray imaging becoming a critical tool to monitor these processes. Here, we extend these efforts to monitoring full thermomechanical deformation during solidification through the use of operando x-ray diffraction during laser melting. With operando diffraction, we analyze thermomechanical deformation modes such as torsion, bending, fragmentation, assimilation, oscillation, and interdendritic growth. Understanding such phenomena can aid the optimization of printing strategies to obtain specific microstructural features, including localized misorientations, dislocation substructure, and grain boundary character. The interpretation of operando diffraction results is supported by post-mortem electron backscatter diffraction analyses.

Dass, Adrita (ORCID:000000019100635X)↗