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Determination of crystal growth rates during rapid solidification of polycrystalline aluminum by nano-scale spatio-temporal resolution in situ transmission electron microscopy
In situ investigations of rapid solidification in polycrystalline Al thin films were conducted using nano-scale spatio-temporal resolution dynamic transmission electron microscopy. Differences in crystal growth rates and asymmetries in melt pool development were observed as the heat extraction geometry was varied by controlling the proximity of the laser-pulse irradiation and the associated induced melt pools to the edge of the transmission electron microscopy support grid, which acts as a large heat sink. Experimental parameters have been established to maximize the reproducibility of the material response to the laser-pulse-related heating and to ensure that observations of the dynamical behavior of the metal are free from artifacts, leading to accurate interpretations and quantifiable measurements with improved precision. Interface migration rate measurements revealed solidification velocities that increased consistently from ∼1.3 m s{sup −1} to ∼2.5 m s{sup −1} during the rapid solidification process of the Al thin films. Under the influence of an additional large heat sink, increased crystal growth rates as high as 3.3 m s{sup −1} have been measured. The in situ experiments also provided evidence for development of a partially melted, two-phase region prior to the onset of rapid solidification facilitated crystal growth. Using the experimental observations and associated measurements as benchmarks, finite-element modeling based calculations of the melt pool evolution after pulsed laser irradiation have been performed to obtain estimates of the temperature evolution in the thin films.
In Situ X-Ray Observations of Dendritic Fragmentation During Directional Solidification of a Sn-Bi Alloy
Dendrite fragmentation is an important phenomenon in microstructural development during solidification. For instance, it plays a key role in initiating the columnar-to-equiaxed transition (CET). Here, we use x-ray radiography to study dendrite fragmentation rate in a Sn-39.5 wt.% Bi alloy during directional solidification. Experiments were performed in which solidification was parallel and anti-parallel to gravity, leading to significantly different fragmentation rates. We quantify the distribution of fragmentation rate as a function of distance from the solidification front, time in the mushy zone, and volume fraction of solid. While the observed fragmentation rate can be high, there is no evidence of a CET, illustrating that it requires more than just fragmentation to occur.
Characterization of compositional variation and solidification condition on rapid solidification behavior of beta stabilized titanium
Rapid solidification (RS) is a field of study that has increased in importance due to the rise of additive manufacturing (AM) techniques. The breakdown of equilibrium at the solid-liquid interface results in an inability to use traditional solidification models that have been applied to great success in casting. As such, there is a current need for a high-throughput testing method to screen alloys at rapid solidification conditions without the significant cost for powder atomization. In this work, twin hammer splat quenching (SQ) is utilized and theoretically developed as a technique uniquely placed to test alloy systems for AM applications. Using analytical thermal spray models and numerical heat transfer simulations, the cooling rate and solidification conditions of splat quenching are compared across several parameters to evaluate the key parameters for generating cooling rates relevant to AM process. Once a framework for the cooling rates and relevancy of SQ are developed, SQ was used to process alloy compositions in the Ti5553 alloy space (AMS 7026) to study the formation of detrimental secondary phases occurring upon rapid quenching from the melt. A martensitic phase is found to occur at the lower end of the standard, but the composition listed in the standard were found to be safe. Finally, the rapid solidification behavior of Ti-5553 is evaluated by comparing splat quenching, laser welding, and plasma atomization that offer a wide window of solidification conditions. The segregation and solidification structure are analyzed and compared to models to provide a deeper understanding of the solidification behavior of beta stabilized titanium alloys.
Microstructure selection in thin-sample directional solidification of an Al-Cu alloy: In situ X-ray imaging and phase-field simulations
We study microstructure selection during directional solidification of a thin metallic sample. We combine in situ X-ray radiography of a dilute Al-Cu alloy solidification experiments with three-dimensional phase-field simulations. We explore a range of temperature gradient G and growth velocity V and build a microstructure selection map for this alloy. We investigate the selection of the primary dendritic spacing Lambda and tip radius rho. While rho shows a good agreement between experimental measurements and dendrite growth theory, with rho similar to V-1/2, Lambda is observed to increase with V (partial derivative Lambda/partial derivative V > 0), in apparent disagreement with classical scaling laws for primary dendritic spacing, which predict that partial derivative Lambda/partial derivative V <0. We show through simulations that this trend inversion for Lambda(V) is due to liquid convection in our experiments, despite the thin sample configuration. We use a classical diffusion boundary-layer approximation to semi-quantitatively incorporate the effect of liquid convection into phase-field simulations. This approximation is implemented by assuming complete solute mixing outside a purely diffusive zone of constant thickness that surrounds the solid-liquid interface. This simple method enables us to quantitatively match experimental measurements of the planar morphological instability threshold and primary spacings over an order of magnitude in V. We explain the observed inversion of partial derivative Lambda/partial derivative V by a combination of slow transient dynamics of microstructural homogenization and the influence of the sample thickness.
Effect of Naturally Deposited Film on the Sub-rapid Solidification of Medium Manganese Steel by Using Droplet Solidification Technique
In this study, the effect of naturally deposited film on the interfacial heat transfer during the sub-rapid solidification of medium manganese steel was studied by means of a droplet solidification technique. The heat transfer rates were calculated by the Inverse Heat Conduction Program (IHCP), through computing the responding temperatures’ gradient inside the cooling mold. The results showed that the contact angle between the mold and solidified droplet becomes lower (from 117.539 to 82.217 deg) with the repeat of the dropping tests, which means the wettability improves after the deposition of the natural film. Meanwhile the liquid time (the time from the start of ejection to the initiation of solidification) decreases from 1.76 to 1.28 seconds during the tests, suggesting that the steel keeps in the liquid state shorter. Therefore, the initiation of solidification is advanced, such that there would be less time for matching the scale of the shell and the mold. Consequently, the maximum heat flux increases from 2.90 to 6.35 MW/m{sup 2} with the deposition of the natural film, as the wettability is getting better leading to the reduction of the interfacial thermal resistance. However, the final maximum heat flux was decreasing to 4.98 MW/m{sup 2} due to the increased thickness of the film and corresponding interfacial thermal resistance. Moreover, it was found that the secondary dendrite arm spacing decreased from 10.84 to 5.01 μm at first, and then it increased to 8.11 μm with the variations of heat flux and cooling rate.
Transmission electron microscopy of the rapid solidification microstructure evolution and solidification interface velocity determination in hypereutectic Al-20at.%Cu after laser melting
The evolution of rapid solidification (RS) microstructure and solidification interface velocity has been studied experimentally by in-situ transmission electron microscopy and postmortem characterization for hypereutectic Al-20at.%Cu (37 wt.%Cu) after laser melting. Four morphologically distinct regions formed via growth modes changing from θ-Al 2 Cu phase dendrites to eutectic cell growth, possibly α-Al dendrite growth (α-cell), banded growth, and α-Al plane front growth. Tendency for faceting and low capacity for solute trapping limited the θ-phase dendrite growth to solidification interface velocity v < 0.07 m/s. Consequently, formation of pro-eutectic micro-constituent was suppressed, and RS microstructure formation was dominated by eutectic, α-cell, and banded morphology grains for the Al-20at.%Cu alloy. Eutectic growth operated for interface velocity of 0.1 m/s ≤ v < 0.3 m/s, with a transition from regular lamellar, 2-λ and 1-λ mode to a dense irregular morphology dominated by α-phase at v = 0.3 m/s. Interface temperature calculations indicated feasibility of α-cell growth mode for 0.3 m/s ≤ v < 0.7 m/s. Banded growth occurred for 0.7 m/s ≤ v < 1.3 m/s. Plane front α-phase growth was evident for interface velocities v ≥ 1.3 m/s. Previous work on rapid solidification microstructure development in hypereutectic Al-Cu alloys reported a regime of α-cell growth subsequently to eutectic and prior to transition to banded growth for Al-19at.%Cu (36 wt.%Cu), while for Al-22at.%Cu (40 wt.%Cu) eutectic growth transitioned directly to α-plane front growth without emergence of a banded regime. Finally, based on the current study the disappearance of the banded growth regime occurs for a composition larger than 20at.%Cu.
Solidification Behavior and Microstructure Evolution in Dissimilar Electron Beam Welds between Commercially Pure Iron and Nickel
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Influence of morphological instability on grain boundary trajectory during directional solidification
Not provided.
Three-Dimensional Multiscale Modeling of Dendritic Spacing Selection During Al-Si Directional Solidification
Abstract not provided
Proton Radiography Peers into Metal Solidification
Historically, metals are cut up and polished to see the structure and to infer how processing influences the evolution. We can now peer into a metal during processing without destroying it using proton radiography. Understanding the link between processing and structure is important because structure profoundly affects the properties of engineering materials. Synchrotron x-ray radiography has enabled real-time glimpses into metal solidification. However, x-ray energies favor the examination of small volumes and low density metals. In this study, we use high energy proton radiography for the first time to image a large metal volume (>10,000 mm 3 ) during melting and solidification. We also show complementary x-ray results from a small volume (<1mm 3 ), bridging four orders of magnitude. In conclusion, real-time imaging will enable efficient process development and the control of the structure evolution to make materials with intended properties; it will also permit the development of experimentally informed, predictive structure and process models.
A computational model for molten corium spreading and solidification
Not Available
Three-dimensional Dendritic Needle Network model with application to Al-Cu directional solidification experiments
Abstract not provided
Rationalization of solidification mechanism of Nd–Fe–B magnets during laser directed-energy deposition [Rationalization of solidification mechanism of neodymium-iron-boron magnets obtained after laser directed-energy deposition process]
Here, near-net fabrication techniques are highly beneficial to minimize rare earth metal usage to fabricate dense fully functional magnets. In this study, feasibility of using the directed-energy deposition technique for fabrication of magnets is evaluated. The results show that despite the ability to fabricate highly reactive materials in the laser deposition process, the magnetic coercivity and remanence of the hard magnets is significantly reduced. X-ray powder diffraction in conjunction with electron microscopy showed that the material experienced a primary Nd 2 Fe 17 B x solidification. Consequently, the absence of the hard magnetic phase resulted in deterioration of the build properties.
In situ Investigation of Magnetism in Metastable Phases of Levitated Fe 83 B 17 During Solidification
Not Available
Proven Technologies for the Solidification of Complex Liquid Radioactive Waste (LRW): Global Case Studies of Applications and Disposal Options - 20424
Legacy radioactive waste streams from the Cold War still exist and newly generated waste streams from nuclear power plants and research institutes go untreated and expose environmental hazards at many nuclear sites. The nature of the waste is diverse, depending upon the source or the process from which it originated. The most problematic waste streams include complex liquids such as organic (tri-butyl-phosphate TBP) solutions contaminated with Pu and U isotopes, mixed sludge types, high acid radioactive waste, H-3 contaminated organic and aqueous streams, etc. Technological, environmental and economic challenges exist for the treatment and disposal of such waste streams. A proven technology that has been applied to LRW on a global basis provides one option as a low-cost solution to legacy streams and small volume, highly complex LRW frequently found during decommissioning at nuclear power plants and weapons sites. The engineered polymer technology from Nochar, USA, is capable of solidifying standard and highly complex LLW and ILW waste streams for interim or final storage, or for incineration. (authors)