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Influence of convection on microstructure

The primary motivation for this research has been to determine the cause for space processing altering the microstructure of some eutectics, especially the MnBi-Bi eutectic. Prior experimental research at Grumman and here showed that the microstructure of MnBi-Bi eutectic is twice as fine when solidified in space or in a magnetic field, is uninfluenced by interfacial temperature gradient, adjusts very quickly to changes in freezing rate, and becomes coarser when spin-up/spin-down (accelerated crucible rotation technique) is used during solidification. Theoretical work at Clarkson predicted that buoyancy driven convection on earth could not account for the two fold change in fiber spacing caused by solidification in space. However, a lamellar structure with a planar interface was assumed, and the Soret effect was not included in the analysis. Experimental work at Clarkson showed that the interface is not planar, and that MnBi fibers project out in front of the Bi matrix on the order of one fiber diameter. Originally four primary hypotheses were to be tested under this current grant: (1) a fibrous microstructure is much more sensitive to convection than a lamellar microstructure, which was assumed in our prior theoretical treatment; (2) an interface with one phase projecting out into the melt is much more sensitive to convection than a planar interface, which was assumed in our prior theoretical treatment; (3) the Soret effect is much more important in the absence of convection and has a sufficiently large influence on microstructure that its action can explain the flight results; and (4) the microstructure is much more sensitive to convection when the composition of the bulk melt is off eutectic. As reported previously, we have learned that while a fibrous microstructure and a non-planar interface are more sensitive to convection than a lamellar microstructure with a planar interface, the influence of convection remains too small to explain the flight and magnetic field results. Similarly addition of the Soret effect does not explain the flight and magnetic field results.

Wilcox, William R.

NASA-UVA light aerospace alloy and structures technology program (LA(sup 2)ST)

The general objective of the Light Aerospace Alloy and Structures Technology (LA(sup 2)ST) Program is to conduct interdisciplinary graduate student research on the performance of next generation, light weight aerospace alloys, composites, and thermal gradient structures in collaboration with Langley researchers. Specific technical objectives are established for each research project. We aim to produce relevant data and basic understanding of material behavior and microstructure, new monolithic and composite alloys, advanced processing methods, new solid and fluid mechanics analyses, measurement advances, and critically, a pool of educated graduate students for aerospace technologies. Four research areas are being actively investigated, including: (1) Mechanical and Environmental Degradation Mechanisms in Advanced Light Metals and Composites; (2) Aerospace Materials Science; (3) Mechanics of Materials and Composites for Aerospace Structures; and (4) Thermal Gradient Structures.

Gangloff, Richard P.

Disorder to Order in Interface Patterns: Thermal Noise to Limit Cycle Transition in Dendrite Sidebranch Formation

Thin sample directional solidification experiments have been carried out in the model succinonitrile-camphor system to examine the origin of secondary branches in dendrite morphologies. Thermal noise at the dendrite tip creates interface instabilities which amplify to form sidebranches. This is accepted as the primary mode of sidebranching in dendritic growth from an undercooled melt and occurs in directional solidification of dendrites. The proposed limit cycle couples the growth of the tip with the initiation of the sidebranch. Directional solidification of curved interfaces is a driven dissipative system with the potential to form a limit cycle. Two sets of experiments were performed, the first holding velocity constant and evolving the gradient and the second imposing oscillating velocities around the natural period of sidebranching. Both experimental methods were found to characterize a transition from disordered sidebranching induced by thermal noise to ordered sidebranching produced by the limit cycle mechanisms. This is the first quantitative measurement of previously hypothesized limit cycle growth. These experiment sets have been quantitatively analyzed for dynamic behavior seen in limit cycles. High-quality data sets of the tip and instability enable the measurement of the FFT and analysis through a power spectrum. At low gradients, the sidebranches are found to be excited by thermal noise far away from the tip. As the gradient increases and velocity is held constant, the distance between the instability and tip decreases until limit cycle growth is found between the tip of the primary dendrite and the first forming sidebranch. An alternative to the deterministic limit cycles seen in experiments of gradient evolution is a limit cycle actively driven through the square wave oscillation of velocity. Crucial observations of the solidified microstructure conclude that this produced periodic interconnected bridges between the primary dendrites. This is a finding with potentially significant implications for commercial applications.

Trevor Lyons

Influence of convection on microstructure

In eutectic growth, as the solid phases grow they reject atoms to the liquid. This results in a variation of melt composition along the solid/liquid interface. In the past, mass transfer in eutectic solidification, in the absence of convection, was considered to be governed only by the diffusion induced by compositional gradients. However, mass transfer can also be generated by a temperature gradient. This is called thermotransport, thermomigration, thermal diffusion or the Soret effect. A theoretical model of the influence of the Soret effect on the growth of eutectic alloys is presented. A differential equation describing the compositional field near the interface during unidirectional solidification of a binary eutectic alloy was formulated by including the contributions of both compositional and thermal gradients in the liquid. A steady-state solution of the differential equation was obtained by applying appropriate boundary conditions and accounting for heat flow in the melt. Following that, the average interfacial composition was converted to a variation of undercooling at the interface, and consequently to microstructural parameters. The results obtained show that thermotransport can, under certain circumstances, be a parameter of paramount importance.

Wilcox, William R.

Microstructure prediction for Ti-22Al-25Nb in laser powder bed fusion

This work presents a physics-informed framework for predicting solidification morphology and defect susceptibility in additively manufactured Ti–22Al–25Nb across a broad processing space. The framework integrates solidification microstructure selection (SMS) analysis with a single-track defect-based printability map to establish a unified methodology linking processing parameters to both interfacial morphology and manufacturability. Thermal gradients G and solidification rates R are first computed using the Thermo-Calc Additive Manufacturing (TC-AM) module, a finite-interface-dissipation (FID) phase-field (PF) model coupled with CALPHAD method is then employed to systematically distinguish planar and dendritic regimes as functions of $G$ and $R$. By superimposing the printability map onto the morphology projections, a comprehensive process–structure framework is obtained. Across most processing conditions, the predicted microstructure is predominantly dendritic, while planar growth emerges only under selected laser power $P$ and scan speed $v$ combinations. In addition to morphology classification, the framework quantifies the dendritic area fraction and introduces a width-based morphology descriptor to characterize the spatial extent of planar/dendritic regions within the melt pool. It provides mechanistic insight into the interplay between solidification physics and defect formation, offering practical guidance for parameter selection and microstructural control in Ti–22Al–25Nb additive manufacturing (AM).

36 MATERIALS SCIENCE

NASA-UVA light aerospace alloy and structures technology program (LA2ST)

The NASA-UVa Light Aerospace Alloy and Structure Technology (LAST) Program continues to maintain a high level of activity, with projects being conducted by graduate students and faculty advisors in the Departments of Materials Science and Engineering, Civil Engineering and Applied Mechanics, and Mechanical and Aerospace Engineering at the University of Virginia. This work is funded by the NASA-Langley Research Center under Grant NAG-1-745. Here, we report on progress achieved between January 1 and June 30, 1992. The objectives of the LA2ST Program is to conduct interdisciplinary graduate student research on the performance of the next generation, light weight aerospace alloys, composites and thermal gradient structures in collaboration with Langley researchers. Technical objectives are established for each research project. We aim to produce relevant data and basic understanding of material mechanical response, corrosion behavior, and microstructure; new monolithic and composite alloys; advanced processing methods; new solid and fluid mechanics analyses; measurement advances; and critically, a pool of educated graduate students for aerospace technologies. The accomplishments presented in this report cover topics including: (1) Mechanical and Environmental Degradation Mechanisms in Advance Light Metals and Composites; (2) Aerospace Materials Science; (3) Mechanics of Materials and Composites for Aerospace Structures; and (4) Thermal Gradient Structures.

Gangloff, Richard P.

ISS-Experiments of Columnar-to-Equiaxed Transition in Solidification Processing

The main topic of the research project CETSOL in the framework of the Microgravity Application Promotion (MAP) programme of the European Space Agency (ESA) is the investigation of the transition from columnar to equiaxed grain growth during solidification. Microgravity environment allows for suppression of buoyancy-driven melt flow and for growth of equiaxed grains free of sedimentation and buoyancy effects. This contribution will present first experimental results obtained in microgravity using hypo-eutectic AlSi alloys in the Materials Science Laboratory (MSL) on-board the International Space Station (ISS). The analysis of the experiments confirms the existence of a columnar to equiaxed transition, especially in the refined alloy. Temperature evolution and grain structure analysis provide critical values for the position, the temperature gradient and the solidification velocity at the columnar to equiaxed transition. These data will be used to improve modeling of solidification microstructures and grain structure on different lengths scales.

Sturz, Laszlo

Directional solidification and characterization of near eutectic Sm2CO17/Co alloys

The effects of directional solidification processing on the microstructural, compositional, and magnetic properties of near eutectic Co-Sm alloys (about 9 at. pct Sm) have been studied. Initial investigations have been performed at modest thermal gradients in the liquid, G(L) less than 60 C/cm and over a range of furnace (solidification) velocities, V = 0.8 45.4 cm/h. The primary dendrite spacing for near eutectic Sm2Co17/Co scaled with 1/sq rt V and varied from about 50 microns for V greater than or equal to 20 cm/h to hundreds of microns for V less than 10 cm/h, while the rod eutectic diameter and interrod spacing were an order of magnitude smaller. For both dendritic and cooperative growth, the associated permanent magnet properties were rather poor, e.g., remanence less than 4 kG and coercive force less than 1 kOe for the smallest dendrite and rod diameter dimensions encountered, although the magnetic hardness for the rod eutetic was larger than for the dendritic microstructure. Magnetization as a function of sample orientation indicated that the easy axis of magnetization was primarily along the direction of solidification for both ferromagnetic phases.

Pirich, Ronald G.

Bi‐Continuous W‐Rich Refractory High Entropy Alloy‐Cu Composite: Toward Material Innovation of Nuclear Reactor Coolant System

Abstract Refractory high‐entropy alloys (RHEAs) are considered promising candidate materials for next‐generation nuclear reactors due to their superior mechanical strength, irradiation resistance, and thermal stability at high temperatures. However, the significant positive heat of mixing between refractory alloying elements and Cu, commonly used in cooling systems, poses challenges in forming composite structures. This study addresses the issue using a liquid metal dealloying (LMD) process. A precursor alloy (WTaVTi) with a directional dendrite‐interdendrite structure is fabricated and reacted with molten Cu at 1200 °C for 96 h. This approach produced a RHEA‐Cu composite with a stable interface between RHEA (W 31.5 Ta 30.9 V 21.4 Ti 14.3 ) and Cu, featuring a spontaneously formed W‐rich interlayer that enhances interfacial bonding. The composite showed excellent irradiation resistance, with 30% less swelling under α‐ion irradiation than pure W. It also exhibited low thermal conductivity at room temperature, but reached ≈120 W m −1 ·K −1 at ≈650 °C, surpassing pure W. This temperature‐dependent rise in κ, with a positive gradient of +0.075 W m −1 ·K − 2 , is attributed to decreasing diffuse mismatch at elevated temperatures. The large‐scale reaction and stable microstructure achieved through LMD process highlight its industrial potential. This work offers a strategy for developing high‐performance materials by combining RHEA's radiation resistance with Cu's thermal conductivity for extreme environments.

Chemistry

Comparison of In-situ Near Infrared Melt Pool Imagery to Optical Microscopy Measurements

Additive manufacturing (AM) is a rapidly growing technology. An area of major importance is the integrity and repeatability of AM parts. The goal is to reduce obstacles to certify AM built parts to allow for use in critical aerospace applications. In-situ nondestructive evaluation sensors can be used for build assessment and can potentially play a key role in certifying AM parts. For example, melt pool features are understood to have a strong correlation to microstructural defects and the use of a near infrared (NIR) camera can be used to record the melt pool, cooling areas, and temperature gradients during the build. This work explores the use of a low cost NIR camera to obtain single line track imagery of the Ti-6Al-4V melt pools for various processing parameters. The NIR camera is radiometrically calibrated and configured in-line with the laser source to obtain high resolution imagery of the melt pool shape and dynamics. The challenge to measure melt pool shapes is to identify the transition points between the metal solid to liquid phase. Factors for melt pool measurements such as thermal camera pixel resolution, surface emissivity, and blurring due to the laser beam movement are discussed. Lastly, the melt pool imagery are compared to optical microscopy measurements for validation.

additive manufacturing

The microstructure of MnBi/Bi eutectic alloys

Directionally solidified eutectic alloys of the system MnBi/Bi have been investigated with reference to the dependence of the fiber spacing on the growth rate and the interfacial temperature gradient. It is found that the fiber spacing varies as the inverse square root of the growth rate and does not depend on the temperature gradient in contrast to the claims that all faceted/non-faceted eutectics should show a temperature gradient influence.

Ravishankar, P. S.

Time at Temperature Experiments on Neutron Irradiated Zircaloy-2 using Conventional & Flash DSC

Dryout events in Boiling Water Reactors (BWRs) are currently treated by NRC regulations as automatic disqualification for continued fuel rod operation, even though this criterion does not account for the rate or duration of power increases, associated changes in material behavior, or the possibility of rewetting. Operational history from Anticipated Operational Occurrences (AOOs) shows that short, transient power excursions often demand only modest heat removal, and industry experience suggests that fuel can briefly enter dryout yet return to safe, stable operation. The lack of detailed understanding of the material response during such events motivates the present series of experiments. This study uses unique and innovative methods to investigate microstructural evolution in irradiated Zircaloy-2 exposed to high temperatures in inert environments. Differential Scanning Calorimetry (DSC) and FlashDSC are combined to build a comprehensive experimental framework capable of identifying the a–ß phase transformation in zirconium and examining defect annealing under steep thermal gradients. FlashDSC enables rapid heating and cooling of Focused Ion Beam (FIB)–prepared large-area lift-outs (LALOs) of irradiated Zircaloy-2 at rates of 1,000 K/s to peak temperatures of 600°C, 750°C, and 900°C. The goal is to determine whether these conditions produce measurable microstructural changes that could influence cladding performance in typical BWR environments. Microstructural characterization includes quantifying dislocation density and assessing secondary phase particle (SPP) size and distribution using Transmission Electron Microscopy (TEM). Ongoing analysis, such as diffraction pattern indexing and 4D STEM processing, will further refine these observations.

36 - MATERIALS SCIENCE

Dusty Gas Model for Solid Oxide Fuel Cell Fuel Electrode

This model applies the Dusty Gas Model simulate multi-component species transport in SOFC (solid oxide fuel cell) anodes which considers the pressure gradient across the fuel electrode. This studyhas been verified with the analytical solution for different fuel electrode thicknesses and with literature values. The model was developed using the VoronoiFVM platform in Julia which is a built in implicit and semi implicit solver that integrates electrochemical behavior, microstructural effects, and transient analysis for accurate prediction of species transport under varying conditions.

dusty gas model (DGM)

Controlled Temperature Gradient Improves Freezing Alloy

Controlled gradient of temperature in advancing zone of solidification increases fatigue life of directionally solidified nickel-base superalloy. Improved solidification process eliminates, reduces, or controls microstructure of deleterious brittle phases, including carbides and gamma/gamma prime eutectic. Also reduces microsegregation and makes discrete carbides (if present) become fine and blocky. Expected to improve properties of other alloys, of both directionally-solidified polycrystalline and single-crystal forms.

Schmidt, Deborah

Processing and Properties of HfB2 Based Materials

Contents include the following: Modified hot pressing schedule has significantly improved UHTC billet processing: density and microstructure uniformity have improved. 2 in. dia. x 2 in. tall UHTC billets have been successfully hot pressed: scaled up billets have slightly higher density gradients axially than 1 in. billets. Hot press schedule has not been optimized for scaled up billets. Strengths and strength distributions are improving with experience: need to evaluate strength uniformity in the center of the billets. CTE or ARC materials compares favorably with heritage materials. Thermal conductivity of ARC materials considerably different than that of heritage materials.

Johnson, Sylvia M.

Fossilization processes in siliceous thermal springs: trends in preservation along thermal gradients

To enhance our ability to extract palaeobiological and palaeoenvironmental information from ancient thermal spring deposits, we have studied the processes responsible for the development and preservation of stromatolites in modern subaerial thermal spring systems in Yellowstone National Park (USA). We investigated specimens collected from silica-depositing thermal springs along the thermal gradient using petrographic techniques and scanning electron microscopy. Although it is known that thermophilic cyanobacteria control the morphogenesis of thermal spring stromatolites below 73 degrees C, we have found that biofilms which contain filamentous thermophiles contribute to the microstructural development of subaerial geyserites that occur along the inner rims of thermal spring pools and geyser effluents. Biofilms intermittently colonize the surfaces of subaerial geyserites and provide a favoured substrate for opaline silica precipitation. We have also found that the preservation of biotically produced microfabrics of thermal spring sinters reflects dynamic balances between rates of population growth, decomposition of organic matter, silica deposition and early diagenesis. Major trends in preservation of thermophilic organisms along the thermal gradient are defined by differences in the mode of fossilization, including replacement, encrustation and permineralization.

NASA Discipline Exobiology

In-situ neutron radiography of pore-water movement in portland cement mortar under subzero temperature exposure: Insights from D 2 O-H 2 O systems

Neutron radiography was employed in this study to monitor real-time pore water movement in portland cement mortar exposed to subzero temperatures, providing novel insights into freeze-thaw (F-T) damage mechanisms. Deuterated water (D 2 O) was used to hydrate the cement in the mortar specimens, and the pore structure was saturated with water (H 2 O), allowing for a contrast that enabled detailed tracking of water movement predominantly in the pore structure. Furthermore, the mortar sample was placed on a chiller plate set to subzero temperatures, thereby providing a one-dimensional temperature gradient vertically in the sample. Neutron radiography revealed that unfrozen water migrated upward as the freezing front advanced, which can create hydraulic pressure within the mortar microstructure and may contribute to the initiation and propagation of microcracks during F-T cycles. Additional characterization of the concrete made with D 2 O showed a marked contrast to the samples made with H 2 O, including delayed hydration, diminished compressive strength, and greater porosity. Therefore, while mortar made with D 2 O allowed for greater neutron contrast to the pores filled with H 2 O, further study is required to produce mortars with similar properties to those made with H 2 O. In addition, further refinement is needed to the radiography experiment to allow for greater control of temperatures and potential quantification of the water concentration.

Air-void system

NASA-UVA Light Aerospace Alloy and Structures Technology Program (LA2ST)

The general objective of the Light Aerospace Alloy and Structures Technology (LA2ST) Program is to conduct interdisciplinary graduate student research on the performance of next generation, light weight aerospace alloys, composites, and associated thermal gradient structures in close collaboration with Langley researchers. Specific technical objectives are established for each research project. Relevant data and basic understanding of material behavior and microstructure, new monolithic and composite alloys, advanced processing methods, new solid and fluid mechanic analyses, measurement advances, and a pool of educated graduate students are sought.

Gangloff, Richard P.