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All sources NASA NTRS DOE OSTI

DOE OSTI2022

Effects of composition and growth parameters on phase formation in multicomponent aluminum garnet crystals

The effects of composition on the phase formation of multicomponent garnet crystals grown via directional solidification by the micro-pulling-down method are studied. A relatively wide range of rare-earth (RE) average ionic radii (AIR) is explored by formulating ten compositions from the system (Lu,Y,Ho,Dy,Tb,Gd) 3 Al 5 O 12 . Crystals were grown at either 0.05 or 0.20 mm min -1 . The hypothesis is that multicomponent compounds with large AIR will form secondary phases as the single-RE aluminum garnets formed by larger Tb 3+ or Gd 3+ ; this will result in crystals of poor optical quality. Crystals with large AIR have a central opaque region in optical microscopy images, which is responsible for their reduced transparency compared to crystals with small AIR. Slow pulling rates suppress the formation of the opaque region in crystals with intermediate AIR. Powder and single-crystal X-ray diffraction and electron probe microanalysis results indicate that the opaque region is a perovskite phase. Scanning electron microscopy and energy dispersive spectroscopy measurements reveal eutectic inclusions at the outer surface of the crystals. Finally, the concentration of the eutectic inclusions increases with increasing AIR.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Process-dependent anisotropic thermal conductivity of laser powder bed fusion AlSi10Mg: impact of microstructure and aluminum-silicon interfaces

Purpose AlSi10Mg alloy is commonly used in laser powder bed fusion due to its printability, relatively high thermal conductivity, low density and good mechanical properties. However, the thermal conductivity of as-built materials as a function of processing (energy density, laser power, laser scanning speed, support structure) and build orientation, are not well explored in the literature. This study aims to elucidate the relationship between processing, microstructure, and thermal conductivity. Design/methodology/approach The thermal conductivity of laser powder bed fusion (L-PBF) AlSi10Mg samples are investigated by the flash diffusivity and frequency domain thermoreflectance (FDTR) techniques. Thermal conductivities are linked to the microstructure of L-PBF AlSi10Mg, which changes with processing conditions. The through-plane exceeded the in-plane thermal conductivity for all energy densities. A co-located thermal conductivity map by frequency domain thermoreflectance (FDTR) and crystallographic grain orientation map by electron backscattered diffraction (EBSD) was used to investigate the effect of microstructure on thermal conductivity. Findings The highest through-plane thermal conductivity (136 ± 2 W/m-K) was achieved at 59 J/mm 3 and exceeded the values reported previously. The in-plane thermal conductivity peaked at 117 ± 2 W/m-K at 50 J/mm 3 . The trend of thermal conductivity reducing with energy density at similar porosity was primarily due to the reduced grain size producing more Al-Si interfaces that pose thermal resistance. At these interfaces, thermal energy must convert from electrons in the aluminum to phonons in the silicon. The co-located thermal conductivity and crystallographic grain orientation maps confirmed that larger colonies of columnar grains have higher thermal conductivity compared to smaller columnar grains. Practical implications The thermal properties of AlSi10Mg are crucial to heat transfer applications including additively manufactured heatsinks, cold plates, vapor chambers, heat pipes, enclosures and heat exchangers. Additionally, thermal-based nondestructive testing methods require these properties for applications such as defect detection and simulation of L-PBF processes. Industrial standards for L-PBF processes and components can use the data for thermal applications. Originality/value To the best of the authors’ knowledge, this paper is the first to make coupled thermal conductivity maps that were matched to microstructure for L-PBF AlSi10Mg aluminum alloy. This was achieved by a unique in-house thermal conductivity mapping setup and relating the data to local SEM EBSD maps. This provides the first conclusive proof that larger grain sizes can achieve higher thermal conductivity for this processing method and material system. This study also shows that control of the solidification can result in higher thermal conductivity. It was also the first to find that the build substrate (with or without support) has a large effect on thermal conductivity.

Engineering↗

DOE OSTI2014

High-Performance MnBi Alloy Prepared Using Profiled Heat Treatment

The profiled heat treatment (PHT) method has been used to synthesize MnBi alloys with high-purity low-temperature phase (LTP). In the PHT method, the arc-melted MnBi alloy was remelted then slowly cooled by a pseudo-equilibrium solidification process to promote the formation of LTP phase. The PHT-treated MnBi alloys had an LTP phase up to 94 wt.% and a magnetization of 73 emu/g under a field of 9 T. Scanning electron microscopy showed that there exist some micrometer-sized Mn-rich inclusions in the LTP matrix of the PHT MnBi alloy. The PHT MnBi alloys were crushed into powders with an average size of ~3 μm by low-energy ball milling. These MnBi powders were aligned in an 18 kOe field and warm compacted into a bulk magnet at 300 °C for 30 min. The magnet had a density of 8.2 g/cm3 and magnetic properties of Ms = 6.7 kG, Mr = 5.3 kGs, i Hc = 5 kOe, and (BH)max = 6.1 MGOe

MnBi↗

DOE OSTI2017

Net shape processing of alnico magnets by additive manufacturing

Alternatives to rare earth permanent magnets, such as alnico, will reduce supply instability, increase sustainability, and could decrease the cost of permanent magnets, especially for high temperature applications, such as traction drive motors. Alnico magnets with moderate coercivity, high remanence, and relatively high energy product are conventionally processed by directional solidification and (significant) final machining, contributing to increased costs and additional material waste. Additive manufacturing (AM) is developing as a cost effective method to build net-shape three-dimensional parts with minimal final machining and properties comparable to wrought parts. This work describes initial studies of net-shape fabrication of alnico magnets by AM using a laser engineered net shaping (LENS) system. High pressure gas atomized (HPGA) pre-alloyed powders of two different modified alnico “8” compositions, with high purity and sphericity, were built into cylinders using the LENS process, followed by heat treatment. The magnetic properties showed improvement over their cast and sintered counterparts. The resulting alnico permanent magnets were characterized using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), and hysteresisgraph measurements. Furthermore, these results display the potential for net-shape processing of alnico permanent magnets for use in next generation traction drive motors and other applications requiring high temperatures and/or complex engineered part geometries.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Assessment of Directionally Solidified Eutectic Sm–Fe(Co)–Ti Alloys as Permanent Magnet Materials

Sm–Fe–Ti and Sm–Fe0.8Co0.2–Ti alloys were prepared via arc-melting and directionally solidified on a water-cooled copper hearth. The as-solidified alloys featured cells of the Sm(Fe,Co,Ti)12–Ti(Fe,Co) 2+δ –(α-Fe) lamellar eutectic. The lamellae of Sm(Fe,Co,Ti)12 phase with a crystal structure of the ThMn12 type were less than 0.2 μm thick, and had their [001] easy-magnetization directions oriented along the temperature gradient of the solidification. The eutectic microstructure led to an increased coercivity, especially in the Co-added alloys. Below 250 °C, this coercivity was found not to vary much with temperature with a temperature coefficient of -0.18 %/°C. However, the modest absolute values, reaching only 0.7 kOe, are insufficient for utilization of the directionally solidified alloys as anisotropic permanent magnets.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Metastability in the MgAl 2 O 4 -Al 2 O 3 System

Aluminum oxide must take a spinel form ( γ-Al 2 O 3 ) at elevated temperatures in order for extensive solid solution to form between MgAl 2 O 4 and α-Al 2 O 3 . The solvus line between MgAl 2 O 4 and Al 2 O 3 has been defined at 79.6 wt% Al 2 O 3 at 1500°C, 83.0 wt% Al 2 O 3 at 1600°C, and 86.5 wt% Al 2 O 3 at 1700°C. A metastable region has been defined at temperatures up to 1700°C which could have significant implications for material processing and properties. Additionally, initial processing could have major implications on final chemistry. The spinel solid solution region has been extended to form an infinite solid solution with Al 2 O 3 at elevated temperatures. A minimum in melting at 1975°C and a chemistry of 96 wt% Al 2 O 3 rather than a eutectic is present, resulting in no eutectic crystal formation during solidification.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Freeze-cast yttria-stabilized zirconia pore networks: Effects of alcohol additives

Freeze casting yttria-stabilized zirconia (YSZ) can be useful in making electrodes for solid oxide fuel cells (SOFCs) by introducing hierarchical porosity to increase triple-phase boundary (TPB) area while maintaining adequate fuel flow. Here, in this work, the influence of alcohol additives on pore structure of aqueous YSZ freeze-cast samples was investigated. Slurries with ethanol, iso-propyl alcohol, or methanol as additives were compared to a control sample. Pore characteristics along sample lengths were measured using X-ray computed tomography reconstructions. The control sample showed significant changes in pore size along sample length, whereas pore size of the alcohol additive samples remained similar, indicating that freezing rates of the additive samples remained constant during solidification. Finally, ice lens formation and interactions between alcohols and slurry functional additives (dispersant, surfactant, and binder) resulted in complex pore structures which show promise in increasing SOFC TPB area.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Determination of heat conductivity of waste glass feed and its applicability for modeling the batch-to-glass conversion

The heat conductivity of reacting melter feed affects the heat transfer and conversion process in the cold cap (the reacting feed floating on molten glass). To investigate it, we simulated the feed conditions and morphology in the cold-cap by preparing “fast-dried slurry blocks”, formed by rapidly evaporating water from feed slurry poured onto a 200°C surface. A heat conductivity meter was used to measure heat conductivity of samples cut from the fast-dried slurry blocks, samples of a cold cap retrieved from a laboratory-scale melter, and loose dry powder feed samples. Our study indicates that the heat conductivity of the feed in the cold cap is significantly higher than that of loose dry powder feed, resulting from the feed solidification during the water evaporation from the feed slurry. To assess the heat transfer at higher temperatures when feed turns into foam, we developed a theoretical model that predicts the foam heat conductivity based on morphology data from in-situ X-ray computed tomography. The implications for the mathematical modeling of the cold cap are discussed.

Hujova, Miroslava↗

DOE OSTI2024

Selective laser sintering and spark plasma sintering of (Zr,Nb,Ta,Ti,W)C compositionally complex carbide ceramics

Abstract Two advanced manufacturing processes, spark plasma sintering (SPS) and selective laser sintering (SLS), have been developed for synthesis of (Zr,Nb,Ta,Ti,W)C compositionally complex carbide (CCC) via reactive sintering of a powder mixture of constitute monocarbides. X‐ray diffraction analysis confirmed that the single‐phase CCC can be formed by both SPS and SLS. While a homogenous microstructure with uniform metal element distributions was developed during SPS, three‐layer microstructures with a thin TiC‐rich layer and two TaC‐rich layers along with a TiO 2 ‐rich surface layer containing W nanoparticles were formed during SLS. In addition, cellular structures with W, Zr, and Ti element segregation and dislocations on cell boundaries were observed in the SLS‐CCC sample, indicating the effect of nonequilibrium conditions on microstructure formation during laser melting followed by rapid cooling and solidification process. Compared to the SPS‐CCC sample, the SLS‐CCC showed enhanced hardness and reduced thermal conductivity, which may be related to their unique cellular structures.

36 MATERIALS SCIENCE↗

DOE OSTI2014

A review of lunar chronology revealing a preponderance of 4.34-4.37 Ga ages

In this study, data obtained from Sm-Nd and Rb-Sr isotopic measurements of lunar highlands’ samples are renormalized to common standard values and then used to define ages with a common isochron regression algorithm. The reliability of these ages is evaluated using five criteria that include whether: (1) the ages are defined by multiple isotopic systems, (2) the data demonstrate limited scatter outside uncertainty, (3) initial isotopic compositions are consistent with the petrogenesis of the samples, (4) the ages are defined by an isotopic system that is resistant to disturbance by impact metamorphism, and (5) the rare-earth element abundances determined by isotope dilution of bulk of mineral fractions match those measured by in situ analyses. From this analysis, it is apparent that the oldest highlands’ rock ages are some of the least reliable, and that there is little support for crustal ages older than ~4.40 Ga. A model age for ur-KREEP formation calculated using the most reliable Mg-suite Sm-Nd isotopic systematics, in conjunction with Sm-Nd analyses of KREEP basalts, is 4389 ± 45 Ma. This age is a good match to the Lu-Hf model age of 4353 ± 37 Ma determined using a subset of this sample suite, the average model age of 4353 ± 25 Ma determined on mare basalts with the 146 Sm- 142 Nd isotopic system, with a peak in Pb-Pb ages observed in lunar zircons of ~4340 ± 20 Ma, and the oldest terrestrial zircon age of 4374 ± 6 Ma. The preponderance of ages between 4.34 and 4.37 Ga reflect either primordial solidification of a lunar magma ocean or a widespread secondary magmatic event on the lunar nearside. The first scenario is not consistent with the oldest ages reported for lunar zircons, whereas the second scenario does not account for concordance between ages of crustal rocks and mantle reservoirs.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2016

Methodology for Estimating Thermal and Neutron Embrittlement of Austenitic Stainless Steel Welds During Service in Light Water Reactors

The effect of thermal aging on the degradation of fracture toughness and Charpy-impact properties of austenitic stainless steel (SS) welds has been characterized at reactor temperatures. The solidification behavior and the distribution and morphology of the ferrite phase in SS welds are described. Thermal aging of the welds results in moderate decreases in Charpy-impact strength and fracture toughness. The upper-shelf Charpy-impact energy of aged welds decreases by 50–80 J/cm2. The decrease in fracture toughness J-R curve, or JIc is relatively small. Thermal aging has minimal effect on the tensile strength. The fracture properties of SS welds are insensitive to filler metal; the welding process has a significant effect. The large variability in the data makes it difficult to establish the effect of the welding process on fracture properties of SS welds. Consequently, the approach used for evaluating thermal and neutron embrittlement of austenitic SS welds relies on establishing a lower-bound fracture toughness J-R curve for unaged and aged, and non-irradiated and irradiated, SS welds. The existing fracture toughness J-R curve data for SS welds have been reviewed and evaluated to define lower-bound J-R curve for submerged arc (SA)/shielded metal arc (SMA)/manual metal arc (MMA) welds and gas tungsten arc (GTA)/tungsten inert gas (TIG) welds in the unaged and aged conditions. At reactor temperatures, the fracture toughness of GTA/TIG welds is a factor of about 2.3 higher than that of SA/SMA/MMA welds. Thermal aging decreases the fracture toughness by about 20%. The potential combined effects of thermal and neutron embrittlement of austenitic SS welds are also described. Lower-bound curves are presented that define the change in coefficient C and exponent n of the power-law J-R curve and the JIc value for SS welds as a function of neutron dose. The potential effects of reactor coolant environment on the fracture toughness of austenitic SS welds are also discussed.

Chopra, O. K.↗

DOE OSTI2020

Controllable Solar Flux Heating for Freeze Recovery in Molten Salt Parabolic Trough Collectors

In molten-salt parabolic trough plants, the melting process is particularly important for freeze recovery of salt that is solidified in a collector loop, should such an event occur. Currently impedance heating is expected for freeze recovery of the collector loops, but this method can be expensive. Here, a lower-cost alternative is proposed to use controllable concentrated solar flux directly from the parabolic mirrors to thaw salt that is frozen in the collector. A computational fluid dynamics model was developed to explore the solidification and melting processes of molten salt in a parabolic trough receiver and to assess the viability of this concept. Results indicate that concentrated solar heating has the potential to melt frozen salt in 5.6 h, compared to that in 8.8 h for a 300 W m –1 impedance heating system. At the same time, controllable solar flux heating introduces nonuniform solar fluxes on the receiver surface, which can induce significant thermal stress on the receiver tube. A preliminary stress analysis indicates that the temperature difference across the receiver tube should be maintained below about 70 °C for heating up to 300 °C at internal pressures ≤10 bar. At these conditions, freeze recovery using solar flux heating will not significantly affect receiver lifetime. These results suggest that controllable solar flux heating could effectively supplement or replace impedance heating in the freeze recovery system. Incorporating this methodology in future parabolic trough concentrating solar power plants is an opportunity for capital and operational cost-savings.

14 SOLAR ENERGY↗

DOE OSTI2020

Experimental Analysis of Salt Hydrate Latent Heat Thermal Energy Storage System With Porous Aluminum Fabric and Salt Hydrate as Phase Change Material With Enhanced Stability and Supercooling

Phase change materials (PCMs), especially salt hydrates possess high volumetric energy storage capacity in their transition temperature range. These materials are used in applications where it is necessary to store thermal energy due to temporary load shift between demand and availability. Thus, possible applications are HVAC, recovery of waste heat, and defense thermal management. Despite salt hydrates potential, the practical feasibility of latent heat storage with salt hydrates is limited due to low power rating, supercooling, phase segregation, and long-term stability. Its low power rating and long-term stability limits its application in most applications. This work experimentally validates the stability and thermal performance of a compact heat exchanger charged with salt hydrate during melting and freezing. The compact heat exchanger was designed with fins on both the heat transfer fluid (HTF) and salt hydrate PCM side. The thermal performance of the latent heat thermal energy storage system (LHTESS) was evaluated for various operating conditions. The results show that LHTESS could achieve an average heat transfer coefficient of 124 and 87 W/(m2 K) during melting and solidification, respectively. The stability of the system in suppressing supercooling was validated over 800 cycles with nucleating agent and active homogenous nucleation techniques. The supercooling was reduced to 3 °C with zinc hydroxyl nitrate as nucleating agent and less than 1 °C with the active homogenous nucleation technique. The LHTESS showed less than 6% degradation in energy storage capacity over 800 cycles.

42 ENGINEERING↗

DOE OSTI2024

Development of Modified Perturbation Solutions to the One-Phase Stefan Problems With a Convective Boundary

The classical Stefan problem is used to track the moving solid-liquid interface during the freezing process. Perturbation theory has often been applied to find an approximate analytical solution due to the nonlinearity of the moving interface. However, the Stefan number (i.e., the sensible over latent heat) must be small and usually less than 0.01 to assume the perturbation expansion, which in turn limits the thermal engineering applications. In this study, a modified perturbation solution is developed by adding a correction term after the leading-order solution to be valid for a much wider range of Stefan numbers (i.e., 0.01 less than or equal to Ste less than or equal to 1). Specifically, a one-phase Stefan problem is first formulated subjected to a convective boundary in the Cartesian, cylindrical, and spherical coordinate systems for inward solidification. The leading-order solution is calculated based on the regular perturbation theory, while the correction term is obtained using the Monte-Carlo method and a multi-variant regression. Results show that the correction term has a linear relationship with the Stefan number and is not significantly influenced by the Biot number. The proposed modified perturbation solution can accurately and rapidly predict the nonlinear moving interface motion for the freezing process.

DIRECT ENERGY CONVERSION,MATHEMATICS AND COMPUTING↗

DOE OSTI2024

Analytical Modeling of Metal Foam Composite Phase Change Materials (PCM) in Thermal Energy Storage Using Asymptotic Analysis

The use of phase change materials (PCMs) for thermal energy storage can release or absorb a significant amount of latent heat during the freezing or melting process, offering a higher energy storage density. One of the main drawbacks of PCMs is their low thermal conductivity, resulting in poor thermal performance. Recent research has attempted to enhance heat transfer and increase the thermal conductivity of PCMs, including the use of metal foams. However, modeling the metal foam composite PCM using conventional methods is computationally expensive. This paper proposes an asymptotic solution for a Stefan-like problem subject to a convective boundary for outward solidification in a hollow cylinder, capable of predicting the freeze-melt cycle of the metal foam composite PCM. Specifically, three temporal regimes and four spatial layers are considered in the asymptotic analysis for each phase change process. The thermal conductivity is calculated by a theoretical three-dimensional tetrakaidecahedron model, while other thermophysical properties are obtained using the method of volume averaging. The results are verified with numerical data and validated against experimental data in the literature. The presented analytical modeling framework could have the potential to be applied to other types of composite PCMs with considerably lower computational costs compared with conventional methods.

analytical model↗

DOE OSTI2026

Enabling On-Demand Aerospace Component Manufacturing: Topology Optimization of GE Engine Bracket and Fabrication Using Metal FFF

Additive Manufacturing (AM) offers advantages over conventional manufacturing processes, particularly by reducing the number of parts produced through multistage combined technologies, but these often result in low manufacturing yields or require post-processing. AM facilitates the production of complex geometries with fine features, overhangs, and lattice structures. For instance, Laser Powder Bed Fusion (LPBF) technology enables the fabrication of intricate parts that can be easily post-processed by removing residual powder. Laser powder bed AM technologies are widely discussed in the literature due to their design freedom in creating complex geometries, with and without the need for support generation. However, rapid solidification due to a thermal gradient in the build direction, which leads to the formation of columnar grains and warpage, is one of the challenges. To address this challenge, we propose layer-by-layer metal FFF technology, followed by the debinding and sintering process, as an alternative to powder- and laser-based approaches. Furthermore, design for additive manufacturing (DfAM) principles are discussed to minimize the need for support generation and enable easy post-processing, thereby improving surface finish to meet high tolerances in fabricating components for aerospace and healthcare applications.

Singh, Abhishek [University of Michigan, Ann Arbor↗

DOE OSTI2022

Analysis of Conduction Cooling Strategies for Wire Arc Additive Manufacturing

Metal additive manufacturing (AM) processing consists of numerous parameters which take time to optimize for various geometries. One aspect of the metal AM process that continues to be explored is the control of thermal energy accumulation during component manufacturing due to the melting and solidification of the feedstock. Excessive energy accumulation causes thermal failure of the component while minimal energy accumulation causes lack of fusion with the build plate or previous layer. The ability to simulate the thermal response of an AM component can increase research efficiency by reducing the time to optimize thermal energy accumulation. This paper presents an effective implementation of finite element analysis to determine the thermal response of a wire arc additive manufactured component with various build plate sizes and cooling methods including, integral build plate cooling, oversized build plates with passive cooling, and non-integral build plate cooling. The use of integral build plate cooling channels was shown to decrease the interpass temperature at the conclusion of the build process by 55% and build plate temperature by 96% compared to the conventionally deposited sample with 20 second dwell time. The use of a tall build plate with passive cooling was shown to reduce the interpass temperature by 32% as compared to the conventionally deposited sample with 20 second dwell time. Each cooling strategy evaluated decreased the interpass temperature within a range of 20–55% which enables higher deposition rates and decreased dwell times during depositions. The cooling strategies are designed to be implemented in a hybrid or retrofit AM platform to mitigate concerns of the thermal input from the additive process having detrimental effects on the precision of the machining process. This paper shows that accurate simulations of all strategies can be used to accurately predict the thermal response of the various strategies discussed. These cooling strategies will allow for increased deposition rates with comparable interpass temperature and decreased dwell time, increasing deposition efficiency. This model and these simulations are verified by experimental results. It is concluded that passive strategies, such as the over-sized tall build plate, can be used when liquid coolant in the AM environment could negatively affect the deposition process. Active cooling strategies, such as the integral build plate cooling could be used if low thermal conductivity materials are deposited or higher material deposition rates are desired. This paper discusses the use of active and passive cooling used during AM and shows how a simulation model can be used to make design choices for cooling strategies. The model also enables verification of select critical process parameters such as dwell times for a desired interpass temperature.

Heinrich, Lauren↗

DOE OSTI2017

Bright and durable field-emission source derived from frozen refractory-metal Taylor cones

A novel method for creating conical field-emission structures possessing unusual and desirable physical characteristics is described. This process is accomplished by solidification of electrostatically formed high-temperature Taylor cones created on the ends of laser melted refractory-metal wires. Extremely rapid freezing ensures that the resultant solid structures preserve the shape and surface smoothness of the flawless liquid Taylor-cones to a very high degree. The method also enables in situ and rapid restoration of the frozen cones to their initial pristine state after undergoing physical degradation during use. This permits maximum current to be delivered without excessive concern for any associated reduction in field-emitter lifetime resulting from operation near or even above the damage threshold. In addition to the production of field emitters using polycrystalline wires as a substrate, the feasibility of producing monocrystalline frozen Taylor-cones having reproducible crystal orientation by growth on single-crystal wires was demonstrated. Finally, the development of the basic field-emission technology, progress to incorporate it into a pulsed electron gun employing laser-assisted field emission for ultrafast experiments, and some additional advances and opportunities are discussed.

36 MATERIALS SCIENCE↗