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At least 109 records · Page 6

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DOE OSTI2024

On the Mechanical Behavior of LP-DED C103 Thin-Wall Structures

Laser Powder Directed Energy Deposition (LP-DED) can produce thin-wall features on the order of 1 mm. These features are essential for large structures operating in extreme environments such as regeneratively cooled nozzles and heat exchangers, which often make use of refractory metals. In this work, the mechanical behavior of LP-DED C103 was investigated via quasi-static tensile testing and low cycle fatigue (LCF) testing. The effects of vacuum stress relief (SR) and hot isostatic pressing (HIP) heat treatments were investigated for specimens in the vertical and horizontal build orientations during tensile testing. The AB and SR properties were lower than literature values for wrought and laser powder bed fusion (L-PBF) bulk components but higher than electron beam powder bed fusion (EB-PBF). The application of a HIP cycle improved strength by 7% and ductility by 27% past the initial as-built condition. Fracture images reveal that interlayer stress concentration sites are responsible for fracture in specimens in the vertical orientation. Meanwhile, fracture in the horizontal specimens mainly propagates at a slanted angle typical of plane stress conditions. The LCF results show cycles to failure ranging from 100 cycles to 8000 cycles for max strain levels of 2% and 0.5%, respectively. Fractography on the fatigue specimens reveals an increasing propagation zone as max strain levels are increased. The impact of these findings and future work are discussed in detail.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Systems and devices for pumping and controlling high temperature fluids

The disclosed technology includes pumps, pipes, valves, seals, and systems for pumping and controlling high temperature fluids, such as liquid tin, at temperatures of between 1000-3000° C. The systems and device may be partially or entirely constructed using brittle materials, such as ceramics, that are capable of withstanding extreme heat without significantly degrading, and may be secured using components made of refractory metals, such as tungsten. The systems and devices may utilize static and dynamic seals made from brittle materials, such as graphite, to enable the high temperature operation of such pumps, pipes, valves, and systems without leakage.

Henry, Asegun↗

DOE OSTI2022

Additive manufacturing of complex objects using refractory matrix materials

A method for the manufacture of a three-dimensional object using a refractory matrix material is provided. The method includes the additive manufacture of a green body from a powder-based refractory matrix material followed by densification via chemical vapor infiltration (CVI). The refractory matrix material can be a refractory ceramic (e.g., silicon carbide, zirconium carbide, or graphite) or a refractory metal (e.g., molybdenum or tungsten). In one embodiment, the matrix material is deposited according to a binder-jet printing process to produce a green body having a complex geometry. The CVI process increases its density, provides a hermetic seal, and yields an object with mechanical integrity. The residual binder content dissociates and is removed from the green body prior to the start of the CVI process as temperatures increase in the CVI reactor. The CVI process selective deposits a fully dense coating on all internal and external surfaces of the finished object.

Terrani, Kurt A.↗

DOE OSTI2023

Permanent magnet alloys for gap magnets

Provided are Ce/Co/Cu permanent magnet alloys containing certain refractory metals, such as Ta and/or Hf, and optionally Fe which represent economically more favorable alternative to Sm-based magnets with respect to both material and processing costs and which retain and/or improve magnetic characteristics useful for GAP MAGNET applications.

Palasyuk, Andriy↗

DOE OSTI2024

Nuclear Data Sensitivity/Uncertainty Studies of Tantalum-Reflected Systems

Tantalum (Ta) is a refractory metal with high melting point and high corrosion resistance. This makes it useful as a mold material for plutonium casting operations. Unfortunately, there are few criticality benchmarks with high nuclear data sensitivities. Given that, it is desirable to design new experiments to provide additional validation data for nuclear criticality safety, which is the objective of the Thales project. Multiple application models were used to represent process conditions (either normal conditions or credible upset conditions) both at Los Alamos National Laboratory (LANL) and Savannah River Site (SRS). A total of 40 application models were obtained. Given this, it was useful to down-select the number of needed application models. This work documents the down-selection based on several nuclear data sensitivity/uncertainty metrics. In addition to showing the result of the specific down-selection used for the Thales project, this work discusses potential ways to represent a large number of application models with a smaller number of proposed experiment designs.

42 ENGINEERING↗

DOE OSTI2024

Additive manufacturing of complex objects using refractory matrix materials

Terrani, Kurt A.↗

DOE OSTI2020

Laser metal deposition of refractory high-entropy alloys for high-throughput synthesis and structure-property characterization

Progress in materials development is often paced by the time required to produce and evaluate a large number of alloys with different chemical compositions. This applies especially to refractory high-entropy alloys (RHEAs), which are difficult to synthesize and process by conventional methods. To evaluate a possible way to accelerate the process, high-throughput laser metal deposition was used in this work to prepare a quinary RHEA, TiZrNbHfTa, as well as its quaternary and ternary subsystems by in-situ alloying of elemental powders. Compositionally graded variants of the quinary RHEA were also analyzed. Our results show that the influence of various parameters such as powder shape and purity, alloy composition, and especially the solidification range, on the processability, microstructure, porosity, and mechanical properties can be investigated rapidly. The strength of these alloys was mainly affected by the oxygen and nitrogen contents of the starting powders, while substitutional solid solution strengthening played a minor role.

additive manufacturing↗

DOE OSTI2026

Probing multi-dimensional composition spaces in search of strong metallic alloys

Refractory complex concentrated alloys (RCCA) offer exceptionally high-temperature strength compared to pure metals and dilute alloys, but predictive theory for RCCA design is lacking. We present large-scale molecular Dynamics (MD) simulations of crystal plasticity to explore alloy compositions for maximum mechanical strength, focusing on Fe-Ta-W and Nb-Ta-Mo-W alloy families modeled with Embedded Atom Model (EAM) and Spectral Neighbor Analysis Potentials (SNAP). To efficiently guide the search for strong alloy compositions, we employ iterative optimization using Gaussian process regression. Many simulated RCCA compositions exhibit pronounced cocktail strengthening, with strengths surpassing their strongest constituent metal, tungsten. Contrary to expectations, the highest strength is found on binary edges of the RCCA composition space. Detailed analyses of atomistic simulations reveal that, similar to pure BCC metals, plastic response in RCCA is primarily governed by screw dislocations. However, at large strains, dislocation multiplication and interactions (Taylor hardening) become the dominant mechanisms contributing to RCCA strength.

Materials science↗

DOE OSTI2024

Reduction of vanadium diffusivity within copper grain boundaries due to enhanced binding

We investigate permeation of vanadium (V) through copper (Cu) layers in V/Cu/niobium (Nb) and molybdenum (Mo)/Cu/V tri-layer composites and compare it with the permeation behavior of Nb. Despite their low solubility in single-crystal Cu, both V and Nb permeate readily due to short-circuit transport through Cu grain boundaries (GBs). However, Nb permeates preferentially to V. Atomistic simulations suggest that this difference is due to lower V diffusivity at general GBs in Cu, compared to Nb. Here, the lower V diffusivity, in turn, arises from stronger V binding to the boundary, which manifests as a greater equilibrium GB concentration as well as a higher activation energy for GB diffusion.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Development of Refractory Alloys and Refractory Coatings for Advanced Nuclear Reactors

The next generation of nuclear reactors will benefit from materials that enable operation at higher temperatures (>500°C), higher irradiation doses (up to 200 displacements per atom (dpa)), and the use of more corrosive and reactive coolants. This work package represents the first experimental steps towards a longer-term effort to develop refractory materials for nuclear energy applications which will enable operation under these conditions. Specifically, this work package focuses on additive manufacturing of refractories as both a refractory liner coating deposited onto the interior surface of a metallic tubular backbone and as bulk refractory alloys. During fiscal year 23 (FY23), several refractory metal coating systems and bulk alloys were examined and selected using a decision criteria matrix. The refractory metal coating systems included molybdenum, tungsten, and zirconium as refractory coatings on backbones of either carbon-carbon (C/C) or silicon carbide-silicon carbide (SiC/SiC) ceramic matrix composites. The bulk refractory alloys included C-103, WTa, and WNiFe as bulk alloys. During FY24 additional bulk refractory alloys and metallic backbones were evaluated using the decision criteria matrix based on input from the AMMT leadership team. These included 316 SS and 316H SS for the metallic backbones and Mo-La, Ta, and Nb1Zr as bulk refractory alloys. The primary focus for the FY24 effort was placed on establishing the capabilities to deposit refractory coatings based on the results of the scoring in the decision criteria matrix and finalizing the additively manufactured TZM studies which were incorporated into the AMMT program from the microreactor program. Further efforts were dedicated to establishing the capabilities to additively manufacture down-selected bulk refractory alloys.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2023

Novel refractory high-entropy metal-ceramic composites with superior mechanical properties

A new concept of refractory high-entropy metal-ceramic composites (HEMCC) has been proposed that combines the outstanding physical properties of both high-entropy alloy (HEA) and high-entropy ceramic (HEC). As the first HEMCC system, to the best of our knowledge, TiTaNbZr-(TiTaNbZr)C, has been developed by a powder metallurgy process. The HEA and HEC phases exhibit body-centered cubic (BCC) and rock-salt B1 crystal structures, respectively, and both phases have non-equimolar chemical compositions. Further, with the increase of the HEC phase in HEMCC, the hardness is enhanced while the density and fracture toughness are decreased. HEA50C sintered from 50vol% HEA and 50vol% HEC precursor powders shows a favorable combination of flexural strength (541±48MPa) and fracture toughness (6.93±0.27 MPa·m 1/2 ) at room temperature and a high compressive strength at 1300ºC (275MPa). The optimized mechanical performance of HEMCC might be attributed to the combination of the ductile HEA and strong HEC phases, smaller grain size, and crack arrest at HEC/HEA interfaces.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Interaction mechanism of transition metal phthalocyanines on transition metal nitride supports

Here, we investigated the electronic interactions between transition metal phthalocyanine (TMPc’s) on a refractory transition metal nitride support, specifically copper phthalocyanine (CuPc) on titanium nitride (TiN). X-ray Photoelectron Spectroscopy (XPS) results suggest a presence of a few nanometer native oxide layer on the surface of the TiN nanoparticles, which consists of TiN, TiO 2 , and Titanium oxynitrides (Ti x O y N z ). A TiNCuPc nanocomposite was synthesized via a simple mixing method due to the strong binding between CuPc and TiN confirmed by density functional theory (DFT) calculations. Both XPS data and DFT calculations revealed an electron transfer from TiN substrate to CuPc molecule. The nature of charge transfer is not influenced by the presence of an oxide layer on the surface of TiN. Substantial deviations are however found between photoelectron emission microscopy (PEEM) measured work function for TiN (4.68 eV) and theoretically calculated work function for pristine stoichiometric TiN (2.63 eV). This behavior is attributed to the presence of an oxide layer on the TiN surface. TiNCuPc composite system has a work function value between those of TiN and CuPc. Our studies open up an opportunity to apply a new class of materials based on transition metal phthalocyanine/transition metal nitride composites to catalysis and optoelectronic devices.

36 MATERIALS SCIENCE↗

DOE OSTI2023

EB Vs PAM Vs VAR for Uranium Alloys

Questions were raised during the February ’97 PDP Meeting at LLNL as to the advisability of funding three separate melting development programs (Advanced Vacuum Arc Remelt (VAR), Plasma Arc Melting (PAM) and Electron Beam Melting (EB)) through PDP in this era of shrinking research funds. The main issues seemed to be: 1) Have we evaluated the potentials of the three processes sufficiently to eliminate any of them out of hand and 2) Have any of these processes to date produced results which show clear advantages over the other two. The feeling at the meeting toward the latter seemed to be that all three processes required further development before they would be accepted by the complex as the standard. As far as evaluating potential for process improvements, however, we at Livermore did go through somewhat of a trade study in 1993 when we proposed the EB route. It seemed to us that even with the elimination of the skull caster via a VIM/VAR/VAR route, the problem of recycle limitations in the VIM step due to excessive carbon pick-up limited the potential for a great improvement in material utilization using this method. A single-step, cold hearth route looked to be the preferable choice. Both EB and PAM are used commercially as cold hearth processes, and both have been used for the production of refractory and specialty metals; EB since the mid 1950’s and PAM since the mid 1980’s. Both seem to have found their individual niches with some applications being suited to EB and others to PAM. Both can be adapted to continuous casting techniques and both are capable of imparting the high heat fluxes necessary to melt refractory metals. The major differences appear to be that for most applications, the EB process is capable of producing a purer product, while PAM results in less loss of volatile components. There exists an abundance of information in the open literature on the results of processing via both routes on various materials. The attached 1984 paper gives a good explanation of electron beam melting and plasma melting, and, I believe, a fair assessment of the advantages and limitations of both processes.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Effect of temperature on abrasion erosion in particle based concentrating solar powerplants

The use of solid particles as a heat transfer medium is being explored for concentrated solar power plants (CSP) to increase their efficiency by achieving operating temperature >700 °C. During operation, these hot particles are expected to move along the various components within the collector system, resulting in material degradation from a combination of high-temperature oxidation and erosion. In the present study, the performance of candidate materials was evaluated through a series of abrasion erosion experiments at room temperature as well as at 800 °C. Wear in metallic and refractory type materials was investigated using CarboBead® HSP 40/70 particles inside a resistance heated kiln. Furthermore, cross-sectional scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDS) analysis on the specimens tested at 800 °C determined that the specific wear rate in Inconel 740H and stainless steel 316 metallic specimens was influenced by the thermally grown oxide morphology. High chromium Inconel 740H specimens exhibited greater resistance to wear with a steady state specific wear rate of 1.92E-4 mm 3 N -1 m –1 compared to 5.7E-3 mm 3 N -1 m –1 for Stainless Steel 316.

14 SOLAR ENERGY↗

DOE OSTI2023

Computational discovery of ultra-strong, stable, and lightweight refractory multi-principal element alloys. Part I: design principles and rapid down-selection

Abstract Refractory metal-based multi-principal element alloys (MPEAs) are compelling materials for high-temperature (1000–2000 K) structural applications. However, only a minuscule fraction of their vast and heterogeneous compositional design space has been explored, leaving many potentially interesting alloys undiscovered. In this two-part work, a large region of the 11-element Al-Cr-Fe-Hf-Mo-Nb-Ta-Ti-V-W-Zr design space is computationally explored to identify refractory MPEAs with simultaneously high yield strength or specific yield strength and body-centered cubic (BCC) solid solution stability. In Part I , two case studies illuminate key factors and considerations in the yield strength versus phase stability tradeoff, provide guidelines for narrowing the expansive design space, and identify many candidates predicted to be stronger than refractory MPEAs reported to date, with BCC phase stability. Our findings indicate that medium entropy ternary alloys can outperform alloys with more elements and highlight the importance of exploring regions away from the equiatomic center of composition space.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Parameter development and characterization of laser powder directed energy deposition of Nb – Alloy C103 for thin wall geometries

This work focuses on the parameter development and microstructural characterization of Nb-based alloy C103 for thin wall structures produced via laser powder – directed energy deposition (LP – DED). Laser power and scanning speeds were varied as part of a design of experiments to identify adequate print parameters. Combinations were evaluated for relative density, porosity, and geometrical accuracy. A combination of a laser power of 1420 W and scanning speed of 14 mm/s resulted in a relative density >99%, exhibited a consistent weld bead profile and was used for further microstructural evaluation. A mix of optical and scanning electron microscopy (SEM) revealed small, slightly elongated grains along the edges and large epitaxial grains in the central region along the Build – Transverse view. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) analysis revealed Hf rich columnar cells in the center that transition into an evenly spaced cellular structure towards the edges of the built sample. Electron backscatter diffraction (EBSD) scans show a sharp [001] texture when looking at the cross section of the sample along the build direction. The Build – Scan view revealed a zig – zag pattern that follows the back – and – forth deposition strategy that was used. Finally, microhardness measurements were taken in the as – built (AB) and stress relieved (SR) conditions to baseline preliminary mechanical properties. The AB condition exhibited a large amount of scatter in the data and averages up to 11% larger than the SR condition. The reduction in scatter upon applying the SR cycle are indicative of a large concertation of dislocations present in the AB condition.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Effect of alloying on intrinsic ductility in WTaCrV high entropy alloys

Tungsten (W) exhibits desirable properties for extreme applications, such as the divertor in magnetic fusion reactors, but its practicality remains limited due to poor formability and insufficient irradiation resistance. In this work, we study the intrinsic ductility of body-centered cubic WTaCrV based high entropy alloys (HEAs), which are known to exhibit excellent irradiation resistance. The ductility evaluations are carried out using a criterion based on the competition between the critical stress intensity factors for emission (K Ie ) and cleavage (K Ic ) in the {110} slip planes and {110} crack planes, which are evaluated within the linear elastic fracture mechanics framework and computed using density functional theory. The results suggest that increasing the alloying concentrations of V and reducing the concentrations of W can significantly improve the ductility in these HEAs. The elastic anisotropy for these HEAs is analyzed using the Zener anisotropy ratio and its correlation with the concentration of W in the alloys is studied. Results indicate that these alloys tend to be fairly isotropic independently from the concentration of W in them. The computed data for the elastic constants of these HEAs is also compared against available experimental data. The results are in good agreement, validating the robustness and accuracy of the computational methods. Multiple phenomenological ductility metrics were also computed and analyzed against the analytical model. Some metrics, mainly the surrogate D parameter, show a good correlation with the Rice model. The potential of these empirical metrics to serve as surrogate screening models for optimizing the compositional space is also discussed.

Anisotropy↗

DOE OSTI2025

Solidification behavior and cracking mechanisms of Ru-containing BCC-B2 superalloys

Many precipitation-strengthened alloys are highly susceptible to cracking during additive manufacturing (AM), which often requires compositional adjustments to mitigate. Recently, it has been demonstrated that refractory BCC alloys can be precipitation strengthened with ordered Ru-containing B2 precipitates to temperatures exceeding 1200 °C. This motivates a study of the potential fabricability of quaternary and quinary refractory BCC-B2 alloys by AM using single track laser experiments. Alloys with greater than 9 at.% Ru exhibit crack formation upon cooling. Solidification cracking was observed in all Zr-containing alloys, which can be mitigated by substituting Hf. Furthermore, this cracking is attributed to the strong partitioning of Zr during solidification, as revealed by characterization of alloy solidus, liquidus, and partition coefficients. Hf 5 Ru 4 -Nb 63 V 28 is identified as a promising BCC-B2 composition with a high B2 solvus (>1300 °C) and solidus (1695 °C) along with a high resistance to cracking.

36 MATERIALS SCIENCE↗