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DOE OSTI2024

A Microchannel Heat Exchanger Produced From a Metal Matrix Composite by Hybrid Laser Powder Bed Fusion and Inkjet Printing

Abstract This paper explores the production of an oxide dispersion strengthened (ODS) 304L stainless steel microchannel heat exchanger (HX) using a hybrid additive manufacturing process of laser powder bed fusion and inkjet printing. The study investigates the capabilities and economics of the hybrid inkjet-laser powder bed fusion (LPBF) process and evaluates the dimensional accuracy, functionality, and mechanical properties of the resulting ODS alloy. The effectiveness and pressure drop of the ODS heat exchangers produced by the hybrid LPBF tool are also determined. Results show that the inkjet-doped samples have a lower mean channel height with higher standard deviation than samples produced by LPBF alone. This is attributed to greater absorption of laser energy for the powder coated with the oxide precursor. The economic analysis shows that the hybrid process has a potential for reducing the unit cost of the heat exchanger based on cost modeling assumptions.

Engineering↗

DOE OSTI2025

Development and Validation of MALAMUTE model for Electric Field Assisted Sintering of Structural Materials

Fusion power plant designs feature extreme material performance requirements for structural material candidates. In addition to conventional alloys, more advanced composites and oxide dispersion strengthened (ODS) alloys are being explored, however, achieving the desired microstructures to maximize performance using traditional manufacturing methods can be challenging. The advanced manufacturing (AM) electric field-assisted sintering (EFAS) technique offers improved control over the final microstructure through higher heating and cooling rates and moderate pressures. Modeling and simulation tools show promise in elucidating the process-structure-property-performance (PSPP) correlation for AM-produced parts, including the EFAS process. An inherently multiscale process, the EFAS technique aligns well with the multiscale modeling capability of the open-source Multiphysics Object-Oriented Simulation Environment (MOOSE)[cite]. We present here an electro-thermo-mechanical approach to modeling the EFAS process using the MOOSE Application Library for Advanced Manufacturing UTilitiEs (MALAMUTE) code. Prediction of the field and gradient distributions across the EFAS tooling is required to accurately describe the conditions for the lower-scale microstructural evolution models. In this work we present the MALAMUTE model developed to predict the electrical potential, temperature, and mechanical stress distribution across the EFAS graphite tooling and part at the larger engineering-scale. Validation of the MALAMUTE engineering-scale model is completed using data from experimental densification and pre-densified runs of iron powder via EFAS at 1000oC. These runs were conducted using a Thermal Technology DCS-5 EFAS system. Data collected during the experiment runs include the direct current (DC) supplied to the graphite tooling, the temperature of the graphite tooling as measured with a pyrometer, and the force applied to the top of the graphite tooling stack, and the data were recorded every 10 seconds. Our validation approach used the current and force data from the EFAS run as boundary condition inputs to the MAMALUTE simulation; the temperature data were used to evaluate the MALAMUTE EFAS model prediction. Results of the MALAMUTE simulations are employed to connect the external pyrometer temperature measurement to the temperature profile across the part undergoing consolidation. We investigate the impact of material property variation and mesh deformation on the temperature profile as predicted by MALAMUTE. We conclude by highlighting projects where the MALAMUTE EFAS modeling and simulation capabilities will be used to assist experimental design.

36 - MATERIALS SCIENCE↗

DOE OSTI2020

Oxide dispersoid coherency of a ferritic-martensitic 12Cr oxide-dispersion-strengthened alloy under self-ion irradiation

Ferritic-martensitic oxide-dispersion-strengthened (ODS) alloy has shown excellent mechanical property and high radiation tolerance. However, the stability of dispersoids during displacive irradiation in the individual ferritic and martensitic phases is unclear. In this work, the correlation among dispersoid coherency, size, density, and matrix phase are studied in dual-phase 12Cr ODS after 100 peak displacements-per-atom (dpa) irradiation at 475°C, using 3.5 MeV Fe 2+ self-ions. The size and density changes of coherent and incoherent dispersoids were analyzed as a function of irradiation depth. The average dispersoid size decreased after irradiation in both phases, and the large incoherent dispersoids in the tempered martensite phase underwent a more dramatic change than those in the ferrite phase. The dispersoid density significantly increased in the ferrite phase within the irradiated region, mostly resulting in an increase in coherent dispersoid density. On the other hand, only a small change in density was observed in the tempered martensite phase for both coherent and incoherent dispersoids. This study shows that dispersoid evolution is dramatically different in ferrite and tempered martensite phases.

36 MATERIALS SCIENCE↗

NASA NTRS2024

Extreme Temperature Additively Manufactured GRX-810 Alloy Development and Hot-fire Testing for Liquid Rocket Engines

Additive manufacturing (AM) has revolutionized component design for liquid rocket engines by offering rapid manufacturing capabilities. This has led to significant opportunities for development and flight programs in the propulsion industry, resulting in cost and schedule savings, as well as performance improvements through new designs and alloy development. A noteworthy example is the GRX-810 oxide dispersion strengthened (ODS) alloy, which was specifically developed for extreme temperatures. This Ni-Co-Cr based alloy was created using integrated computational materials engineering (ICME) techniques to focus on a new class of materials with exceptional temperature and oxidation-resistant properties. The GRX-810 alloy utilizes AM processes to incorporate nano-scale yttria particles throughout its microstructure, resulting in remarkable enhancements. Compared to traditional Nickel-based superalloys, the GRX-810 alloy offers a two-fold increase in tensile strength, 1,000-fold better creep properties, and two-fold improvement in oxidation resistance. NASA successfully demonstrated the development and manufacturing of components using the GRX-810 alloy through laser powder bed fusion (L-PBF) and laser powder directed energy deposition (LP-DED) processes. Extensive efforts were made to model, evaluate metallurgical properties, develop heat treatment processes, characterize the microstructure, and determine mechanical properties. The GRX-810 alloy was specifically designed for aerospace applications, including liquid rocket engine injectors, preburners, turbines, and hot-section components, capable of withstanding temperatures up to 1,100 °C. The objective of this alloy development is to bridge the temperature gap between traditional Nickel-based superalloys and refractory alloys. This paper provides a comprehensive comparison of the GRX-810 alloy with other aerospace alloys, discussing its microstructure, mechanical properties, processing advancements, component development, and hot-fire testing results. The ultimate goal of this development was to elevate the Technology Readiness Level (TRL) of the GRX-810 alloy, enabling its integration into NASA and commercial aerospace applications.

GRX-810↗

NASA NTRS2024

Extreme Temperature Additively Manufactured GRX-810 Alloy Development and Hot-fire Testing for Liquid Rocket Engines

GRX-810↗

DOE OSTI2024

Transmission electron microscopy of ion irradiated ODS MA956 samples

Oxide dispersion strengthened (ODS) alloys are promising candidate materials for the next generation advanced nuclear reactors due to their superior irradiation resistance and mechanical properties. To better understand the effect of irradiation on MA956, it is essential to study higher dose (50-100 dpa) samples, so that the general trend of microstructural evolution and the resulting radiation-hardening can be deduced. Currently, ion irradiations are considered the only way to achieve doses beyond ~50 dpa in a practical time frame relevant to alloy and welding development programs. This dataset contains TEM characterization results of ODS MA956 samples that were ion irradiated under different conditions: Sample #5 (1.25 dpa at 190℃); Sample #9 (50 dpa at 190℃); Sample #15 (1.25dpa under 320℃); and Sample 17 (25 dpa at 320℃). TEM characterization focused on the irradiation induced defects (dislocation lines and loops) using the on-zone axis bright field STEM technique. These data were collected using a FEI Tecnai G2 F30 S/TEM at Microscopy and Characterization Suite (MaCS) at Center for Advanced Energy Studies (CAES), Idaho Falls, ID. This project (ion irradiation and TEM studies) was supported by the U.S. Department of Energy, Office of Nuclear Energy under DOE Idaho Operations Office Contract DE-AC07-05ID14517 as part of Nuclear Science User Facilities award #18-14784 (PI: Ramprashad Prabhakaran, PNNL).

Prabhakaran, Ramprashad↗

NASA NTRS1977

Progress in advanced high temperature turbine materials, coatings, and technology

Several NASA-sponsored benefit-cost studies have shown that very substantial benefits can be obtained by increasing material capability for aircraft gas turbines. Prealloyed powder processing holds promise for providing superalloys with increased strength for turbine disk applications. The developement of advanced powder metallurgy disk alloys must be based on a design of optimum processing and heat treating procedures. Materials considered for high temperature application include oxide dispersion strengthened (ODS) alloys, directionally solidified superalloys, ceramics, directionally solidified eutectics, materials combining the high strength of a gamma prime strengthened alloy with the elevated temperature strength of an ODS, and composites. Attention is also given to the use of high pressure turbine seals, approaches for promoting environmental protection, and turbine cooling technology.

Freche, J. C.↗

NASA NTRS1982

Energy efficient engine high pressure turbine test hardware detailed design report

The high pressure turbine configuration for the Energy Efficient Engine is built around a two-stage design system. Moderate aerodynamic loading for both stages is used to achieve the high level of turbine efficiency. Flowpath components are designed for 18,000 hours of life, while the static and rotating structures are designed for 36,000 hours of engine operation. Both stages of turbine blades and vanes are air-cooled incorporating advanced state of the art in cooling technology. Direct solidification (DS) alloys are used for blades and one stage of vanes, and an oxide dispersion system (ODS) alloy is used for the Stage 1 nozzle airfoils. Ceramic shrouds are used as the material composition for the Stage 1 shroud. An active clearance control (ACC) system is used to control the blade tip to shroud clearances for both stages. Fan air is used to impinge on the shroud casing support rings, thereby controlling the growth rate of the shroud. This procedure allows close clearance control while minimizing blade tip to shroud rubs.

Halila, E. E.↗

DOE OSTI2020

The effect of Zr on precipitation in oxide dispersion strengthened FeCrAl alloys

Oxide dispersion strengthened (ODS) FeCrAl alloys are promising candidate materials for advanced nuclear reactor applications requiring high-temperature strength, corrosion resistance, and irradiation tolerance. As these alloys have increased in compositional complexity through attempts to use highly reactive elements such as Zr to refine particle sizes and optimize nanoprecipitate dispersion characteristics, much debate has ensued as to the effects of these alloying element additions on alloy properties. In an attempt to reconcile differences in nanoprecipitate distributions reported in the literature over the past decade, a detailed investigation of a recently developed ODS FeCrAl alloy with nominal composition Fe–10Cr-6.1Al-0.3Zr+0.3Y 2 O 3 is presented here using a combination of atom probe tomography (APT), scanning/transmission electron microscopy (S/TEM), and computational thermodynamics modeling. It is illustrated that based on the amount of Zr available in the lattice, Zr competes with Al and Cr to form carbides and nitrides as opposed to oxygen-rich precipitates. This alloy system has a high number density (>10 23 m -3 ) of ~2–4 nm diameter (Y,Al,O)-rich nanoprecipitates, but it is shown that due to the compositional spread and unknown partitioning of Al between the matrix and precipitates, significant challenges still exist for quantifying the exact compositions of these precipitates using APT. However, the noted compositional spread is supported by identified complex oxides yttrium aluminum monoclinic (YAM) and yttrium aluminum garnet (YAG) using S/TEM. As a result of these findings, researchers developing ODS FeCrAl with reactive element additions must pay careful attention to C and N impurities when optimizing reactive element additions.

electron microscopy↗

DOE OSTI2022

Friction stir welding and self-ion irradiation effects on microstructure and mechanical properties changes within oxide dispersion strengthened steel $\mathrm{MA956}$

We report the joining process for oxide dispersion strengthened (ODS) alloys remains a key challenge facing the nuclear community. The microstructure and mechanical properties were characterized in the base material and friction stir welded ODS MA956 irradiated with 5 MeV Fe 2+ ions from 400 to 500°C up to 25 dpa. Nanoindentation was performed to assess changes in hardness and yield stress, and the dispersed barrier hardening (DBH) model was applied to described results. A combination of scanning transmission electron microscopy (STEM) and atom probe tomography (APT) were used to assess evolution of the microstructure including dispersoids, network dislocations and dislocation loops, nanoclusters, and solid solution concentrations. Overall, softening was observed as a result of increased dose, which was exacerbated at 500°C. The formation and coarsening of new dispersoids was noted while nanoclusters tended to dissolve in the base material, and were not observed in the stir zone. Solute nanocluster evolution was identified as a primary driver of the changes in mechanical properties.

36 MATERIALS SCIENCE↗

NASA NTRS1988

Low cycle fatigue

The papers contained in this volume focus on various aspects of low cycle fatigue, including cyclic deformation, crack propagation, high-temperature low cycle fatigue, microstructural defects, multiaxial and variable amplitude loading, and life prediction. Papers are presented on the low cycle fatigue of some aluminum alloys, prediction of crack growth under creep-fatigue loading conditions, high-temperature low cycle fatigue behavior and lifetime prediction of a nickel-base ODS alloy, and an integrated approach to creep-fatigue life prediction. Other topics discussed include thermal fatigue testing of coated monocrystalline superalloys, low cycle fatigue of Al-Mg-Si alloys, and the effect of superimposed stresses at high frequency on low cycle fatigue.

Solomon, H. D.↗

DOE OSTI2020

Microstructures and mechanical properties of a modified 9Cr ferritic-martensitic steel in the as-built condition after additive manufacturing

A newly developed nano-structured high-Mn 9Cr ferritic-martensitic (FM) steel designed for additive manufacturing (Additive-manufactured Nanostructured Alloy, ANA) was fabricated via the direct energy deposition method. The as-printed ANA2 showed tensile properties (strength and elongation) and Charpy impact toughness (upper-shelf energy and ductile-brittle transition temperature) comparable to oxide-dispersion-strengthened (ODS) Eurofer and PM2000. Compared with wrought P91, the as-built ANA2 showed significantly higher yield strength but inferior Charpy impact toughness and ductility. Microstructural characterization revealed uniformly distributed sub-micron pores, an extremely high dislocation density, and a high density of ultrafine nano-structured precipitates in the matrix. The microstructures indicated the dislocations as the dominant strengthening element and the ultrafine precipitates as the primary contribution to estimated irradiation sink density. This work demonstrates the ability to exploit the unique consolidation properties of additive manufacturing to fabricate steels which marry the benefits of both ODS alloys and conventionally processed FM steels.

36 MATERIALS SCIENCE↗

NASA NTRS2002

Oxidation of Copper Alloy Candidates for Rocket Engine Applications

The gateway to affordable and reliable space transportation in the near future remains long-lived rocket-based propulsion systems; and because of their high conductivities, copper alloys remain the best materials for lining rocket engines and dissipating their enormous thermal loads. However, Cu and its alloys are prone to oxidative degradation -- especially via the ratcheting phenomenon of blanching, which occurs in situations where the local ambient can oscillate between oxidation and reduction, as it does in a H2/02- fuelled rocket engine. Accordingly, resistance to blanching degradation is one of the key requirements for the next generation of reusable launch vehicle (RLV) liner materials. Candidate copper alloys have been studied with a view to comparing their oxidation behavior, and hence resistance to blanching, in ambients corresponding to conditions expected in rocket engine service. These candidate materials include GRCop-84 and GRCop-42 (Cu - Cr-8 - Nb-4 and Cu - Cr-4 - Nb-2 respectively); NARloy-Z (Cu-3%Ag-0.5%Y), and GlidCop (Cu-O.l5%Al2O3 ODS alloy); they represent different approaches to improving the mechanical properties of Cu without incurring a large drop in thermal conductivity. Pure Cu (OFHC-Cu) was included in the study to provide a baseline for comparison. The samples were exposed for 10 hours in the TGA to oxygen partial pressures ranging from 322 ppm to 1.0 atmosphere and at temperatures of up to 700 C, and examined by SEM-EDS and other techniques of metallography. This paper will summarize the results obtained.

Ogbuji, Linus U. Thomas↗

DOE OSTI2026

Irradiation of Advanced Cladding Specimens in the High Flux Isotope Reactor: Capsule Designs and Test Matrix

The Advanced Fuels Campaign (AFC) has initiated the Advanced Reactor Cladding (ARC) irradiation campaign to generate irradiation performance data for candidate fuel cladding concepts. The campaign includes a diverse set of ferritic/martensitic steels, oxide dispersion strengthened (ODS) alloys, FeCrAlbased alloys, coated materials, and welded cladding specimens produced through multiple US Department of Energy (DOE) programs and international collaborations. Three complementary experimental thrusts comprise the campaign: tensile testing (ARC Tensile) to rapidly screen candidate alloys, fracture toughness testing (ARC Fracture) to evaluate irradiation effects on crack resistance, and tubular weld testing (ARC Weld) to quantify irradiation-induced changes in the mechanical performance of end cap welds. This report documents the irradiation campaign design, including the selected materials, specimen types, irradiation matrix, and capsule designs for irradiation within the High Flux Isotope Reactor (HFIR). A total of 14 irradiation capsules were developed to achieve target irradiation temperatures between 300°C and 600°C and doses up to 30 dpa. Thermal analyses were performed using finite element methods to establish capsule geometries capable of achieving the desired specimen temperatures while accommodating differences in specimen geometry and material properties. The resulting capsule designs provide the basis for irradiation of the AFC-ARC experimental matrix and subsequent post-irradiation examination to assess the effects of neutron irradiation on advanced cladding materials.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1975

Deformation and annealing study of Nicraly

Extensive experiments were carried out on the ODS alloy Nicraly, (an alloy prepared by mechanical alloying and consolidating a powder blend consisting of 16% chromium, 4% aluminum, 2-3% yttria, balance nickel), in efforts to develop methods of controlling the grain size and grain shape of the material. The experiments fell into two general categories: variations in the annealing parameters using the as-extruded material as it was received, and various thermomechanical processing schedules (various combinations of cold work and annealing). Success was achieved in gaining grain size and grain shape control by annealing of the as-extruded material. By proper selection of annealing temperature and cooling rates, the grain size of the as-received material was increased almost two orders of magnitude (from an average grain dimension of 0.023 mm to 1.668 mm) while the aspect ratio was increased by some 50% (from 20:1 to 30:1). No success was achieved in gaining significant control of the grain size and shape of the material by thermo-mechanical processing.

Trela, D. M.↗

NASA NTRS2019

Additive Manufacturing of Oxide Dispersion Strengthened (ODS) Nickel-Based Superalloys

Additive manufacturing of oxide dispersion strengthened (ODS) Ni-based superalloys, via powder bed techniques, could enable near-net-shape manufacturing of intricately shaped components for aerospace applications. This has the potential to transform the design and manufacturing of hot sections of engines which face demands for ever-rising operating temperatures. The goal of this project is to lay the scientific foundation for additive manufacturing of ODS alloys. The objective of this poster is to present work to date as well as proposed future work.

Wilson, Laura G.↗

NASA NTRSDate not supplied

Scalable Variable Charge Molecular Dynamics Simulations of Metal-Oxide Systems

Interfaces between metals and oxides are an important feature in many technologically relevant materials, e.g., oxidation of metal surfaces, oxide-dispersion strengthened (ODS) alloys, dielectric components, and thermal barrier coatings among others. Experimental studies of such interfaces are challenging since the majority are buried within the bulk, making computational modeling an attractive alternative. Molecular dynamics (MD) simulations operate at the length scales relevant to many interface-mediated mechanisms, but the requisite interatomic potentials for metal-oxide systems require computationally expensive variable charge schemes to account for the disparate bonding types, thus often limiting their effectiveness. Here we introduce several improvements to the charge transfer interatomic potential (CTIP) model which enable greater computational efficiency for large scale MD simulations. Then, using a new CTIP parametrization for the Ni-O system, we demonstrate its capabilities to capture critical atomic scale mechanisms associated with metal-oxide interfaces. Long time scale simulations (>10 ns) are used to investigate high temperature oxidation and oxide precipitation from the melt, and large length scale simulations (> 1 million atoms) are used to study the interaction of dislocations with oxide particles. We have implemented the new CTIP model in the widely used, open-source MD code LAMMPS.

Gabriel Plummer↗

NASA NTRSDate not supplied

Quick and Correlative TOF-SIMS Analysis of Dispersoid Content in Powder Feedstock and Printed Oxide Dispersion Strengthened Alloys

Oxide dispersion strengthening (ODS) of metal alloys, when combined with additive manufacturing (AM), can be used to solve high-temperature material application problems. The performance of ODS materials is dependent on nano-scale oxide being distributed uniformly throughout the metal matrix; a homogenous distribution is critical to the creep and yield strength. Therefore, quantifying and analyzing these oxide nanoparticles is essential for ODS alloy development. Assessing the chemistry and morphology of dispersoids in a material can be conducted using a variety of X-ray and electron-based methods. Time of Flight Secondary Ion Mass Spectrometry (TOF-SIMS), which assesses chemical concentrations from ion masses, provides the necessary spatial resolution and avoids potential spectral overlap of all elements present. In this work, preparing ODS powder feedstock and Laser Powder Bed Fusion AM was conducted with a NiCoCr alloy and yttria dispersoid, mixed with a Resodyn resonance mixer and printed on an EOS M100 3D printer at NASA Glenn. TOF-SIMS was performed on a Physical Electronics NanoTOF TRIFT V TOF-SIMS at Case Western Reserve University. The TOF-SIMS results collected on the feedstock powder samples correspond to the qualitative interpretation of the homogeneity of the oxide coating on the metal powder from SEM images. This provides quantitative support to the qualitative microscopy images collected earlier in the process design phase. The variance in the yttrium distribution on the powder feedstock samples also correlated with the variance of the yttrium distribution detected in the printed samples. This correlation supported the hypothesis that an even coating of yttria on the metal powders contributes to an even distribution of yttria in the printed material.

Laura G. Wilson↗