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Metal Additive Manufacturing for Rocket Engines: Successes and Failures

NASA has been developing additive manufacturing (AM) for various technical and programmatic advantages for complex rocket engine and aerospace components. This maturation has focused on various AM processes, new alloys, characterizing material properties, developing standards, producing demonstrator parts, and integrating AM hardware in liquid rocket engines through test-fail-fix cycles, as well as application and dissemination of lessons learned of the AM lifecycle. The importance of proper AM processing was made evident in the failure of a Laser Powder Bed Fusion (L-PBF) copper-alloy combustion chamber during a hot-fire test due to a degraded material quality. The hot-fire test aimed to demonstrate high duty cycle under a risk-tolerant development project, where consequences of component failure would be minimal. However, the unintentional component failure emphasized the necessity of robust material characterization and rigorous process control procedures for the safe use of AM components in critical applications. This presentation provides an overview of the development failure, a discussion on the evaluation of the failed chamber and supplemental chambers produced at the same time, a representative material samples that included intentional build witness lines, and a summary of the key results and recommendations from the evaluations. NASA continues to approach AM processes and designs with a level of risk and acceptance of failures that is appropriate for the project objectives, with the overall goal of safe implementation of AM technology and transferring AM technology into commercial space applications. This presentation with provide critical awareness to the community lessons learned on proper implementation of AM.

L-PBF↗

Quantifying Trapped Powder in Electron Beam Powder Bed Fusion

Abstract Electron beam powder bed fusion (PBF-EB) shows great potential for manufacturing complex parts including those with internal cavities for heat exchanger, manifold systems, or energy absorption purposes. PBF-EB allows for the manufacture of channel geometries without the need for support structures. Due to the nature of the powder spreading process, powder feedstock is often trapped in intentionally manufactured cavities. This trapped powder can often be difficult to remove and can disturb the intended flow of fluid through the cavity or damage downstream components in its use case. These trapped powder particles present a risk of contamination and component failure if not completely evacuated. Ti6Al4V is a choice material for aerospace applications due to its high strength to weight ratio and its composition as a nonferrous metal; however, in weight sensitive applications excess entrapped powders or powders loosely attached to the surface could cause undesirable weight increases. The inherent spreading process of PBF-EB is different than laser powder bed fusion (PBF-LB) in its operational temperature, sintering. In addition, PBF-EB is less commonly studied in literature compared to its PBF-LB counterpart, and as a result the complexity of the semi-sintered powder and its spreading behavior are not well understood. Prior work has investigated the difficulty in removing trapped powder from PBF-EB, but these studies do not address how to quantify the amount of trapped powder in the cavity. Thus, an accurate method to measure the amount of trapped powder in the cavity must be investigated. In this work, Ti6Al4V coupons were manufactured with horizontal and vertical cavities of three different sizes. Archimedes testing allows for the determination of density differences caused by porosity and trapped powders by measuring mass and volumetric dispersion. Computed tomography (CT) is well suited for segmenting the internal structure and features of a part and has been studied for applications including voids, porosity, and dross. Thus, CT was explored as a method for evaluating trapped powder content in this work. The volumetric representation of the segmentation of the reconstructed CT volume can vary greatly depending on the input filter and thresholding methods. In this study, four different types of segmentation approaches were evaluated to determine the best approach for segmenting the volume as compared to an operator labeled ground truth. The percentage density results from the Archimedes testing were compared to the volumetric percent density from the computed tomography approach. Differences in packing density between two different internal channel features were investigated. Overall, this work sought to validate the use of computed tomography for the detection of trapped powders and present a framework for volumetric segmentation.

Johnstone, Brian↗

Printing Outside the Box: Additive Manufacturing Processes for Fabrication of Large Aerospace Structures

To achieve NASA's mission of space exploration, innovative manufacturing processes are being applied to the fabrication of propulsion elements. Liquid rocket engines (LREs) are comprised of a thrust chamber and nozzle extension as illustrated in figure 1 for the J2X upper stage engine. Development of the J2X engine, designed for the Ares I launch vehicle, is currently being incorporated on the Space Launch System. A nozzle extension is attached to the combustion chamber to obtain the expansion ratio needed to increase specific impulse. If the nozzle extension could be printed as one piece using free-form additive manufacturing (AM) processes, rather than the current method of forming welded parts, a considerable time savings could be realized. Not only would this provide a more homogenous microstructure than a welded structure, but could also greatly shorten the overall fabrication time. The main objective of this study is to fabricate test specimens using a pulsed arc source and solid wire as shown in figure 2. The mechanical properties of these specimens will be compared with those fabricated using the powder bed, selective laser melting technology at NASA Marshall Space Flight Center. As printed components become larger, maintaining a constant temperature during the build process becomes critical. This predictive capability will require modeling of the moving heat source as illustrated in figure 3. Predictive understanding of the heat profile will allow a constant temperature to be maintained as a function of height from substrate while printing complex shapes. In addition, to avoid slumping, this will also allow better control of the microstructural development and hence the properties. Figure 4 shows a preliminary comparison of the mechanical properties obtained.

Babai, Majid↗

Strength stability at high temperatures for additively manufactured alumina forming austenitic alloy

Several fast-spectrum nuclear reactors designed to generate high power (~450 MWe) rely on forced convection of media such as supercritical CO 2 , sodium, or liquid lead to cool the nuclear core, operating at temperatures up to 600 °C. Cost-effective, high-strength Fe-based alumina forming austenitic (AFA) alloys are a promising candidate for the fabrication of critical nuclear components. This study investigated laser powder bed fusion (LPBF) processing of an AFA alloy composition optimized for improved creep resistance. Electron microscopy revealed an elongated grain structure along the build direction with a fine sub-grain cellular structure decorated with (Cr,Fe,Nb) 23 C 6 carbide precipitates at the intercellular boundaries. Finally, at temperatures of 20–900 °C, the LPBF alloy's superior tensile properties compared to its arc-melted counterpart and other advanced steels (e.g., SS316) were attributed to the distribution of nano-sized carbide precipitates, whereas the high ductility was attributed to the LPBF alloy's elongated grain structure.

36 MATERIALS SCIENCE↗

Evaluation of DED and LPBF Fe-based Alloys Process Application Envelopes based on Performance, Process Economics, Supply Chain Risks, and Reactor-specific Targeted Components

The U.S. Department of Energy (DOE), Office of Nuclear Energy (NE), Advanced Materials and Manufacturing Technologies (AMMT) program aims to develop extreme-environment materials solutions for use in the deployment of advanced nuclear reactors and the sustainment of the current fleet. To achieve this objective, a combination of experiment, a computational tool, and machine learning (ML) for the design of materials is adopted for the maturation of materials for nuclear technology. Through advanced manufacturing techniques such as laser powder bed fusion (LPBF) and laser powder direct energy deposition (LP-DED), components with complex geometries can be fabricated with reduced time and effort. Such advanced manufacturing methods can also provide the opportunity to improve materials performance through optimized microstructures and mechanical properties. However, existing engineering alloys are not always well suited for fabrication with additive manufacturing (AM), as their compositions have been tuned to optimize fabrication via conventional methods. Thus, similar alloys with modified compositions that are better suited for AM can be studied for improved performance. Over the past three years, the AMMT teams from Argonne National Laboratory (ANL) and Pacific Northwest National Laboratory (PNNL) studied various known Fe-based alloys by evaluating their initial printability using LPBF, and an AMMT-developed down-selection and decision matrix reduced the number of alloys to be studied from six to three in fiscal year (FY) 2024. Additionally, in FY 2024, for parallel evaluation, these three alloys were studied using LPDED. While LPBF is better for small- to medium-sized components with high detail and internal features, LP-DED combines a material feed system to place the powder onto the exact spot where the laser will melt the material. This AM method can be easily scaled to extremely large components and provides high build rate speeds compared to those of conventional LPBF systems. Additionally, DED is a better choice for complex geometries and compositional gradients.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Additive manufacturing of AISI M2 tool steel by binder jetting (BJ): Investigation of microstructural and mechanical properties

The presented research demonstrates for the first time the successful processing of AISI M2 tool steel by binder jetting, a promising additive manufacturing technique capable of producing complex shapes with minimal residual stresses and isotropic properties. The optimal printing parameters were explored by varying processing parameters such as the binder saturation (45 %–105 %), binder set time (0 to 10 s), targeted bed temperature (50–60 °C), oscillator (2600–2750 rpm), recoater (20–28 mm/s), and roller speeds (200–300 rpm). Microstructural characterization and evaluation of mechanical properties of binder jetted parts were performed using x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS) to study their chemical composition, powder morphology, microstructure, carbide morphologies, relative density, hardness, compressive strength, and ductility. Two powder sizes (5 and 10 μm) were used, and sintering was performed at varying temperatures (1270, 1280, and 1300 °C) and durations (60 and 120 min), followed by a furnace, air, and water cooling. An optimum hardness of ~970 HV was obtained when parts were sintered at 1270 °C for 60 min, followed by water quenching. Impressive compressive strength of ~ 3580 MPa was observed in the sample sintered at 1280 °C for 60 min duration, followed by air cooling. Furnace-cooled parts showed the highest density of ~95 %, whereas the relative density of air- and water-cooled parts varied between ~91 to 93.50 %, respectively. The microstructure of sintered samples revealed the formation of M 6 C stable carbide, M 2 C metastable carbide, MC as a secondary carbide, and a-Fe matrix, which contributed to the observed increase in mechanical properties.

36 MATERIALS SCIENCE↗

Design of Novel Hot Gas Component for Gas Turbine Engines Enabled by Materials and Additive Manufacturing Process Development

This CRADA project was the result of a project award under FOA-DOE-0001980. The overarching FOA project team consisted of researchers from Carpenter Technology Corporation (CTC), Solar Turbines Incorporated (Solar), Pennsylvania State University (PSU), University of California-Santa Barbara (UCSB), and Oak Ridge National Laboratory (ORNL). Evaluations were conducted on two high-γ’ superalloys that were designed by CTC and the UCSB. One alloy named GammaPrint-700 (GP-700) is a cobalt-base superalloy. The other alloy named GammaPrint-1100 (GP-1100) is a nickel-base (Ni-base) superalloy. PSU provided expertise and experimental testing of the thermal performance of AM micro-cooling architectures. ORNL provided expertise with the AM superalloy materials characterization and AM processing science. Solar provided turbine component design expertise. The focus of this CRADA report is to document the efforts between ORNL and CTC towards the development of superalloys designed for AM. The project goal was to use an AM processable high-temperature superalloy and design for Additive Manufacturing (DfAM) techniques to design an efficient turbine component (i.e. a turbine tip shoe) with enhanced cooling features that can only be fabricated through additive manufacturing (AM). The efficiencies of existing combined heat and power (CHP) engines are capped by both component design and materials limitations. However, AM of a tip shoe component from a γ’strengthened superalloy offers the design flexibility to increase the efficiency and power of an industrial gas turbine. This project brought about advancements in the DfAM tip shoe design space and in the area of high temperature superalloys processable through laser powder bed fusion (LPBF) AM. State of art computation design tools were utilized to optimize unique cooling features into a tip shoe component design. A two-prong materials development approach was taken to support development of the AM tip shoe geometry. The first approach centered on investigating the processability and the appropriate process science for the industry standard high-γ’ nickel-base (Ni-base) superalloy Mar-M247. This superalloy is typically cast and considered non-weldable by traditional welding standards. In the course of this work, the alloy was not deemed feasible for process scale-up due to significant cracking issues during printing. The second approach focused on the development and evaluation of a novel cobalt-base superalloy, GammaPrint™-700 (GP-700 and a Ni-base superalloy, GammaPrint™-1100 (GP-1100) designed to mitigate the significant AM processing issues with Mar-M247. The processability of these two alloys were investigated through electron beam melting (EBM) binder-jet AM (BJAM), and LPBF as a risk mitigation for manufacturability. To be considered a candidate material for down-selection to proceed to full-scale AM tip shoe engine testing trials, the high temperature creep rupture strength was required to achieve at a minimum, a Larsen Miller Parameter (LMP) increase of 10.9% over the baseline material LPBF AM Hastelloy X.

99 GENERAL AND MISCELLANEOUS↗

Optimization of overhang printing in ceramic binder jetting additive manufacturing

Cylindrical-shaped horizontally-hanging overhangs with different heights on a solid cubic body were printed via binder jetting additive manufacturing with sililcon carbide powder feedstock. Cracking on the overhang neck and sagging on the overhang body were observed both pre- and post-curing, especially on printed design with a smaller particle size of 10 μm. Here, it was found that the width of cracking and depth of sagging were dependent on the height relative to the solid body in the powder bed, and elevated position of overhang with large volume of underneath loose powder led to increased extend of cracking and sagging. Overhang diameter and weight were varied, which were found with no apparent effects on its deformation extend. To mitigate cracking and sagging, contactless support was designed and tested, which could significantly improve the overhang stability and avoid any overhang deformations. Support gap and support distance were studied for their effects on support capability. The printing processes with and without contactless support were simulated by a finite element modeling approach to understand the stress distribution and evolution of the overhang structures, which revealed stress concentrations on the upper neck point of the designed overhang.

Binder jetting↗

Having a Come-Apart: Lessons Learned from Additively Manufactured Hardware Failures

NASA has been engaged with additively manufactured (AM) process and component development since the 2000’s. AM offers various technical advantages, such as enhanced hardware design complexity, part consolidation, and processing of novel alloys in addition to programmatic advantages for reduction in processing time and cost. The focus of much of the AM development at NASA has been to mature the various processes, characterize material properties, develop standards, produce demonstrator parts, and integrate AM hardware in liquid rocket engines. These aspects have been demonstrated through process and design iterations using a methodical characterization, test-fail-fix cycles, as well as application and dissemination of lessons learned. In addition to these fundamental demonstrations of the AM process and hardware development, alloys that provide performance advantages in the high temperature and high-pressure environments have been matured for use in rocket engines. These environments are challenging for any alloy and any design, and the AM process is required to fully meet the intended design requirements. The importance of proper AM process was made evident in the failure of a Laser Powder Bed Fusion (L-PBF) copper-alloy combustion chamber during a hot-fire test due to a degraded material quality resulted from an AM process issue. The hot-fire test aimed to demonstrate high duty cycle under a risk-tolerant development project, where consequences of component failure would be minimal. However, the unintentional component failure emphasized the necessity of robust material characterization and rigorous process control procedures for the safe use of AM components in critical applications. In part, such concerns motivate the AM certification approach that NASA has recently adopted in NASA-STD-6030 “Additive Manufacturing Requirements for Spaceflight Systems”. This presentation provides an overview of the previously mentioned failure, a discussion on the evaluation of the failed chamber and supplemental chambers produced at the same time, a representative material samples that included intentional build witness lines, and a summary of the key results and recommendations from the evaluations. NASA continues to approach AM processes and designs with a level of risk and acceptance of failures that is appropriate for the project objectives, with the overall goal of safe implementation of AM technology and transferring AM technology into commercial space applications. The objective of this presentation is to provide awareness to the community working critical and non-critical AM components and the lessons learned on proper implementation of AM.

Additive Manufacturing↗

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↗

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↗

Robust Solar Receivers Using MAX Phase Materials

This work was supported by the U.S. Department of Energy’s Office of Energy Efficiency and Renewable Energy under the Solar Energy Technologies Office Award Number 35928. The objective of the proposed effort was to develop and optimize additive manufacturing technologies for low-cost fabrication of high-temperature receivers using MAX phase-based materials (Ti 3 SiC 2 and Ti 3 AlC 2 ). MAX phase materials are a group of ternary metal carbides and nitrides where M stands for an early transition metal element, A is a group 13–16 element, and X is C and/or N. In Phase 1, the binder jetting additive manufacturing process was used to synthesize and characterize the Ti 3 SiC 2 MAX phase material. The typical process involved first producing a TiC preform using binder jetting followed by infiltration of the preform with silicon melt to form Ti 3 SiC 2 in situ. The reaction-infiltrated samples showed formation of MAX phase in the sample core; however, the surface showed cracking. Various process conditions—cooling rates, hold times, Si proportion, etc.—were varied to minimize the surface cracking. The fabricated MAX phase core was characterized by microstructure analysis and evaluations of mechanical properties such as hardness and thermal shock. In Phase 2, the focus included fabrication of Ti 3 SiC 2 MAX phase materials by spark plasma sintering (SPS) and synthesis of Ti 3 AlC 2 MAX phase materials by the Al melt infiltration process. It is expected that Al infiltration will not cause sample cracking, since Al does not expand during solidification. In addition, other processing approaches were investigated to fabricate the MAX phase materials, such as SPS with a graphite bedding approach for producing short-length Ti 3 AlC 2 MAX phase tubes for demonstration of prototypical Concentrating Solar Power receiver tubes. Fabricated samples underwent thermo-mechanical testing to validate the materials for the solar receiver application at temperatures >1000°C. In Phase 3, the effort focused on the development and optimization of the Ti-Al-C MAX phase composite material using the Al melt infiltration approach. We started with optimization of precursor powders and making preform structures by either pressing them in a die or using the binder jetting additive manufacturing process followed by Al melt infiltration. In addition, we investigated the formation of preform structures by cold isostatic pressing followed by Al melt infiltration for making Ti-Al-C MAX phase composite. Thermo-mechanical characterizations, such as creep, strength, and thermal shock, were conducted to establish the structures’ performance.

36 MATERIALS SCIENCE↗

Establishing model credibility for process-microstructure-property relationships in additive manufacturing using exascale computing

Additive Manufacturing (AM) of alloys holds significant promise as a disruptive technology in various industries, yet its adoption is often hindered by challenges in achieving consistent part quality. These issues are primarily due to the complex process-microstructure-property (PSP) relationships inherent to AM. Computational models can greatly aid in understanding these relationships, but their widespread impact and adoption has been limited by a lack of validated, open-source, and computationally efficient PSP modeling frameworks and hardware limitations. Here, this study leverages the ExaAM software suite and data from the AMBench-2018 series of laser powder bed fusion (LPBF) benchmark experiments to perform a comprehensive model assessment, including verification, validation, sensitivity analysis, and uncertainty quantification. The RADICAL-EnTK workflow manager was used to perform an ensemble of heat transport, solidification, and mechanical response simulations on the exascale computer Frontier, considering uncertainties in critical model inputs such as laser spot size and nucleation parameters, and consisting of 125 explicit grain structure simulations and 7875 crystal plasticity simulations. For a selected location within the Inconel 625 AMBench-2018 test artifact, sensitivity analysis and uncertainty quantification were performed using the predicted distributions of grain structure and mechanical properties. Qualitative agreement was found between the predicted grain size and texture and the observed AMBench-2018 microstructure, the mean predicted yield stress was within 5% of the experimental measurement mean, and the mean predicted engineering stress at 5% strain was within 10% of the experimental measurement mean. The insights gained from development and validation of the ExaAM PSP modeling framework will help guide future directions for enhancing the credibility and reliability of PSP models in AM, thereby accelerating the adoption of AM technologies in various industries.

Additive manufacturing↗

Advancement of Novel Additively Manufactured Alloys for Space Applications

NASA has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the late 2000’s. Several efforts have focused on the understanding of AM processes through material characterization and testing, standards development, component fabrication, and infusion into development and flight applications. While many common aerospace alloys have been and continue to be a focus of ongoing development, the need for custom-alloy developments for high performance applications enabled by AM processes has been realized. The applications being targeted are liquid rocket engines with high heat fluxes, high pressure, and that utilize propellants such as hydrogen, which can degrade the alloy. NASA has recently focused on the development and advancement of novel alloy advancement using AM for use in these harsh environments, such as GRCop-42, GRCop-84, NASA HR-1, and JBK-75. These alloys have been evaluated using the laser powder bed fusion (L-PBF) and laser powder directed energy deposition (LP-DED) processes. The results from these processes have demonstrated that AM can enable rapid development of new alloy systems that can yield higher performances. These alloys have undergone the fundamental metallurgical evaluations, heat treatment study, and microstructure characterization and mechanical testing campaign. This, combined with direct application-specific component fabrication and hot-fire testing, enabled the increase of the Technology Readiness Level (TRL). This presentation will provide a background and overview of these AM-enabled novel alloys, AM processing development including metallurgical and mechanical property studies. It will also cover the latest advancement in the parallel component development and testing and future developments. The goal of these alloy development is to allow for technology infusion into NASA and commercial spaceflight missions as well as to establish and sustain the needed commercial AM supply chain.

Additive Manufacturing↗

Design of Novel Hot Gas Component for Gas Turbine Engines Enabled by Materials and Additive Manufacturing Process Development

This CRADA project was the result of a project award under FOA-DOE-0001980. The overarching FOA project team consisted of researchers from Carpenter Technology Corporation (CTC), Solar Turbines Incorporated (Solar), Pennsylvania State University (PSU), University of California-Santa Barbara (UCSB), and Oak Ridge National Laboratory (ORNL). Evaluations were conducted on two high-γ’ superalloys that were designed by CTC and the UCSB. One alloy named GammaPrint-700 (GP-700) is a cobalt-base superalloy. The other alloy named GammaPrint-1100 (GP-1100) is a nickel-base (Ni-base) superalloy. PSU provided expertise and experimental testing of the thermal performance of AM micro-cooling architectures. ORNL provided expertise with the AM superalloy materials characterization and AM processing science. Solar provided turbine component design expertise. The focus of this CRADA report is to document the efforts between ORNL and CTC towards the development of superalloys designed for AM. The project goal was to use an AM processable high-temperature superalloy and design for Additive Manufacturing (DfAM) techniques to design an efficient turbine component (i.e. a turbine tip shoe) with enhanced cooling features that can only be fabricated through additive manufacturing (AM). The efficiencies of existing combined heat and power (CHP) engines are capped by both component design and materials limitations. However, AM of a tip shoe component from a γ’strengthened superalloy offers the design flexibility to increase the efficiency and power of an industrial gas turbine. This project brought about advancements in the DfAM tip shoe design space and in the area of high temperature superalloys processable through laser powder bed fusion (LPBF) AM. State of art computation design tools were utilized to optimize unique cooling features into a tip shoe component design. A two-prong materials development approach was taken to support development of the AM tip shoe geometry. The first approach centered on investigating the processability and the appropriate process science for the industry standard high-γ’ nickel-base (Ni-base) superalloy Mar-M247. This superalloy is typically cast and considered non-weldable by traditional welding standards. In the course of this work, the alloy was not deemed feasible for process scale-up due to significant cracking issues during printing. The second approach focused on the development and evaluation of a novel cobalt-base superalloy, GammaPrint™-700 (GP-700 and a Ni-base superalloy, GammaPrint™-1100 (GP-1100) designed to mitigate the significant AM processing issues with Mar-M247. The processability of these two alloys were investigated through electron beam melting (EBM) binder-jet AM (BJAM), and LPBF as a risk mitigation for manufacturability. To be considered a candidate material for down-selection to proceed to fullscale AM tip shoe engine testing trials, the high temperature creep rupture strength was required to achieve at a minimum, a Larsen Miller Parameter (LMP) increase of 10.9% over the baseline material LPBF AM Hastelloy X.

36 MATERIALS SCIENCE↗

Additive Manufacturing of Fe-based Alloys for Nuclear Reactor Environments

This report is a Milestone 2 deliverable in FY2025, under work package MT-25AN090211 to support research and qualification activities supported by the Advanced Materials and Manufacturing Technologies (AMMT) program. It provides an update on the work done on the laser based additive manufacturing of steels for nuclear applications, conducted collaboratively by Argonne National Laboratory and Pacific Northwestern National Laboratory. Building upon FY23 and FY24 efforts, the focus of FY25 includes continued optimization of process parameters for the alloys: A709 & G92. The work package also includes fabricating test samples to conduct a thorough microstructural analysis and perform preliminary mechanical testing. The major accomplishments of this work package are summarized below, applicable to both Laser Powder Bed Fusion (LPBF) processes conducted at Argonne National Laboratory and Laser Powder Directed Energy Deposition (LP-DED) processes conducted at Pacific Northwest National Laboratory.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Quantifying Microstructure Variability in Laser Powder Bed Fusion 316 L Stainless Steel Microstructures with Spatial Statistics

Here, we have explored data-driven methods for material microstructure quantification that improve sensitivity to microstructural changes compared to traditional approaches. The methods integrate multiple microstructural properties, including grain morphology, crystallographic orientation, and material phase information. The simpler method employs maps of the Euclidean distance transformation metric to evaluate the morphology of grain boundary networks. The more intensive approach employs generalized spherical harmonic mapping for crystallographic orientations, per-pixel phase information, and a variational auto-encoder for dimensionality reduction and results in a multidimensional clustering of by microstructure similarity. Applied to an experimental dataset of additively manufactured steel, both methods detected slight variations in samples produced under nominally identical processing conditions. Both methods were able to distinguish between samples from multiple (nominally identical) builds, while the generalized spherical harmonics-based method could additionally cluster data samples rotated at two orientations on the build plate. The improved sensitivity of the methods, demonstrated through comparison with traditional microstructure characterization techniques, offers advantages for microstructure quantification and comparisons in advanced manufacturing applications.

SS316L↗

The Effect of Composition on Microstructure and Properties for Additively Manufactured Superalloy 718

Additive manufacturing (AM) represents an exciting new approach towards producing metallic aerospace components. The ability to make complex geometries that were impossible to create using conventional manufacturing methods has sparked interest from the aerospace community, including NASA. The use of AM components for crucial and human rated space missions necessitates a full characterization of the differences between AM and more conventional wrought and cast processes. For this study, sixteen different commercially available superalloy 718 powder feedstocks were obtained, built using laser powder bed fusion(L-PBF), and microstructurally and mechanically analyzed. These measurements revealed a wide range of build qualities and microstructures despite all powder lots falling within the 718chemical specification and being processed using the same prescribed build and heat treatment parameters. Statistical analysis found a strong correlation of the amount of carbon in the powder with the final grain size and strength of the heat-treated 718 part. Ultimately, this study highlights the need of a refined superalloy 718 chemical specification for powder lots to be used in AM.

Timothy M Smith↗