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Long-term thermal aging behavior and strength reduction in a laser powder bed fusion 316H stainless steel

The long-term thermal stability of structural alloys is essential for ensuring the safe and reliable operation of nuclear reactors and other power plants. While extensive research has explored the effects of thermal aging on conventional stainless steels, the behavior of additively manufactured (AM) alloys remains less understood. This study examines the thermal aging response of laser powder bed fusion (LPBF) 316H stainless steel (SS) at temperatures ranging from 550 °C to 750 °C over durations of up to 10,000 h (approximately 1.14 years). Advanced characterization techniques, including electron microscopy and synchrotron X-ray diffraction, were used to investigate dislocation recovery and phase evolution. Based on these findings, a time-temperature-precipitation (TTP) diagram was developed for LPBF 316H SS, revealing a 10- to100-fold acceleration in precipitation kinetics compared to wrought 316H SS. A physics-informed model was calibrated using the short-term experimental data, enabling predictions of average precipitate sizes, volume fractions of M 23 C 6 and Laves phases, and changes in molybdenum solute concentration for aging up to 1 × 10⁶ h (114 years). These microstructural insights were further utilized to estimate yield strength and extrapolate strength reduction factors over the extended aging period. Despite the accelerated aging kinetics, LPBF 316H SS demonstrated superior yield strength retention compared to its wrought counterpart. In conclusion, this study establishes a framework for evaluating long-term performance using short-term experimental data and supports the accelerated qualification of AM materials for high-temperature structural applications.

Laser powder bed fusion↗

Parameter, Post-Processing Sensitivities, and Qualification Approach of Laser Powder Bed Fusion Hydrogen Resistant Alloy NASA HR-1

Metal additive manufacturing (AM) processes are being used to enable economical manufacturing of legacy alloys as well as advancing new alloys. Laser powder bed fusion (L-PBF) is a metal AM process that has high maturity and being used to produce a variety of parts for space applications including complex propulsion components. The National Aeronautics and Space Administration (NASA) has identified the need to develop and advance new materials in unique space applications such as high-pressure hydrogen environments. NASA HR-1 is a high strength Fe-Ni based superalloy designed to resist high pressure hydrogen environment embrittlement (HEE), oxidation, and corrosion that has been successfully adapted to laser powder directed energy deposition (LP-DED). Insights gained from the NASA HR-1 development for LP-DED have guided the development process for L-PBF. However, adapting NASA HR-1 to L-PBF posed new challenges due to the distinct differences between the additive manufacturing processes. During parameter development, sensitivities were observed in post-processing that necessitated additional optimization of heat treatments. Additionally, the variations in thickness and how it influenced the microstructural response during heat treatment was characterized. Understanding these sensitivities is important to qualification of the material in a L-PBF machine. This ensures that the microstructures and properties of the material maintain consistency in production. This presentation will cover parameter development along with post-processing challenges and solutions will be discussed in addition to key material properties as it pertains to application performance and qualification per NASA-STD-6030. Improvements made by developing a derivative alloy, NASA HR-2, will be highlighted through preliminary small scale parameter development, material characterization, and initial property testing.

NASA HR-1↗

Laser Powder Bed Fusion Manufactured Alloys 625 and 282 and Properties Relevant to Advanced Nuclear Components

Under the Advanced Materials and Manufacturing Technologies program, two Ni-based alloys fabricated by laser powder bed fusion (LPBF) have been evaluated: γ′-strengthened Haynes 282 and solution-strengthened Inconel 625. Large printing defects were observed in the LPBF 282 alloy fabricated using a Renishaw AM250 machine, likely due to particle spattering during printing. Annealing at 1,180°C for 1 h followed by 4 h at 800°C in a high density of 50 nm γ′-strengthening precipitates as well as partial recrystallization resulted in a bimodal grain distribution. Creep testing performed at 750°C revealed lower creep life and ductility for the LPBF 282 compared with wrought 282. X-ray computed tomography combined with optical and scanning electron microscopy microstructural characterization revealed crack formation during creep testing, initiated either from printing defects or from creep cavitation at grain boundaries. Printing defects were the likely reason for the lower creep performance of LPBF 282 and could be suppressed by optimizing the build configuration. Printing 625 on an EOS M290 machine using the recommended EOS parameters resulted in a very low defect density. Superior creep strength at 725°C was observed for the as-printed LPBF 625 along the build direction when compared with wrought 625. No defect larger than ~50 µm could be detected by X-ray computed tomography in the as-printed conditions and after creep testing for 1,000 h at 725°C and 150 MPa. Small, needle-like δ-phase precipitates were observed after creep testing for 100 h at 725°C and 200 MPa. The rapid formation of the γ phase is directly related to the initial Nb and Mo segregation in the LPBF 625 cell walls, and its effect on the alloy’s high-temperature performance will be evaluated. Solution annealing was carried out at 1,150°C for 1 h and led to full recrystallization of the alloy. A decrease in strength and increase in ductility were observed after solution annealing, and the alloy recrystallization resulted in isotropic tensile properties at room temperature, contrary to what was observed for the as-printed LPBF 625.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Multimodal Defect Imaging of Pure Tungsten Components Fabricated via Electron Beam Powder Bed Fusion

The utilization of additive manufacturing (AM) techniques for refractory materials in high-temperature environments has significantly expanded because of the ability to fabricate geometrically complex components. Electron beam powder bed fusion (EB-PBF), which provides lower residual stress, a cleaner vacuum environment, and better efficiency for high melting point, is one of the best-suited AM methods to produce advanced refractory components. However, the property variation attributed to the heterogeneous microstructure and process-induced defects has hindered the widespread adoption of EB-PBF-produced material like tungsten. While numerous in-situ monitoring and defect detection methods have been demonstrated for EB-PBF, a workflow that compares and evaluates process-induced abnormalities from different imaging perspectives is still limited. This study examines a feature-embedded tungsten component manufactured via the EB-PBF process to demonstrate the defect detection capabilities of a multimodal defect imaging workflow. The predefined and process-induced defects are evaluated by harnessing various imaging techniques, including in-situ electron imaging, layerwise near-infrared (NIR) imaging, post-build high-energy x-ray computed tomography (CT), and conventional destructive metallography. The results highlight the strengths and limitations of distinctive defect imaging techniques concerning specific defect types, sizes, and conditions. It was found that electron imaging can provide more abnormal detection capabilities while maintaining a higher measuring accuracy, against the conventional metallography in this case study, compared with NIR and CT imaging techniques.

36 MATERIALS SCIENCE↗

In situ Visible Light and Thermal Imaging Data from a Laser Powder Bed Fusion Additive Manufacturing Process Co-Registered to X-ray Computed Tomography and Fatigue Data

This dataset is comprised of in situ sensing data collected during a laser-based powder bed fusion additive manufacturing process, as well as rasterized scan path information, post-build X-ray computed tomography (XCT), and fatigue test results. A total of 64 cylinders, approximately 15 mm in diameter and 102 mm tall, were printed out of stainless steel 316H on a Colibrium Additive Concept Laser M2 Series 5 machine. Parameters known to produce dense material were used to construct 56 of these cylinders, while the remaining 8 cylinders were printed with relatively high energy density parameters prone to producing keyhole pores. In addition, two spatter generation blocks were constructed upstream of the 64 cylinders such that ejecta produced during the melting of the spatter generators were stochastically seeded onto the 64 cylinders. Based on previous experiments, these spatter particles were theorized to produce stochastic lack-of-fusion pores. During the construction of the build, high-resolution images of reflected light in the visible spectrum were captured both before and after recoating for each print layer. Additionally, temporally integrated thermal imaging in the near infrared spectrum produced integrated sum and max images on a layerwise basis. The multimodal in situ data has been co-registered to the build plate coordinate system, allowing for identification of process anomalies (e.g., spatter particles) apparent in the two sensors. Following construction of the build, the cylinders were subjected to XCT to identify internal flaws, and the resulting data have also been registered to the build plate coordinate system. Finally, 60 of the 64 cylinders were machined into fatigue coupons conforming to ASTM E466 and subsequently subjected to either high- or -low-cycle fatigue testing. The results of the fatigue tests have also been included in the dataset, and the XCT data corresponded to the approximate location of the gauge sections of the machine fatigue specimen geometry.

42 ENGINEERING↗

A high-throughput approach for statistical process optimization in Laser Powder Bed Fusion

Process variability is inherent in metal additive manufacturing (AM). However, it is often overlooked in process optimization frameworks, constraining the understanding of process uncertainties and their influence on parameter selection. To address this, we present an integrated framework that combines high-throughput single-track experiments, GAN-based melt pool geometry extraction, robust statistical and machine learning modeling, and uncertainty-quantified process mapping. Process variability is characterized through single-track melt pool behaviors, and its influence on defect formation is systematically quantified to enable statistically guided process parameter optimization. This approach is demonstrated on Laser Powder Bed Fusion (L-PBF) of stainless steel 316L, effectively capturing the interplay between process parameters, melt pool variability, and defect probability. By integrating uncertainty quantification into process optimization, this study provides a structured methodology for addressing variability challenges in AM quality control, ultimately contributing to enhanced manufacturing reliability.

Laser Powder Bed Fusion↗

Microstructure and Mechanical Properties of Ni-based Alloys Fabricated by Laser Powder Bed Fusion

The Advanced Materials and Manufacturing Technologies (AMMT) program is aiming at the accelerated incorporation of new materials and manufacturing technologies into nuclear-related systems. Complex Ni-based components fabricated by laser powder bed fusion (LPBF) could enable operating temperatures at T > 700°C in aggressive environments such as molten salts or liquid metals. However, available mechanical properties data relevant to material qualification remains limited, in particular for Ni-based alloys routinely fabricated by LPBF such as IN718 (Ni- 19Cr-18Fe-5Nb-3Mo) and Haynes 282 (Ni-20Cr-10Co-8.5Mo-2.1Ti-1.5Al). Creep testing was conducted on LPBF 718 at 600°C and 650°C and on LPBF 282 at 750°C. finding that the creep strength of the two alloys was close to that of wrought counterparts. with lower ductility at rupture. Heat treatments were tailored to the LPBF-specific microstructure to achieve grain recrystallization and form strengthening γ' precipitates for LPBF 282 and γ' and γ" precipitates for LPBF 718. In-situ data generated during printing and ex-situ X-ray computed tomography (XCT) scans were used to correlate the creep properties of LPBF 282 to the material flaw distribution. In- situ data revealed that spatter particles are the potential causes for flaws formation in LPBF 282. with significant variation between rods based on their location on the build plate. XCT scans revealed the formation of a larger number of creep flaws after testing in the specimens with a higher initial flaw density. which led to a lower ductility for the specimen.

Dryepondt, Sebastien↗

Additive Manufacturing Model-Based Process Metrics: Reduced Order Modeling of the Laser Powder Bed Fusion Process

The multi-scale and complex process of printing additively manufactured (AM) parts can have unexpected, but predictable, build conditions that result in material microstructure variability. In this work, we describe a fully parallel reduced order modeling approach that has been developed to evaluate the evolution of AM processes, termed the AM moment measure method. This method couples the known sequence of the AM process with a physically informed nearest neighbors’ calculation to map the conditions of a part-scale build. The result is a map of the build that is derived directly from build files or in-situ process monitoring sensors. The methodology and terminology of the approach will be described, and computed build maps will be calculated and compared for various laser powder bed fusion (LPBF) builds of Ti-6Al-4V. Such comparative results develop understanding of how the sequential process actions can affect the LPBF-AM build quality and microstructure variability.

Laser Powder Bed Fusion↗

Compositional Homogeneity in Rapidly Solidified 316L stainless steel produced by laser powder-bed fusion processing

The segregation of alloying elements in rapidly solidified 316L stainless steel produced using additive manufacturing technologies is widely reported throughout literature. The microstructure of thin walls manufactured from 316L stainless steel using laser powder bed fusion are examined for the presence of alloy segregation, i.e. the rejection of solutes to grain boundaries. Metallographic methods including mechanical polishing and chemical etching are used to prepare samples for microanalysis m

Jankowski, Alan F. [Sandia National Laboratories (↗

Suppressing Ordering in Equiatomic Fe-Co via Laser Powder Bed Fusion

Neutron and electron diffraction was employed to evaluate the effectiveness of thermal management strategies in suppressing the formation of the equilibrium-ordered B2 (CsCl) phase in equiatomic binary Fe-Co specimens fabricated by laser powder bed fusion additive manufacturing. Specimens with a tensile dogbone geometry were fabricated using various combinations of process parameters (laser power and raster speed) and thermal management strategies (no support struts, struts only in the top gauge section, and struts throughout the gauge section). Diffraction results demonstrate that the rapid solidification during PBF-L effectively minimized B2 formation, with laser power and effective scan velocity having no significant impact on the degree of ordering. Furthermore, the inclusion of support struts in the top grip region had no perceivable impact on ordering, whereas specimens with support struts in the gauge region exhibited no detectable ordering. Results are discussed in the context of thermal finite element analysis predictions.

Laser Material Processing↗

The Additive Manufacturing Moment Measure - A Parallel Computation Technique for Determining Build Variance in the Laser Powder Bed Fusion Process

Additive manufacturing (AM) has unique process attributes that facilitate the creation of optimized, complex, and unique parts for aerospace applications. However, the multi-scale and complicated building process for AM parts can cause unexpected build conditions that result in microstructural variability within the deposited material. The need for richer datasets and computational modeling capabilities to improve AM process reliability is a consequence of this microstructural variability. A computational approach, referred to as the Additive Manufacturing Moment Measure (AM3), addresses this need by leveraging the way AM processes fuse material in precise, incremental steps. During the layering sequence, each previous step contributes to the condition of the current step at the center of the heat source. The precise steps can be selected to systematically create a time-space point field with co-located machine input and in-situ sensor data. The sequential nature of the AM process, coupled with nearest neighbor calculations, allows for a fully parallel computation for part-scale build profile analysis. The AM3 concept introduced here enables part-scale assessment directly from build files and in-situ process monitoring sensors alike. The AM moment measures were calculated for build point fields and compared with co-located in-situ and ex-situ nondestructive evaluation and optical microscopy observations. These comparisons permit a better understanding of how the sequential process actions can affect the quality of a laser powder bed fusion (LPBF) build. Details of the AM3technique will be discussed and compared to measured LPBF part characteristics. The AM3 results indicate a strong potential to advance the qualification process for aerospace applications.

Additive Manufacturing↗

Ink-based laser powder bed fusion of barium titanate

Barium titanate (BTO) is a lead-free functional ceramic that is widely used in sensors, transducers, and actuators. The increasing demand for complex geometries and quick design iterations motivates the use of additive manufacturing techniques. Laser powder bed fusion (L-PBF) additive manufacturing technique enables the net-shape or near-net-shape fabrication of metals and alloys. Ceramic L-PBF remains challenging due to their high melting temperature. Here, to address this challenge, a nanoparticle ink feedstock was incorporated into the L-PBF process to allow low power melting of BTO. Key print parameters (i.e. laser power, scanning speed, and hatching spacing) were optimized to fabricate millimeter-scale BTO parts. The printed BTO samples possessed an inhomogeneous equiaxed-columnar-cellular microstructure. Semiconducting current-voltage behavior was observed in as-printed samples, which was attributed to the creation of oxygen vacancies. The piezoelectric d 33 coefficient was measured to be 4.6 pC/N.

Dielectrics↗

Effect of Heat Treatment on Microstructure and Mechanical Property of 316L Stainless Steel Produced by Laser Powder Bed Fusion

The advanced non-light water reactor designs (Gen IV reactors), including molten salt/ very high temperature/ sodium-cooled and lead-cooled fast reactors, typically operate at higher temperatures and more extreme radiation conditions than light water reactors. An intrinsic part of the deployment and progress of Gen IV reactor designs is selecting the most suitable structural material for a specific application. Additive manufacturing (AM), a fairly new process of making physical, three-dimensional objects from a computer design file, is going to completely change the way of design, build and certify nuclear systems. It offers a range of opportunities to produce complex geometries from existing materials, offers new routes for processing of previously difficult to process materials, allows for design of new high-performance materials, and finally facilitates hybridization of dissimilar materials. This emerging technology has successfully produced cars, wind turbine blade molds and even live cells. It could also open up big opportunities for the nuclear industry to quickly deploy technologies at a fraction of the cost. So far, AM techniques have been preliminarily applied in the field of nuclear reactors, including the classical parts such as the pressure vessel of a small reactor with 508-III steel, the bottom nozzle of a fuel assembly with 304L steel, the fuel cladding with zirconium alloy and the integrated impeller of a pump and the multi-channel valve body with 316L steel [6,7]. The AM applications for operating nuclear reactors started in auxiliary plant components and have slowly migrated to metallic reactors and core components, but many of these are not safety critical components. Although many parts used for nuclear reactors have been fabricated by AM techniques, practical applications in engineering are still a long way off due to the uncertainty factors focused on the processing, material properties, analysis methods and application standards, which feeds the safety and life-cycle of the nuclear reactor. Due to rapid, repeated heating and cooling during production, a high dislocation density was present in the AM material. This microstructure feature is unstable at elevated temperature while high temperature is one of the typical operation environments for nuclear reactors. Thus, it is important to understand the thermal effect on the microstructure of AM material. The objectives of this study are to investigate the effect of heat treatment on the microstructure and mechanical properties of 316L stainless steel produced by laser powder bed fusion additive manufacturing, and to determine an appropriate heat treatment practice that will be applied to the lightweight AM lattice-structured material with the same chemistry. The heat treatment study consisted of annealing the samples at a temperature range of 800 to 1200 oC with a 50 oC increment for different times (1-24 hours), followed by vacuum or air cooling. Microstructural characterization was carried out by Scanning Electron Microscope (SEM). Grain size and crystallographic orientation were investigated by Electron Backscatter Diffraction (EBSD). Vickers hardness tests with a 0.5 kg load were employed to determine the hardness of samples after different heat treatments. After heat treatment, the random crystallographic orientation was preserved, and the volume fraction of high-angle grain boundaries (grain boundary misorientation =15 oC) remained the same. The dislocation density decreased with annealing temperature due to recovery. The fine subgrain structures in the as-printed specimen were quite stable up to 1200 oC. Minimal recrystallization was observed up to 1200 oC. Recrystallization initiated only after 8.5 hours at 1200 oC. The SEM images did not show obvious dependence of microstructure on cooling rate. The hardness of the specimens decreased with increasing annealing temperature as a result of the decrease in dislocation density. It is interesting to note that the AM material showed very similar hardness to the wrought material when annealing at similar temperature, although the microstructures are very different. Annealing at 1050 oC for 1 hour followed by air cooling was selected as the heat treatment procedure for the lattice designed lightweight AM 316L material.

36 MATERIALS SCIENCE↗

Powder Bed Fusion Additive Manufacturing of JBK-75

JBK-75 is an iron-nickel derivative alloy of A-286 that has been of interest to NASA’s propulsion community for use in fuel injectors and other components that are used in hot, corrosive environments. To enable the rapid production of these components in JBK-75, Marshall Space Flight Center has developed parameters for manufacturing fully dense JBK-75 components using powder bed fusion additive manufacturing (PBFAM). These parameters were developed in a two-step development. First, the depth of laser penetration in the powdered material was measured across a spectrum of laser powers to determine the optimal power necessary for generating the desired meltpool depth. The parameter set’s vector-to-vector spacing was then then tailored to guarantee the full densification of the desired area. The results of this development was a readily implementable parameter that produced 99.6% dense material when using a 147W power running at 600mm/s with a 85μm(32%) vector-to-vector spacing.

Jones, Z. C.↗

Evaluation of Directed Energy Deposition and Laser Powder Bed Fusion Nickel-Based Alloys Process Application Envelopes Based on Performance, Process Economics, Supply Chain Risks, and Reactor-Specific Targeted Components

The goal of the Advanced Materials and Manufacturing Technologies (AMMT) program is to accelerate the deployment of new materials and manufacturing technologies into advanced nuclear-related systems. Although 316H stainless steel fabricated by laser powder bed fusion (LPBF) has already been identified as an alloy that could have a significant effect on various reactor technologies, many other materials and manufacturing techniques are being evaluated. Nickel-based alloys typically offer higher-temperature capabilities compared with advanced stainless steels, and previous reports looked at three Ni-based alloy categories: low-Co alloys with a potential use close to the reactor core; high-temperature, high-strength alloys; and molten salt–compatible alloys. Due to the increasing interest in the low Co 625 alloy for nuclear applications, the alloy was compared at the Oak Ridge National Laboratory (ORNL) with 617, 230, two high-temperature, high-strength solution-strengthened alloys. Hot cracking could not be suppressed for alloy 230, and it was shown that these cracks, which were elongated along the build direction (BD), had a drastic effect on the ductility of alloy 230 at room temperature when specimens were machined perpendicular to the BD. Cracking was not as significant for alloy 617, but still led to significant variation in ductility at room temperature along the build direction. On the contrary, LPBF printing of crack-free alloy 625 was achieved using similar printing parameters, and the alloy looks like a very promising candidate for various reactor technologies.

36 MATERIALS SCIENCE↗

Assessment of Segmentation-Induced Deviations of Porosity Metrics in Powder Bed Fusion Additively Manufactured Components

Post processing X-ray computational tomography (CT) inspection data for additively manufactured (AM) components can induce deviations in defect quantification, affecting subsequent fatigue and failure predictions. To assess the influence and potential impact of segmentation-induced measurement deviations, this paper applies several segmentation techniques to X-ray CT data for powder bed fusion Ti-6Al-4V specimens exhibiting porosity conditions. X-ray CT reconstructions were segmented with varying techniques including Otsu’s thresholding, random forest, k-nearest neighbors, and the multilayer perceptron. Metrics such as pore size and global porosity were compared for internal validity. Then, top-down X-ray CT measurements of surface-breaking porosity were compared to optical profilometry for cross-validation.

Data fusion↗

Development of Laser Powder Bed Fusion NASA HR-2 for Hydrogen Sensitive Liquid Rocket Engine Applications

The National Aeronautics and Space Administration (NASA) has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the late 2000s. AM has provided new design and manufacturing opportunities to reduce cost and schedule, consolidate parts, and optimize performance. Laser Powder Bed Fusion (L-PBF) is one of the most commonly used AM processes to fabricate components of complex shape requiring fine feature resolution. Due to exposure to high-pressure gaseous hydrogen, mechanical property degradation caused by hydrogen environment embrittlement (HEE) is a critical concern for many materials in liquid hydrogen propulsion systems. NASA has identified the need to develop and advance new materials in unique engine applications using liquid hydrogen as a propellant. One such material being developed at NASA Marshall Space Flight Center is L-PBF NASA HR-2 (Hydrogen Resistant-2), a high-strength Fe-Ni-based superalloy resistant to HEE. The chemistry of NASA HR-2 was formulated to meet requirements for key liquid rocket engine (LRE) components that operate in high-pressure hydrogen environments. Initial development and material characterization found that NASA HR-2 has excellent L-PBF printability, and its microstructure evolves well after heat treatment. This new alloy has undergone fundamental metallurgical evaluations, heat treatment studies, detailed microstructure characterization, and mechanical testing across a range of temperatures. Tensile testing was performed in a pressurized gaseous hydrogen (GH2) environment to assess its resistance to HEE. L-PBF NASA HR-2 has an average yield stress of 95 ksi, an ultimate tensile stress of 165 ksi, and a very high fracture elongation of 34 - 36% when tested in a high-pressure (5 ksi) hydrogen environment. The tensile property data confirms hydrogen has little influence on HR-2’s ductility, strength, and fracture behavior. L-PBF NASA HR-2 is a promising option for many hydrogen-sensitive LRE components that require exceptional resistance to HEE. This paper will provide an overview of the L-PBF process development, material characterization, mechanical and thermophysical properties, and LRE hardware development for NASA HR-2.

Po S Chen↗