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An Initial Evaluation of the Elevated-Temperature Cyclic Properties of Optimized 316H Stainless Steel Fabricated by Powder Metallurgy Hot Isostatic Pressing

Powder metallurgy hot isostatic pressing (PM-HIP) is a mature advanced manufacturing technology, which can consolidate metallic powder under high temperature and pressure to generate near-net shape components. This process can lower production costs and reduce component lead times for nuclear reactor construction and can be readily deployed in the near term for microreactor components because of their smaller size. The purpose of this work is to continue the evaluation of elevated-temperature cyclic material properties for PM-HIP 316H stainless steel. Prior scoping results have shown that the commercially procured PM-HIP stainless-steel materials have reduced creep-fatigue performance compared to wrought 316 stainless steels. To better understand how PM-HIP processed material properties compare to traditional manufacturing methods, additional billets of PM-HIP 316H stainless steel were procured and tested. This testing is necessary to understand how elevated-temperature properties are influenced by the PM-HIP process and what data are needed for incorporating PM HIP 316H into the American Society of Mechanical Engineers Boiler Pressure Vessel Code, Section III, Division 5 for high temperature reactor construction. Specifically, an additional PM-HIP 316H stainless steel billet with lower oxygen and nitrogen concentrations was fabricated by the Nuclear Advanced Manufacturing Research Centre of the United Kingdom and tested to understand if elevated-temperature cyclic properties can be improved. The creep-fatigue resistance of the material from this new billet did not show appreciable improvement compared to prior testing.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Effect of heat treatment on creep behavior of 316 L stainless steel manufactured by laser powder bed fusion

The objective of this study is to understand the thermal stability of microstructure and its effect on the creep behavior of additively-manufactured 316L stainless steel (AM 316L SS). Creep specimens were fabricated from rods printed by a laser powder bed fusion process. Six different heat treatments, namely 650 °C/1 h, 700 °C/1 h, 750 °C/1 h, 800 °C/1 h, 900 °C/1 h and 1050 °C/1 h were applied to the creep specimens. The heat-treated specimens were creep-tested under the same condition, 550 °C/275 MPa to evaluate the effect of post-build heat treatment on the creep behavior of AM 316L SS. In the temperature range of 650-750 °C, dislocation density within cells, and cell size and wall thickness were affected by the heat treatment, while elemental segregation at boundaries remained unchanged and Mn-enriched Si oxide particles remained stable. In the temperature range of 750-900 °C, concurrent changes were observed in dislocation cell structures, elemental segregation and oxide particles. The 1050 °C-heat treatment removed cell structures and boundary solute segregations, leading to formation of equiaxed grains; Mn-enriched Si oxide particles in the as-built specimen were replaced by more stable Mn-enriched Cr oxides. The creep life of AM 316L SS increased after the heat treatment at 650 °C and then decreased with increasing temperature up to 900 °C where cell/subgrain structures still existed. The creep rate and creep elongation followed an opposite trend. The creep rate can be correlated with the structural parameters of cell/subgrain size and cell wall/boundary thickness and can be rationalized by different strengthening mechanisms of dislocation cells and subgrains. The heat treatment affected strongly the primary and secondary creep but had a minimal effect on the tertiary creep of AM 316L SS.

316L stainless steel↗

Report Outlining Computed Tomography Strategy and Microscopy Approach to Qualifying AM 316 Materials

This report is part of work package CR-22OR0406012, Automated, High-Throughput Materials Characterization Techniques , under the Advanced Materials and Manufacturing Technologies program (AMMT). The project’s primary objective is to leverage our AI-based rapid and high-throughput automated characterization framework to qualify additively manufactured 316 materials comprehensively, focusing on optimizing the additive manufacturing process and evaluating the performance of 3D-printed stainless steel components. This report outlines our strategy for leveraging the automated characterization process for qualifying 316H materials.

36 MATERIALS SCIENCE↗

Development of a 120-mm Aperture Nb 3 Sn Dipole Coil With Stress Management

This paper describes a 120-mm aperture 2-layer dipole coil with stress management (SM) developed at Fermilab based on cos-theta coil geometry. A model of the coil support structure made of plastic was printed using additive manufacturing technology and used for practice coil winding. The real coil support structure was printed using the 316 stainless steel. The results of the SM structure size control and the key coil fabrication steps are reported in the paper. Finally, the design of coil SM structure and the coil FEA in the dipole mirror test configurations are presented and discussed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Computer vision models and advanced TEM imaging for microstructures of irradiated AM316 stainless steels

Advancements were made in automating microscopy-based material characterization, particularly in studying irradiation effects on additively manufactured (AM) materials using machine learning (ML) and computer vision (CV). These automation efforts address the challenges of analyzing complex microstructures, accelerating the detection of irradiation-induced defects. Two CV models were developed at Argonne National Laboratory (ANL) to enhance transmission electron microscopy (TEM) analysis of irradiated AM 316 stainless steel. The first model focused on the detection of irradiation-induced dislocation loops, which contribute to material hardening and embrittlement. These loops, categorized as faulted or perfect, were automatically detected and classified using a Mask R-CNN model trained on TEM images from both in-situ and ex-situ ion irradiation experiments. The model achieved high accuracy, with precision, recall, and F1 scores of 0.839, 0.734, and 0.776, respectively, demonstrating its effectiveness in analyzing dislocation loops in irradiated AM materials. The second CV model was developed to analyze the size and wall thickness of dislocation cells in laser powder bed fusion (LPBF) 316 stainless steel. Using a U-Net++ architecture with EfficientNet as the encoder, the model was trained on TEM images to segment and measure cell size and wall thickness.

36 MATERIALS SCIENCE↗

Crystal plasticity model of residual stress in additive manufacturing using the element elimination and reactivation method

Selective laser melting is receiving increasing interest as an additive manufacturing technique. Residual stresses induced by the large temperature gradients and inhomogeneous cooling process can favour the generation of cracks. In this work, a crystal plasticity finite element model is developed to simulate the formation of residual stresses and to understand the correlation between plastic deformation, grain orientation and residual stresses in the additive manufacturing process. The temperature profile and grain structure from thermal-fluid flow and grain growth simulations are implemented into the crystal plasticity model. An element elimination and reactivation method is proposed to model the melting and solidification and to reinitialize state variables, such as the plastic deformation, in the reactivated elements. The accuracy of this method is judged against previous method based on the stiffness degradation of liquid regions by comparing the plastic deformation as a function of time induced by thermal stresses. The method is used to investigate residual stresses parallel and perpendicular to the laser scan direction, and the correlation with the maximum Schmid factor of the grains along those directions. The magnitude of the residual stress can be predicted as a function of the depth, grain orientation and position with respect to the molten pool. The simulation results are directly comparable to X-ray diffraction experiments and stress–strain curves.

316 stainless steel↗

Preliminary prediction of long-term aging and creep behavior of AM 316 SS

This report describes the development of initial mechanism models for the long term behavior of additively manufactured (AM), laser powder-bed fusion 316H stainless steel under the conditions expected in future advanced nuclear reactors. These models focus on key features of the material microstructure and response that differ from the conventionally-manufactured wrought material. Specifically, the report describes the development of models to capture the unique response of the AM material focusing on irradiation creep and swelling, the effect of internal stress, for example caused by dislocation structure, on precipitation, and the effect of the AM grain and dislocation structure on the macroscale creep and thermal aging behavior. This single mechanism models represent progress towards a complete, physics-based model for the long-term material behavior as well as elucidate key differences in the AM material behavior, when compared to the better-understood, conventionally-manufactured 316H.

36 MATERIALS SCIENCE↗

Preliminary Characterization and Evaluation on FFF Manufactured 316H and ODS Steels

The Advanced Materials and Manufacturing Technology (AMMT) program develops cross-cutting technologies in support of a broad range of nuclear reactor technologies and maintains U.S. leadership in materials and manufacturing technologies for nuclear energy applications. The overarching vision of AMMT is to accelerate the development, qualification, demonstration, and deployment of advanced materials and manufacturing technologies to enable reliable and economical nuclear energy. Solid-state advanced manufacturing techniques can overcome some of the challenges in liquid-based additive manufacturing (AM) processes and should therefore be considered in material design and manufacturing as well. The work presented in this report forms part of a study on solid-state AM techniques of 316 stainless steels (SS) and oxide dispersion strengthened (ODS) steel components and supports the vision and goals of the AMMT program relevant to accelerate the development and deployment of advanced manufacturing processes. Achieving this can provide a safety improvement through larger safety margins, economic benefit for higher efficiency during operation, and a cost reduction through more effective manufacturing processes and less waste. This study provides preliminary information on development of the fused-filament fabrication (FFF) process using different powder types to demonstrate the sensitivity, and therefore the characterization of these sample components. The full solid-state manufacturing feasibility study will be completed and reported in a final feasibility evaluation during 2025. The study investigation used two 14YWT ODS powder batches, which provided information and the effect of different powder morphologies on manufacturability. The two 316SS powders demonstrated the effect of powder size on the manufacturability using FFF. Two product forms, namely a honeycomb structure and flat samples, were manufactured to demonstrate the flexibility of product form.

36 MATERIALS SCIENCE↗

Leveraging the digital thread for physics-based prediction of microstructure heterogeneity in additively manufactured parts

A major limitation of additive manufacturing (AM) processes is that local conditions of material deposition frequently lead to unintentional heterogeneities in microstructure and properties within a single component, despite nominally uniform process conditions. Up to now, there has been no way to a priori determine the distribution of these heterogeneities, requiring expensive trial-and-error approaches to fabrication, testing, and characterization. Here, a physics-based framework for creating a digital representation of the laser powder bed fusion (PBF) process is proposed to predict the variation in solidification behavior that leads to heterogeneous microstructures in an as-built part. By leveraging in situ process data stored in the part’s digital thread, the scan path and process parameters were input into a heat transfer model which predicted solidification data at the melt pool scale. A two-step unsupervised clustering algorithm was used to first cluster the local solidification conditions (12.5µm 3 voxels) and then to cluster the regional behavior on the scale of multiple scan passes and print layers (250µm 3 super-voxels). This process was used to identify regions with similar solidification characteristics for multiple locations in a Stainless Steel 316-L component. The corresponding as-built part was sectioned and characterized using electron backscatter diffraction (EBSD). Quantitative analysis of the pole figures confirmed that the predicted regions of heterogeneity in the solidification conditions corresponded with differences in the observed microstructure. In conclusion, this work shows a viable path for estimating the microstructural heterogeneity for additively manufactured parts to either limit microstructural variation throughout a part or to enable functionality-based variation of the microstructure.

36 MATERIALS SCIENCE↗

Embedding Sensors in 3D Printed Metal Structures

The Transformational Challenge Reactor (TCR) program is leveraging recent advances in modeling and simulation, materials, and additive manufacturing (AM) technologies to design a modern nuclear reactor. Some of the main TCR technologies include in situ monitoring and the integration of sensors during the manufacturing of quality-significant nuclear reactor components. This report describes the general procedure and process optimization for embedding sensors within generic stainless steel 316 (SS316) components using laser powder bed fusion (LPBF). A more detailed, quality-significant test plan and supporting procedures are available upon request (ORNL/TM-2021/2127). LPBF involves the use of a scanning laser to selectively melt regions of a powder bed, additively building a part layer by layer. This report describes the LPBF processing technique and discusses the effects of LPBF processing parameters on the success of the sensor embedding process. Experiments used machined cavities in the form of channels in an SS316 base for the sensors to lay in while material is additively built over the top, thereby embedding them in an SS316 matrix. A preliminary investigation involved using empty SS316 sheaths as surrogates to explore the effects of various LPBF processing parameters and the dimensional requirements of the machined channels. Microstructural investigations showed that a smaller channel width/depth combination closer to the sensor’s diameter was best for the embedding process. After the desired parameters were selected, Type-K thermocouples were embedded and evaluated post-embedding using nondestructive thermal testing, as well as destructive sectioning and microscopy. Post-build characterization showed that the thermocouples were well-bonded to the SS316 matrix and were fully functional after embedding. During thermal testing to temperatures up to 500 °C, the embedded thermocouples read consistently with one another and deviated only slightly from the readings of a nonembedded thermocouple located within the furnace. This slight discrepancy was most likely due to differences in the thermal time constants for a nonembedded thermocouple vs. a thermocouple embedded in a solid SS316 block. The results presented in this report will serve as the foundation for future work that will focus on embedding sensors in relevant TCR reactor components and eventually testing those components under neutron irradiation.

36 MATERIALS SCIENCE↗

Estimation of elastic properties of an additively manufactured lattice using resonant ultrasound spectroscopy

Development of improved approaches in the characterization of additively manufactured structures continues to be a topic of interest for the advanced manufacturing community. This article will investigate an approach using resonant ultrasound spectroscopy (RUS) to determine the effective elastic constants of an orthotropic lattice structure. The evaluation is performed on a cube shaped 316 L stainless steel test specimen, constructed using selective laser melting techniques. The approach uses RUS techniques in conjunction with the assumption that in the frequency regime of interest, the wavelength of the diagnostic ultrasound is greater than the discrete structural features of the unit cell of the lattice; thus, the AM structure can be treated as an anisotropic continuum with effective material properties and symmetry inherited from the unit cell. The RUS analysis estimates the nine elastic coefficients associated with orthotropic sample symmetry, which, in turn, are used to determine the elastic moduli and Poisson ratios. Current results show good agreement between experiments and modeled data. Comparisons to published results are also in good agreement, indicating the potential applicability of this characterization technique for estimating the linear elastic properties of innovative additive manufactured metal lattice structures.

36 MATERIALS SCIENCE↗

Report on Updated Properties Handbook of Printed Stainless Steel 316

This report focuses on summarizing mechanical behavior of 316H stainless steel (SS) printed using laser powder bed fusion (LPBF). 316H SS is one of the six alloys that has been qualified for use in nuclear reactors. The Advanced Materials and Manufacturing Technologies (AMMT) program has identified the use of the additive manufacturing (AM) process of LPBF as one of the manufacturing modalities to fabricate components for nuclear applications. Unlike wrought material, AM material displays significant heterogeneity in properties, resulting from changes in process parameters, machine-to-machine variability, and minor changes in feedstock chemistry from one batch to another. Although significant work has been done on 316L SS in the literature and has been summarized in several review papers, very limited data exist on 316H SS. Therefore, this report aims to provide a concise summary of the properties of 316H SS printed using different machines and at different locations as a part of the AMMT program.

36 MATERIALS SCIENCE↗

Investigating relationship between surface topography and emissivity of metallic additively manufactured parts

Due to the direct relationship between thermal history and mechanical behavior, in situ thermal monitoring is key in gauging quality of parts produced with additive manufacturing (AM). Accurate monitoring of temperatures in an AM process requires knowledge of environment and object parameters including object emissivity. The emissivity is dependent on several variables, including: wavelength, material composition, temperature, and surface topography. Researchers have been concerned with the thermal emissivity dependence on temperature since large ranges are seen in metal powder bed processes, but there is also an extensive range of surfaces produced by AM. This work focused on discovering what roughness characteristics control thermal emissivity through investigation of prototypic 316 stainless steel AM samples produced with a range of build conditions on a laser powder bed fusion machine. Through experimental measurements of emissivity using hemispherical directional reflectance (HDR), guided by simulations using a finite-difference time-domain (FDTD) Maxwell solver, it was found that combinations of existing roughness parameters describing both height and slope of the surface correlate well with emissivity changes. Furthermore, these parameters work well due to their apt description of surface features encouraging internal reflection, which is the phenomenon that increases emissivity when a surface falls under the geometric optical region conditions.

36 MATERIALS SCIENCE↗

Detecting keyhole porosity and monitoring process signatures in additive manufacturing: an in situ pyrometry and ex situ X-ray radiography correlation

Creation of pores and defects during laser powder bed fusion (LPBF) can lead to poor mechanical properties and thus must be minimized. Post-build inspection is required to ensure the printed parts contain acceptably low defect concentrations. These inspections are time consuming and costly, especially for large or complex parts. As a potential solution, in situ process monitoring can be used to detect the creation of defects, characterize local material behavior and predict expected component properties. However, the precise relationship between pore creation and in situ process monitoring still needs to be understood. In this work, high-speed infrared diode-based pyrometry and high-speed optical imaging signals were used to monitor LPBF printing of 446 stainless steel 316 L single tracks with varying laser power and velocity. Results indicate an increase in pyrometer signal and melt pool dimensions with increasing laser power and decreasing velocity in agreement with previous work. In addition, careful analysis of pyrometer signal reveals a distinct signature of the conduction-to-keyhole mode transition which was confirmed by metallography. Critically, pore defect initiation as characterized by ex situ X-ray radiography was correlated with in situ thermal monitoring signals to derive the probability of defect creation. Our results show that, in principle, a probabilistic prediction of pore formation can be achieved based on in situ high-speed pyrometry monitoring of the LPBF melt pool.

36 MATERIALS SCIENCE↗

Effect of powder layer thickness on the microstructural development of additively manufactured SS316

By Increasing the powder layer thickness we could increase material deposition rates and reduce build times during laser powder bed fusion (LPBF). However, increasing the powder layer thickness could also negatively affect the local melting and subsequent microstructure of the printed material. This study systematically investigated, for the first time, the defect evolution and microstructural changes of LPBF stainless steel 316 (SS316) processed by using various powder layer thicknesses of 40, 80, and 120 μm while also varying the laser dwell time for the pulsed laser. Through image analysis, the pore density was found to increase with increasing powder layer thickness, particularly when the dwell time was too high or too low. The maximum achievable density (>99%) was found over a wide processing window when using the smallest powder layer thickness of 40 μm between dwell times of 60 and 100 μs. Increasing the powder layer thicknesses to 80 and 120 μm resulted in maximum densities of 98.7 and 96.8%, respectively, but the window for acceptable laser dwell times that could achieve these densities narrowed considerably. A microstructural analysis of the melt pools was performed to measure the melt pool depths and widths, both of which increased with increasing dwell time. However, increasing the powder layer thickness did not affect the melt pool depth and only minorly affected the width. A sub-grain cellular structure distinguished the melt pool boundaries. The cell size increased with increasing dwell time and decreasing powder layer thickness. Moreover, the cell size was used to calculate a cooling rate that had a magnitude of 10 7 K/s and increased with increasing powder layer thickness.

36 MATERIALS SCIENCE↗

Multiscale and Machine Learning Modeling for Process-informed Microstructure Prediction in Additively Manufactured Materials using MALAMUTE

The Advanced Materials and Manufacturing Technologies (AMMT) program under the Department of Energy Office of Nuclear Energy aims to develop and qualify additively manufactured materials for nuclear applications. One key challenge to this is the microstructural variability observed in the additively manufactured products and their impact on the properties and performance of the material in extreme environments. AMMT is using a combination of high-throughput experimental and modeling techniques to accelerate qualification. Conventionally, in-situ and ex-situ characterizations and testing are performed to correlate different aspects of the additive manufacturing process to the final product and its performance. However, adopting a trial-and-error approach to experimentally evaluate the vast range of process parameters required to capture microstructural variability is cost-prohibitive. Modeling and simulation provide a comparatively inexpensive way to understand and correlate the microstructural evolution to the processing conditions. The modeling and simulation work-packages within the AMMT program aims to use physics-based and machine learning models to develop a digital twin for additive manufacturing that can correlate the process conditions to the final product and establish a process-structure-property-performance (PSPP) correlation. The melting and subsequent solidification that occurs during the additive process is a complex phenomenon that requires multiscale multiphysics analysis. This work package focuses on understanding the role of process variabilities on the unique microstructural characteristics of additively manufactured materials. Microstructural features at the subgrain level, such as compositional micro-heterogeneity and dislocation cells, are of particular interest here since they can influence the creep properties and radiation performance. Idaho National Laboratory’s Multiphysics Object-Oriented Simulation Environment (MOOSE), specifically the MOOSE Application Library for Advanced Manufacturing UTilitiEs (MALAMUTE) software, provides an ideal platform for developing the multiphysics multiscale model to explore the intricacies of the microstructural evolution during the AM processes within a single framework. Furthermore, given that such full-fidelity simulations can be computationally intensive, reduced order models are necessary to explore the PSPP space for additively manufactured materials in an efficient, reliable, and cost-effective way. This work focuses on capturing the microstructural variabilities at the subgrain level that are often missing in the part-scale models. In fiscal year 2025, we significantly advanced upon our work in the last fiscal year, in terms of the predictive capabilities of the physics-based and ML models, by adding the capabilities to capture subgrain-level micro-segregation during solidification using phase-field model and to predict the time-dependent dynamics of the AM process through the MOGPAR model. The alloy solidification model in MOOSE incorporates the thermodynamic properties and free energy relevant to 316 stainless steel. The model demonstrates the Cr and Ni segregation that occurs during solidification, including that the rate of solidification. The microstructural evolution model is connected to the process conditions via the surrogate model developed in this work. This enables predictions of the final microstructure in conjunctions with the manufacturing process. This work supports AMMT's rapid qualification goals by laying the foundation for an efficient and cost-effective model establishing the PSPP correlation for AM. The generated microstructures and predicted micro-segregation can be used by other work packages under AMMT to evaluate the properties and environmental response of the material at the mesoscale. Thus, this work helps to identify the key microstructural features at the subgrain level that are significant in property and performance predictions of additively manufactured components. This work will also provide inputs to the large-scale process variability models to reevaluate and validate assumptions and simplifications made in the part-scale models. Furthermore, through active learning this work can help identify the data need from both modeling and experimental sides for development of a robust digital twin for additive manufacturing and accelerate the AMMT's qualification efforts.

36 - MATERIALS SCIENCE↗

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↗

Alternating chempolishing and electropolishing for interior and exterior surface finishing of additively manufactured (AM) metal components

Additively manufactured (AM) components’ surface finishing is crucial in adopting them for intended applications in challenging environments involving fatigue, corrosion, high temperature, and nuclear radiation. In our prior research, chempolishing (C) was utilized as an electroless etching process that uniformly smoothens complex AM components’ accessible interior and exterior surfaces (Tyagi et al. Additive Manufacturing, 25:32–38, 22). A wide range of electropolishing (E) has been demonstrated for AM surface finishing. However, electropolishing can impact a surface that can be juxtaposed to counter electrode and can yield a very smooth surface to sub-micrometer level roughness. However, a knowledge gap exists about the impact of applying both approaches on the same surface one after another and what new advantages may arise because of combining two methods. This paper uses dual-stage liquid-based surface finishing strategies produced by alternating the chempolishing (C) and electropolishing (E) steps. Two dual-stage surface finishing approaches, i.e., chempolishing followed by electropolishing (CE) and electropolishing followed by chempolishing (EC), were performed on the 316 stainless AM steel component. Impacts of EC and CE approaches were compared with single-stage C and E surface finishing approaches. An optical microscope and mechanical profilometer were utilized to investigate the wide range of surface roughness parameters. CE and EC produced Ra ~ 1.4 µm and ~ 1.6 µm, respectively. Surface roughness on CE- and EC-treated AM samples was lower than those individually treated by C and E approaches. Scanning electron microscopy provided further insights into the microstructural difference between CE- and EC-treated AM samples. This paper reports a liquid contact angle study on CE- and EC-treated AM samples to provide insights into the relative difference in surface energy that is crucial for making coatings on AM parts. A spectroscopic reflectance study was also employed to register the difference in physical properties of AM components treated with CE and EC approaches. Further, this study reveals industrially practicable interior and exterior surface finishing approaches for complex AM metal components that require minimum tooling and real-time process monitoring.

36 MATERIALS SCIENCE↗