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Survey Corrosion Testing Methodologies for Additively Manufactured Materials – PNNL

The Advanced Materials and Manufacturing Technology (AMMT) Program intends to develop cross-cutting technologies in support of a broad range of nuclear reactor technologies, and to maintain U.S. leadership in materials and manufacturing technologies for nuclear energy applications. The overarching vision of the AMMT Program is to accelerate the development, qualification, demonstration, and deployment of advanced materials and manufacturing technologies to enable reliable and economical nuclear energy.

36 MATERIALS SCIENCE↗

Evaluation of an Additively Manufactured Respirator for Personnel Protection from Particulates

Additively manufactured respirators (AMRs) made using rigid plastic can be fitted with repurposed filter media to yield a wearable mask capable of passing a quantitative fit test with criteria set for commercial, N95 health care particulate respirators. This has been verified through an evaluation study assessing AMR masks fabricated using open-source design files and a commercial fused-filament fabrication machine, using N95 filter cloth and a P100 respirator cartridge. A few examples of filter media not designed for human respiratory protection were also evaluated in an AMR mask but did not demonstrate filtering sufficient to pass the N95 test criteria. All attributes of an AMR mask system must be considered during design and when testing performance, including the mask frame, gasket, and the cord used to secure the mask to the face. AMR masks are not the same as commercially available respiratory masks. If AMR masks are used as personal protective equipment (PPE) during a crisis when there is a shortage of regular PPE it is important that wearers are fully informed of the differences, tradeoffs, and risks associated with their use. Quantitative fit testing and proper training on how to don and doff the AMR mask are important to help achieve the best possible outcome when they are used.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Wide Bandgap Generation (WBGen): Developing the Future Wide Bandgap Power Electronics Engineering Workforce

This Final Technical Report (FTR) summarizes the work conducted at the Center for Power Electronics Systems (CPES) under the Wide-Bandgap Generation (WBGen) fellowship and traineeship program established by the Advanced Manufacturing and Technologies Office (AMMTO) of the U.S. Department of Energy Office of Energy Efficiency and Renewable Energy (EERE) at Virginia Tech, which had as main objective to train the next generation of U.S. citizen power engineers with wide-bandgap (WBG) power semiconductor expertise, with the intent to aid in fulfilling the future workforce needs in this field. The latter was deemed of strategic importance given the fast-paced growth observed—and predicted—in the demand of this technical expertise, whose practitioners have become the enablers and executioners of the electrification transformation process that not just the U.S., but the whole world, is currently undergoing as it seeks for more effective and efficient ways to use energy. As such, the WBGen program set forth to achieve its educational goals, which in addition sought to broaden the range of WBG-based power electronics by conducting research and development on high-efficiency grid apparatus and high-efficiency electrical power systems, and to also enhance the power engineering curriculum by formalizing WBG-oriented design procedures replacing existent yet now obsolete design procedures developed for Silicon (Si) based power electronics. This effort led CPES to spearhead the development of a new major within The Bradley Electrical and Computer Engineering (ECE) Department at Virginia Tech, namely Electronic Power and Energy Systems (EPES), which coalesced power electronics and power systems courses to provide undergraduate students with a strong formation in the power engineering field, while creating a pipeline of graduate students that could pursue the WBG-based curriculum and conduct research at CPES. In all, in what is considered a true success, eight of the twenty WBGen fellows that graduated program were recruited from the ECE department undergraduate cohort. The traineeship emphasized as well, from its beginning, the partnership with industry and national laboratories, which took advantage of the successful industry consortium at CPES that has historically been formed by 80–90 power and energy companies working in close collaboration with the center. This gave WBGen fellows the accessibility and possibility to conduct internships at partner facilities during the summer months, focused solely on the evaluation, testing, and adoption of WBG devices, which were many times tightly related to their respective research work and plans. In addition, WBGen fellows conducted their main research work within the confines of research programs at CPES conducted with these industry partners, providing them with a unique opportunity to develop not just their technical expertise—while advancing their knowledge, but to also learn and practice a slew of skills needed for their professional growth. As such, the fellows tackled a variety of WBG-related research topics, from device reliability and capability aspects as well as packaging and integration, encompassing the use of advanced materials and new structures, current sharing challenges, and insulation systems, to advanced gate-drivers with integrated sensors and protection mechanisms and active current- and voltage-based control, to optimized layouts seeking to maximize the switching and power processing performance of these devices, to power processing solutions adopting Gallium-Nitride (GaN) and Silicon-Carbide (SiC) power semiconductors for a variety of applications; including radiation-hardened converters for space dc distribution systems, direct three-phase ac-to-ac power converters for aerospace systems, dc-ac inverters for automotive traction drives, high-frequency isolated dc-dc battery chargers also for heavy transportation systems, and medium-voltage dc-dc and dc-ac converters for distribution systems and future power grids. The WBGen program ultimately graduated a total of 20 power engineers, all experts on WBG-based power electronics, awarding 18 M.S. and 2 PhD degrees in the process. These fellows, all U.S. citizens, allowed CPES to increase the number of citizens students to 33 % at the peak of the program, as the traineeship made possible the recruitment of talent with more attractive graduate research assistantship (GRA) contracts. Unfortunately, the present U.S. citizen enrollment at CPES has declined back to historic levels—approximately 10 %, as the regular GRA rates are not competitive enough when compared with entry-level industry jobs. In all, WBGen fellows published a total of 7 peer-reviewed journal articles, 44 papers at international technical conferences, made 42 presentations at international technical conferences, and filed 4 invention disclosures and patent applications, which have since then been granted by the U.S. Patent and Trademark Office (USPTO). Their contribution to CPES, Virginia Tech, the United States, and the world, has been significant, and continues to yield results thanks to the exemplary career that the fellows have initiated at many of the partners of the program, which include Wolfspeed, Raytheon Technologies, Infineon, Lockheed Martin, Dominion Energy, Northrop Grumman, Rivian, Aerospace Corporation, Sandia National Laboratory, National Renewable Energy Laboratory, John Hopkins University, and Virginia Tech.

14 SOLAR ENERGY↗

Embedding thermocouples in SS316 with laser powder bed fusion

Recent advances in manufacturing technologies have enabled the fabrication of complex geometries for a wide range of applications, including the energy, aerospace, and civil sectors. The ability to integrate sensors at critical locations within these complex components during the manufacturing process could benefit process monitoring and control by reducing reliance on models to relate surface measurements to internal phenomena. This study investigated embedding thermocouples in a SS316 matrix using laser powder bed fusion. Under optimal processing conditions, embedded thermocouples were characterized post-building, finding good bonding to the matrix with no melt pool penetration to the sensing elements. Futher, the embedded thermocouple performed similarly to an identical non-embedded thermocouple during thermal testing to 500 °C with only a slight difference in response time, which was attributed to the differences in mass and the associated thermal time constants.

image analysis↗

Cost of Using Laser Powder Bed Fusion to Fabricate a Molten Salt-to-Supercritial Carbon Dioxide Heat Exchanger for Concentrating Solar Power

Advances in manufacturing technologies and materials are crucial to the commercial deployment of energy technologies. We present the case of concentrating solar power (CSP) with molten salt (MS) thermal storage, where low-cost, high-efficiency heat exchangers (HXs) are needed to achieve cost competitiveness. Here, the materials required to tolerate the extreme operating conditions in CSP systems make it difficult or infeasible to produce them using conventional manufacturing processes. Although it is technically possible to produce HXs with adequate performance using additive manufacturing, specifically laser powder bed fusion (LPBF), here we assess whether doing so is cost-effective. We describe a process-based cost model (PBCM) to estimate the cost of fabricating a MS-to-supercritical carbon dioxide HX using LPBF. The PBCM is designed to identify modifications to designs, process choices, and manufacturing innovations that have the greatest effect on manufacturing cost. Our PBCM identified HX design and LPBF process modifications that reduced projected HX cost from $\$750$ per kilo-Watt thermal (kW-th) ($\$8$ /cm 3 ) to $\$350$ /kW-th ($\$6/$ cm 3 ) using currently available LPBF technology, and down to $\$220$ /kW-th ($\$4$ /cm 3 ) with improvements in LPBF technology that are likely to be achieved in the near term. The PBCM also informed a redesign of the HX design that reduced projected costs to $\$140$ –160/kW-th ($\$3$ /cm 3 ).

36 MATERIALS SCIENCE↗

Advanced Sensors for Hydrogen Technology

This gap analysis study included all parts of the hydrogen value chain, from hydrogen generation, to storage, and end use, with the exception of transportation applications. While these research projects are not always commercially viable, they are important in advancing technology, and especially in reaching goals such as improved efficiency and reducing emissions. Without emissions targets enforced by the government, or incentives for industry for emissions reduction, investing in advanced technology and manufacturing system upgrades can be exceedingly difficult to justify. This analysis identifies and prioritizes sensor R&D development areas that are critical to enable the hydrogen economy.

08 HYDROGEN↗

Process Intensification for Nanostructure Aluminum Extrusions

A new technology called Shear Assisted Processing and Extrusion (ShAPE™), pioneered at the Pacific Northwest National Laboratory (PNNL), has the potential to revolutionize the US extrusion industry. Maturation of the ShAPE™ process would create a new cross cutting US manufacturing technology that advances three key the objectives within AMO; namely, nanomaterials processing, process intensification, and materials for extreme and harsh environments. PNNL and SCM Metals Products, Inc. (SCM), a division of Kymera International, will collaborate to mature the ShAPE™ extrusion process beyond TRL 3 to increase the likelihood of its adoption by industry. PNNL’s custom (one-of-a-kind in the world) ShAPE™ machine will be used to extrude round rods of high strength aluminum alloy feedstock powder provided by SCM. As proof-of-concept, PNNL has previously extruded 5 mm diameter rods with SCM aluminum alloy powder AL-12.4TM. This project aims to scale up the process to a diameter of 25 mm while retaining the excellent mechanical properties achieved for the 5 mm diameter rods. The degree of process intensification with ShAPE™ will also be estimated. The primary objectives of this project are as follows. 1) Fabricate 25 mm diameter nanostructured extrusions in bulk, directly from AL-12.4TM aluminum alloy powder without the need for canning, degassing, compaction, and other intermediate steps typical of powder metallurgy extrusion. 2) Achieve a microstructure with an ultrafine grained (UFG <1 µm) aluminum matrix having refined and homogenously distributed nanoscale second phases. 3) Show that the ram force can be significantly reduced compared to conventional powder metallurgy extrusion of the same material and estimate the extent of process intensification that may be possible with ShAPE™. 4) Demonstrate improved high-temperature mechanical properties compared to conventional extrusion of the same material. The following tasks will be undertaken to achieve these objectives. PNNL will develop the die set and process parameters necessary to fabricate Al-12.4TM extrusions with a 25 mm diameter. Microstructural analysis will be performed by PNNL while mechanical testing will be conducted by SCM. With information learned from the process development and characterization, PNNL will perform an estimate of the degree of process intensification that may be possible with ShAPE™.

42 ENGINEERING↗

Central Density and Low-Mode Perturbation Control of Inertial Confinement Fusion Dynamic-Shell Targets

The dynamic-shell target is a new class of design for inertial confinement fusion (ICF). These targets address some of the target fabrication challenges prevalent in current ICF targets and take advantage of advances in manufacturing technologies. This study first examines how the dynamic-shell design can be used to control the density of the central region and therefore convergence ratio, thus expanding the design space for ICF. Additionally, the concern of low-mode perturbation growth is considered. A new class of high-performing beam configurations, based on icosahedral polyhedra and charged-particle simulations is proposed. These configurations achieve low levels of irradiation nonuniformity through selection of beam shapes that suppress the dominant symmetrical mode.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

An Overview of Emerging Nuclear Sensor Technologies: Challenges, Advancements and Applications

Nuclear sensors are essential for detecting and measuring nuclear radiation in various applications, including nuclear power plants, medical imaging, and environmental monitoring. Traditional nuclear sensors have served these fields for decades, but recent advancements in emerging sensor technologies offer novel improvements in accuracy, sensitivity, and reliability. This review presents an up-to-date overview of recent progress in the advancements of nuclear sensor technologies, their diverse applications, challenges in implementation, and opportunities for future research.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

A Primer on Using Analysis to Guide Plastic Circularity

BOTTLE, funded by DOE's Advanced Materials & Manufacturing Technologies Office and Bioenergy Technologies Office (BETO), conducts analysis-guided R&D to change the way we recycle plastics. But what does analysis really mean? In this webinar, BOTTLE Analysis Co-Lead Dr. Taylor Uekert, a researcher with the National Renewable Energy Laboratory (NREL), will introduce key analysis techniques such as techno-economic analysis, life cycle assessment, and environmental justice evaluation. Relevant to both analysts and non-analysts, Dr. Uekert will cover the basics of analysis techniques and discuss how these methods are conducted and interpreted. She will provide examples from the BOTTLE portfolio demonstrating their use in benchmarking and optimizing the costs and environmental impacts of new innovations in plastic redesign and recycling. If you are working in the plastics recycling field - from experimental work to analysis to community-focused projects - you won't want to miss this talk. The webinar will end with a Q&A session.

analysis↗

Preliminary Report on Compositional Specification for Printed 316SS

The Advanced Materials and Manufacturing Technologies Program is focused on accelerating the development and deployment of advanced materials and components fabricated via additive manufacturing (AM). A key challenge for the widespread adoption of AM is the variability in material properties, which can originate from powder feedstock, process parameters, geometry, and the machine. AM powder feedstock compositions are based on those developed for conventional manufacturing. However, the smaller melt pools combined with multiple melt cycles over the course of a build can have substantial effects on the local phase selection resulting from minor batch-to-batch feedstock variability. Therefore, this report focuses on coupling CALPHAD calculations with data mining and visualization to aid the development of compositional specifications for stainless steel 316, an important alloy for nuclear applications and suitable for AM. This work reports that δ-ferrite formation has a stronger dependence on the amount of nickel in the alloy despite nickel being an austenite stabilizer. These findings show the need for exercising a tighter control on the amount of nickel in the alloy compared with the amount of chromium, which is a ferrite stabilizer.

36 MATERIALS SCIENCE↗

Data-Driven Optimization of the Processing Window for 316H Components Fabricated Using Laser Powder Bed Fusion

The Advanced Materials and Manufacturing Technologies Program is focused on accelerating the development and deployment of advanced materials and components fabricated via additive manufacturing with a specific focus on laser powder bed fusion (LPBF). As an initial case study, the program has selected 316H stainless steel (SS) as an initial material around which to develop a code case development strategy. This strategy involves two parallel approaches: (1) an equivalency approach whereby round-robin testing across multiple collaborating laboratories demonstrates repeatability in processing and direct comparisons with conventional wrought 316H material and (2) a revolutionary approach to code qualification combining in situ data collection and high-fidelity modeling to capture, predict, and bound the performance of LPBF 316HSS components. As part of this campaign, this work package has initiated an extensive process optimization campaign across three laboratories, each printing variations of LPBF 316HSS using three different LPBF units (Concept Laser, EOS, and Renishaw). In FY23, ORNL has focused on unique experimental designs spanning wide ranges in energy inputs and turning knobs such as scan speed, laser power, hatch spacing, layer thickness, spot size, scan rotation, and more. On the Concept Laser M2, 72 different combinations of processing variables were investigated with duplicate samples and different powder compositions. In total, 252 samples were printed with combined in situ sensing data. A parallel design of experiments was conducted on the Renishaw AM400 with an additional 390 printed specimens for analysis. All 642 miniature specimens, each with unique features included in each print to capture geometry-related heterogeneity, were subjected to high-throughput x-ray computed tomography (XCT) analysis to enable the downselection of specific processing parameters of interest. Then, using electrical discharge machining (EDM), miniature tensile specimens were extracted for mechanical testing and microscopy investigations. From the analysis performed in FY23, it was found that powder composition drastically affects the resulting microstructure and mechanical performance of 316SS. Specifically, changing from 316L to 316HSS powder results in a wide range of grain sizes with varying degrees of preferred grain orientation, which increases as a function of energy density. It was also found that due to stored heat in thin fin–type features, large microstructural differences can be seen within one part printed with one set of processing parameters. These variations in microstructure features, including grain size, the nanoscale dislocation structure, and grain texture, will all affect the irradiation performance and high-temperature mechanical performance of LPBF 316HSS parts. Two sets of concept laser processing parameters, spanning both refined and columnar grain structures, were scaled to print larger 316H builds for campaign testing (high-temperature creep and irradiation). In addition, at least two optimized processing parameter sets were identified for the Renishaw AM400 for round-robin testing in FY24 with Argonne National Laboratory. Future work includes printing samples using identical parameters identified by partner institutions, providing material for corrosion and high-temperature mechanical testing, and continuing evaluations of heterogeneity in larger printed parts.

36 MATERIALS SCIENCE↗

Data-Driven Optimization of the Processing Window for 316H Components Fabricated Using Laser Powder Bed Fusion

The Advanced Materials and Manufacturing Technologies Program is focused on accelerating the development and deployment of advanced materials and components fabricated via additive manufacturing with a specific focus on laser powder bed fusion (LPBF). As an initial case study, the program has selected 316H stainless steel (SS) as an initial material around which to develop a code case development strategy. This strategy involves two parallel approaches: (1) an equivalency approach whereby round-robin testing across multiple collaborating laboratories demonstrates repeatability in processing and direct comparisons with conventional wrought 316H material and (2) a revolutionary approach to code qualification combining in situ data collection and high-fidelity modeling to capture, predict, and bound the performance of LPBF 316HSS components. As part of this campaign, this work package has initiated an extensive process optimization campaign across three laboratories, each printing variations of LPBF 316HSS using three different LPBF units (Concept Laser, EOS, and Renishaw). In FY23, ORNL has focused on unique experimental designs spanning wide ranges in energy inputs and turning knobs such as scan speed, laser power, hatch spacing, layer thickness, spot size, scan rotation, and more. On the Concept Laser M2, 72 different combinations of processing variables were investigated with duplicate samples and different powder compositions. In total, 252 samples were printed with combined in situ sensing data. A parallel design of experiments was conducted on the Renishaw AM400 with an additional 390 printed specimens for analysis. All 642 miniature specimens, each with unique features included in each print to capture geometry-related heterogeneity, were subjected to high-throughput x-ray computed tomography (XCT) analysis to enable the downselection of specific processing parameters of interest. Then, using electrical discharge machining (EDM), miniature tensile specimens were extracted for mechanical testing and microscopy investigations. From the analysis performed in FY23, it was found that powder composition drastically affects the resulting microstructure and mechanical performance of 316SS. Specifically, changing from 316L to 316HSS powder results in a wide range of grain sizes with varying degrees of preferred grain orientation, which increases as a function of energy density. It was also found that due to stored heat in thin fin–type features, large microstructural differences can be seen within one part printed with one set of processing parameters. These variations in microstructure features, including grain size, the nanoscale dislocation structure, and grain texture, will all affect the irradiation performance and high-temperature mechanical performance of LPBF 316HSS parts. Two sets of concept laser processing parameters, spanning both refined and columnar grain structures, were scaled to print larger 316H builds for campaign testing (high-temperature creep and irradiation). In addition, at least two optimized processing parameter sets were identified for the Renishaw AM400 for round-robin testing in FY24 with Argonne National Laboratory. Future work includes printing samples using identical parameters identified by partner institutions, providing material for corrosion and high-temperature mechanical testing, and continuing evaluations of heterogeneity in larger printed parts.

36 MATERIALS SCIENCE↗

Transitioning to a Sustainable, Circular Economy for Plastics [Workshop Report]

The “Transitioning to a Sustainable, Circular Economy for Plastics” workshop, coordinated by the Bioenergy Technologies Office (BETO) and the Advanced Materials and Manufacturing Technologies Office (AMMTO) in collaboration with The Climate Pledge, brought together a diverse group of stakeholders to discuss the current challenges and opportunities in transitioning to a sustainable, circular economy for plastics in the United States. Input from the workshop will be used to ensure the U.S. Department of Energy’s (DOE) Strategy for Plastics Innovation (SPI) evolves with the rapidly changing landscape. Presentations, panel discussions, and breakout sessions provided a framework for sharing information and building direct connections among stakeholders across the value chain. This document summarizes the content discussed at the workshop to provide an update on the state of plastic sustainability in the United States.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

Evaluation of In-Situ AM Process Monitoring Techniques and Potential for Detecting Process Anomalies and Undesirable Microstructures

The US Department of Energy’s Advanced Materials and Manufacturing Technologies (AMMT) program is pursuing rapid qualification of new materials for fabrication of nuclear relevant components using advanced manufacturing techniques. Particular interest is placed on code-qualifying stainless steel (SS) 316H processed by laser powder bed fusion (LPBF) additive manufacturing. A paradigm that incorporates data from in-situ sensing during the printing, ex-situ characterization, and advanced artificial intelligence–based models was established under the Transformation Challenge Reactor (TCR) program to develop a pedigree for each fabricated component that could be tracked from the feedstock to the component’s release for application. Under the TCR program, the Peregrine software was developed as a tool for incorporating the vast amounts of in-situ and ex-situ characterization data collected; all data stored on a rapidly growing digital platform. The digital platform allows for users to link site-specific process anomalies to the macro- and microstructure. The platform will eventually be able to predict component performance, which will be crucial to qualifying materials and components in risk-averse industries such as those supporting and building nuclear reactors. Current in-situ process monitoring techniques that are already integrated with software like Peregrine are advantageous for identifying process anomalies including powder spatter, component edge swelling, recoating-build interactions, and so on. However, additional data are required to fully predict the resulting microstructures needed for identifying relationships to component performance. The rapid cooling rates observed in LPBF are some of the highest of any bulk manufacturing process, resulting in heterogenous microstructures and typically causing anisotropy in mechanical properties. Moreover, evolved residual thermal stresses are high, which can cause severe defects such as delamination or cracking. Therefore, other in-situ monitoring methods are warranted for exploration to measure and map the thermal history, and potentially the stress state, of each build. This report summarizes different in-situ monitoring strategies proposed for LPBF with a focus on the more developed sensor systems. Novel capabilities for measuring melt pool temperatures are also addressed to better inform modeling efforts.

36 MATERIALS SCIENCE↗

Prototyping of N95 Respirators Using Additive Manufacturing NETL NLVB (Final Report)

Final report for National Energy Technology Laboratory (NETL) project involving the use of advanced manufacturing and 3D printing technologies to help address personal protective equipment (PPE) shortages due to COVID-19. Work was performed in support of Joint DOE Laboratory Plan for Manufacturing Medical Supplies and funded through the DOE Office of Science.

3D Printing↗

A NEA review on innovative structural materials solutions, including advanced manufacturing processes for nuclear applications based on technology readiness assessment

The Nuclear Energy Agency (NEA) Expert Group on Innovative Structural Materials (EGISM) was established in 2008 under the guidance of the Nuclear Science Committee (NSC). Its objectives are to conduct joint and comparative studies to support the development, selection and characterisation of innovative structural materials that can be implemented in advanced nuclear fuel cycles, under long service lifetime and extreme conditions, such as high temperature, high dose/dose rate and corrosive chemical environments. In this context of growing interest and initiatives, the EGISM initiated at the beginning of 2018 an activity among its members to: Identify, in a non-exhaustive way, the currently existing programs on innovative materials and fabrication processes in NEA member countries and China; Establish a first cartography of the activities that are underway on these topics and identify common subjects and thematic; Propose a Technology Readiness Level scale to estimate the maturity of both innovative materials and fabrication processes; Carry out a reflection on what the enablers are to quickly climb this TRL scale, as well as the obstacles, in order to identify solutions to overcome them. This paper first gives definitions shared between the EGISM members on what are considered as advanced structural materials solutions. Next, some international initiatives for the accelerated development of high performance materials are presented both in non-nuclear and nuclear fields. Then, the methodology adopted for technology readiness assessment is explained. A non-exhaustive synthesis of the projects identified among the EGISM members on innovative structural materials and advanced manufacturing solutions such as additive manufacturing is presented. The TRL level of these projects is evaluated. A focus is also made on some of these projects to illustrate and explain the TRLs chosen as well as highlighting enablers or obstacles identified to climbing up the TRL scale.

36 MATERIALS SCIENCE↗