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DOE OSTI2023

Linkage Transformations in a Three-Dimensional Covalent Organic Framework for High-Capacity Adsorption of Perfluoroalkyl Substances

Despite their many advantages, covalent organic frameworks (COFs) built from three-dimensional monomers are synthetically difficult to functionalize. Herein, we provide a new synthetic approach to the functionalization of a three-dimensional covalent organic framework (COF-300) by using a series of solid-state linkage transformations. By reducing the imine linkages of the framework to amine linkages, we produced a more hydrolytically stable material and liberated a nucleophilic amino group, poised for further functionalization. We then treated the amine-linked COF with diverse electrophiles to generate a library of functionalized materials, which we tested for their ability to adsorb perfluoroalkyl substances (PFAS) from water. The framework functionalized with dimethylammonium groups, COF-300-dimethyl, adsorbed more than 250 mg of perfluorooctanoic acid (PFOA) per 1 g of COF, which represents an approximately 14,500-fold improvement over that of COF-300 and underscores the importance of electrostatic interactions to PFAS adsorption performance. In conclusion, this work provides a conceptually new approach to the design and synthesis of functional three-dimensional COFs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Development of Low-Cost, High-Performance, Easy-To-Apply, Non-Flammable, Inorganic Phase Change Material (PCM) Technology (Project Final Report)

This report describes a 45-months long research program focused on the development of novel, easy-to-apply, non-flammable, and high-performance inorganic phase change materials (PCMs) for building and industrial applications. The University of Massachusetts Lowell (UML) formed a world-class team consisting of researchers form InsolCorp (only N. American manufacturer of inorganic PCM systems for building applications), and a group of industrial advisors, to develop a universal/multipurpose, simple-to-manufacture and cost-effective PCM technology. The project team expects that the results of this work will spur in the future the adoption of thermal storage materials – a key building energy saving technology as identified by DOE BTO – for a variety of building envelope applications. The main goal of this project was to demonstrate a suite of low-cost, multipurpose, and durable inorganic PCM formulations with phase transition temperatures encompassing typical building applications (between +5 o C and +55 o C). The first objective was to design, fabricate, and experimentally validate a performance of inexpensive, durable, highly efficient, non-flammable, and easy to manufacture PCMs. To allow a variety of building applications, the project team focused on formulations that exhibit repeatable phase transitions between +5 o C and +55 o C. To follow the DOE BTO cost efficiency target without compromising thermal performance, our work was based on inorganic compounds (mostly salt hydrates) and their blends, which represent a fraction of the cost of most of organic PCMs with about twice as high density as well as significantly higher thermal conductivity and phase change enthalpy. The second objective was to develop easy-to-manufacture and -install packaging/encapsulation designs that are 1) a superior barrier to current state-of-the-art macro-packaging, which significantly reduces the risk of loss of hydration water and PCM leak, and 2) optimal in enhancing the heat exchange rates with the surroundings and within the PCM core to ensure complete charging/discharging of the entire PCM within the product. Finally, the project’s intend was to scale-up the fabrication process to demonstrate installation on system-scale applications, and to validate the performance under field conditions. This work aimed at developing low-cost, high-energy storage, and reliable latent heat storage technology for building applications. This development was realized by formulating and integrating the following two technology components: 1) inorganic salt hydrate based PCMs that have high latent enthalpies and are low-cost and durable, and 2) PCM encapsulation (packaging) technology that maximizes PCM concentration and enhances heat transport characteristics in the product and with the external environment/materials. High thermal storage capacity, low cost and fire resistance are key to the building market entry for PCM technology. Therefore, the project’s focus was on salt-hydrate-based formulations which satisfy all these criteria. Packaging and/or encapsulation of PCM is a key processing step. The project team recognized that a low-cost and simple-to-manufacture salt hydrate-based PCM technology holds the best chance to be successful in the building construction market, a market which is traditionally extremely sensitive to cost and where commodity thermal insulations are the benchmark for envelope-related energy saving measures. That is why, in this project, the main intention was to minimize the production cost and maximize the product energy storage density without sacrificing the PCM performance. It was achieved through: 1. Minimizing the non-PCM components (plastics, additives, packaging/encapsulation materials, etc.) because they are significantly more expensive than salt hydrates, 2. Using highly thermally conductive and lightweight PCM carrier (packaging material) to facilitate more complete phase cycling, and 3. Optimizing the thickness and minimizing air spaces in product design (such as in pouched PCM). For this purpose, our approach was to enable an easy system design, including selection of the PCM operating temperatures, optimizing the necessary heat storage capacity (by stacking together several layers of PCM products), and if needed, a synchronized usage of PCM products of different temperatures. A specially designed, robust, highly thermally conducting and highly impermeable packaging (to retain salt hydrate water during phase transition cycles) was designed and tested to increase the overall system thermal performance and durability. All PCM products developed during this project were tested in both lab scale and in full scale field conditions. It is expected that, after further developments and commercialization, the developed PCM technologies may be also applied in space conditioning, energy storage technologies, and heat transfer applications.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

DOE OSTI2022

H-Canyon Jumper Gasket Sealing Evaluation

H-Canyon Documented Safety Analysis approved December 2019 credits the leak integrity of H-Canyon (HCA) process tanks, piping, and jumpers in preventing the release of radioactive material in a post seismic environment. Demonstration of leak tightness capability for this equipment was achieved through substantial analytical effort. However, one potential weak point that affects leak integrity exists at the gasketed joint between Hanford Connectors (HC) and nozzles. Review of the HCA Crane Log over a three-year period indicates the HCs periodically leak. Savannah River National Laboratory (SRNL) was requested to perform gasket compression tests that evaluate gasket relaxation characteristics, i.e., creep, and provide improvements to the HC installation process that can reduce or eliminate the frequency of leaks at HCs. A HC torque value of 312 ft-lbf is the target value used because it is the minimum torque value, with 95% confidence, when an unlubricated HC is impacted for standard sealing period of 9 seconds. In the HCA pipe-jumper connections are installed remotely by using HCs. HCs inherently add to the uncertainty of a gasketed joint because a calibrated torque value cannot be applied. The gasket material is a special material made of asbestos-fiber impregnated with Teflon. This material has been used for decades and generally performs well but does leak intermittently as gaskets creep and preloaded torque is lost. Gasket types are either snap-ring (SR) or lampshade (LS). Both gasket types cover the same seating area. The SR gasket is designed to remain with the jumper when the jumper is removed leaving the nozzle faces clean of any debris. SR gaskets are initially installed when the jumper is fabricated. Changing gaskets is time consuming and the radioactive environment presents risks to personnel. When jumpers are removed LS gaskets could be used to better seal the connection to reduce down time and ALARA concerns. That is, an LS gasket would be remotely positioned over the nozzle and the HC reinstalled. Testing also included two situations not typical of plant operation. One situation was the use of the non-standard double-layered gaskets (DG), and the other situation was the use of a LS without removal of the installed SR gasket. The DG was used when the supply of LS gaskets ended, so that testing could continue. It was of interest to demonstrate this gasket’s creep response because the DG, which was two gaskets glued together, was thicker than the LS gasket and the thicker material was expected to elicit a greater creep characteristics. The second situation of using two gaskets together by installing an LS gasket without removing the installed gasket is not allowed by the ASME Codes. However, by demonstrating the creep history of such a gasket arrangement it could be considered as an option that could possibly seal a connection while significantly reducing operational down time and personnel risk. Forty tests were conducted, and the overall results demonstrate the initial applied force and how the gasket changes with time. The change in sealing force, in terms of torque, was then measured to obtain a force history as the gaskets creep. This report documents the results of those tests as well as the method used to perform the tests.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

Hydrogen Permeation in FeCrAl APMT Alloy for Accident Tolerant Fuel Cladding

Iron-chromium-aluminum (FeCrAl) alloys such as APMT (advanced powder metallurgy tubing) are candidate materials to replace zirconium alloys for the light water reactor fuel cladding. This alloy meets the requirements to be a material more tolerant of high-temperature accidents than the current zirconium alloys. One concern is that the use of FeCrAl may result in an increase in tritium presence in the coolant compared to the current design. The aim of the current research was to obtain effective diffusion coefficients (D eff ) for hydrogen through APMT using the Devanathan-Stachurski cell. Results showed that at 30°C the D eff value was 2.8 × 10 -8 cm 2 /s. Results also showed a linear relationship between the permeated hydrogen flux and the inverse of the test specimen thickness, which demonstrated the validity of the permeation measurements.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Large Scale Synthesis of Manganese Oxide/Reduced Graphene Oxide Composites as Anode Materials for Long Cycle Lithium Ion Batteries

Manganese oxides have been frequently used as cathodes in primary batteries. Applications of manganese oxides in secondary batteries are limited by low electrical conductivity and rapid capacity fading because of electrode pulverization and aggregation. In this study, a solid-state synthetic strategy is presented that successfully combines nanosize (~ 50 nm) nickel doped α-MnO 2 with reduced graphene oxides as highly stable composite anodes in lithium ion batteries. The synthesis approach is easy to scale up and suitable for industrial applications. Here, the rationally designed Ni-α-MnO 2 /RGO was tested in galvanostatic half coin cells for Li + charge-discharge studies. The results show that this composite maintains a high capacity of 615 mAh g -1 even after 200 cycles at a high current rate of 1 C (830 mA g -1 ), and with a high Coulombic efficiency near 99%. The anodes exhibit excellent rate capability in a wide range of rate testing from 0.2 to 10 C, without showing capacity decay. This superior anode performance is ascribed to the reduced size of α-MnO 2 domains that are well dispersed in an RGO matrix, which affords good ionic/elec. cond., low charge transfer resistance and mitigates issues of vol. expansion of the anodic active materials. This study opens up an avenue for developing the manufacturing of high-performance electrodes for real applications, such as batteries in electrical vehicles.

25 ENERGY STORAGE↗

DOE OSTI2021

Determination of oxidation rates and volatile oxidation products for HTGR graphite matrix material exposed to steam atmospheres

High-temperature gas-cooled reactors (HTGRs) in operation use tristructural isotropic (TRISO) particles embedded in graphite and carbonized resin matrix to form the fuel element. This graphite matrix material serves as a supportive structural element, heat transfer medium, and neutron moderator. In HTGR designs, fuel compacts are exposed to helium coolant, which facilitates high outlet temperatures (750°C 2 O, 800°C 2 , and H 2 , are quantified in varied oxidant atmospheres using a coupled thermogravimetric analyzer and mass spectrometer. Furthermore, oxidation rates reported here for varied steam (H 2 O [g]) atmospheres are predominantly linear and comparable with literature values in the range of tested temperatures (800–1200°C). Changes in dominant matrix oxidation products from primarily CO to a mixture of CO, CO 2 , and H 2 were observed at higher temperatures (≥1000°C) and steam atmospheres (≥5 kPa pH 2 O). Kinetic data indicates that there was no shift in oxidation regime with chemical oxidation occurring at all temperatures and H2O (g) atmospheres tested. These data provide insight into the oxidation behavior of graphite matrix material and will inform future testing conditions, notably mixed atmospheric conditions, of HTGR fuel elements.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Innovative Nuclear Materials Outboard-A Project Specimen Preparation Guide

The Innovative Nuclear Materials (INM) Program was recently established by the U.S. Department of Energy (DOE) to develop advanced material technologies for use in nuclear reactors. The INM program is presently focused on researching in-core non-fueled materials for application in fast spectrum nuclear reactors. The widespread deployment of fast reactors continues to be a prominent aspiration for advanced nuclear technology developers. However, companies working to license these reactors have no choice but to rely on historic material technologies since further optimization and advancement of these materials is impeded by the lack of fast neutron irradiation test facilities. INM-OA is a non-fueled drop-in experiment which will irradiate material specimens of interest to fast reactor applications. This experiment will be irradiated at Idaho National Laboratory (INL) in the Advanced Test Reactor (ATR) outboard-A (OA) position during normal and high temperature steady state (HTSS) cycles. It will include material specimens supplied by members of the INM program and will utilize a cadmium-lined basket to filter out incident thermal neutrons, thus simulating a faster neutron energy spectrum. Material specimens will undergo post-irradiation examination including microscopy and mechanical testing. In addition to absorption reactions, fast neutrons cause microstructural damage in materials by atom displacement, which can cause exacerbated changes in physical properties and behavior. Thus, the data obtained from the INM-OA experiment will be crucial for understanding the engineering-scale behavior of reactor materials. This document is intended for the Principal Investigators providing samples for this project. Topics included are a general description of the experiment, the irradiation experiment/capsule design, sample geometries, number of samples to be provided, documentation to be provided, a brief list potentially useful characterization methods that can be leveraged at INL, and other miscellaneous requirements specific to this project. This document is intended for informational use only.

innovative nuclear materials↗

DOE OSTI2020

Image-driven discriminative and generative machine learning algorithms for establishing microstructure–processing relationships

We investigate methods of microstructure representation for the purpose of predicting processing condition from microstructure image data. A binary alloy that is currently under development as a nuclear fuel was studied for the purpose of developing an improved machine learning approach to image recognition, characterization, and building predictive capabilities linking microstructure to processing conditions. Here, we test different microstructure representations and evaluate model performance based on classification accuracy. A classification accuracy of 95.8% was achieved fordistinguishing between micrographs corresponding to ten different thermo-mechanical material processing conditions.We find that our newly developed microstructure representation describes image data well, and the traditional approachof utilizing area fractions of different phases is insufficient for distinguishing between multiple classes using a relativelysmall, imbalanced original data set of 272 images. To explore the applicability of generative methods for supplementing such limited data sets, generative adversarial networks were trained to generate artificial microstructure images. Two different generative networks were trained and tested to assess performance. Challenges and best practices associated with applying machine learning to limited microstructure image data sets is also discussed. Our work has implications for quantitative microstructure analysis, and development of microstructure-processing relationships in limited data sets typical of metallurgical process design studies.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Development and preliminary validation of a mechanistic multiscale model for fuel-cladding chemical interaction in metallic nuclear fuels

Despite decades of fuel rod material and design improvements, fuel-cladding chemical interaction (FCCI) remains the single-most lifetime-limiting behavior for modern metallic fuel rods. Constraining fuel lifetime increases operating costs, limiting the economic viability of commercializing metallic nuclear fuel technology. A mechanistic multiscale model utilizing the finite element method-based MARMOT and BISON codes was developed to more confidently predict cladding-side FCCI and its impact on fuel performance. The new BISON model incorporates mesoscale models for the effects of fuel microstructure evolution on the transport of wastage-inducing lanthanides through the fuel and for the kinetics of cladding wastage layer growth. The mesoscale models, in turn, build on lanthanide transport property data obtained from the atomistic scale. Preliminary validation studies using wastage thickness and cladding profilometry data from four fuel rods irradiated in Experimental Breeder Reactor II experiment X447 and one fuel rod from Fast Flux Test Facility experiment IFR1 show that the new model predicts cladding wastage and its effects on cladding deformation as well as existing empirical FCCI correlations. The new model is expected to aid in the design of new metallic fuel concepts, including fuel additives, cladding liners, and sodium-free annular fuel geometries. In conclusion, future work will focus on broader validation and refinement of the model’s treatment of different fuel alloys and cladding materials.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2020

An Initial Assessment of the Design Margins of Different ASME Section III, Division 5 Design Rules

This report develops a method for assessing the design margin of the ASME Section III, Division 5 Class A design rules, focusing on a definition of margin as the ratio between the actual, expected component life and the ASME design life. Full inelastic finite element simulations with a complete damage model capturing the available creep, creep-fatigue, fatigue, and tension test failure data produce the expected component lives, which can then be compared to corresponding ASME design calculations. The focus of this particular work is on Alloy 617 and the ASME creep-fatigue design rules, but the approach is general and could be applied to other design limits and to other materials. A margin assessment of a representative Alloy 617 component shows the ASME creep-fatigue design rules applied to this component have a margin of 10 on design life. The report describes several challenges in completing a more comprehensive margin assessment of the ASME rules, in particular challenges in developing probabilistic assessment methods for high temperature structural components. The report details these challenge and discusses the immediate possibilities of the deterministic margin assessment method developed here.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2022

Developing novel electrodes with ultralow catalyst loading for high-efficiency hydrogen production in proton exchange membrane electrolyzer cells

Hydrogen plays more crucial roles for decarbonizing the planets and meeting the climate challenges because of its high energy density and zero-emission. It can be produced with proton exchange membrane electrolyzer cells (PEMECs) driven by sustainable and renewable energy resources. Although PEMECs have a number of advantages, including high purity production, quick response, and the ability to operate at high pressure facilitating the gas delivering, their performance and cost greatly hinder their commercial-scale applications. To achieve high-efficiency and cost-reduced hydrogen production in PEMECs, we proposed thin engineered liquid/gas diffusion layers (LGDLs) and associated electrodes, i.e., catalyst-coated LGDLs (CCLGDLs), over conventional porous transport layers (PTLs) and catalyst-coated membranes (CCMs). The research approaches in this project are based on material synthesis, in-situ and ex-situ characterizations, component design and treatment, numerical modeling, and cost analysis. The thin and tunable LGDLs (TT-LGDLs) and CCLGDLs were successfully developed with great performance improvement as demonstrated in lab-scale, bench-scale, and system-scale electrolyzer tests. The electrode thickness was reduced from 370 µm to less than 100 µm with simplified fabrication processes. With the catalytically enhanced Ir-based catalyst coating, the as-developed CCLGDLs with a catalyst loading of 0.34 mg Ir /cm 2 achieved a cell performance of 1.77 V at 2 A cm -2 , exhibiting the catalyst mass activity enhanced by >20 times with significant catalyst saving over conventional catalyst cell design. In-situ PEMEC characterizations, including the current distribution mapping and high-speed and multiscale visualizations, were conducted for a deeper understanding of mass transport and electrochemical reactions within an electrolyzer with LGDLs and CCLGDLs. A 2D cell model was developed and validated for the enhanced performance on TT-LGDL through reducing ohmic losses due to nonuniform hydration and water transport. Further, the cost analysis results have shown a path to move beyond equivalency and surpass costs associated with the project baseline. In this project, the design and fabrication of TT-LGDLs and CCLGDLs will contribute to the performance enhancement, manufacturing simplification, and cost reduction for PEMECs and other energy conversion devices, thus shortening their pathways towards commercialization. This project also provides a good foundation for furthering the in-situ reaction interface research.

08 HYDROGEN↗

DOE OSTI2020

NMDQi Nuclear Materials Discovery and Qualification Initiative Conference Overview

The Nuclear Materials Discovery and Qualification Initiative (NMDQi) is designed to accelerate nuclear materials qualification to fulfill the promises of early and advanced reactor technologies as a safe, clean, and low-cost baseload energy. Materials development and qualification in the nuclear industry is by definition challenging due to stringent safety requirements, limited availability of specialized facilities for materials irradiation and testing, and the challenging high-temperature, high-radiation environment. NMDQi will establish tools and capabilities that will greatly accelerate the nuclear fuels and materials development process. These tools will provide both computationally informed insights and high-throughput infrastructure with the goal of completing qualification in a single pass. In this approach, materials must be fabricated with a range of properties of interest so that materials performance can be examined in parallel, rather than with multiple discrete specimens. Advanced manufacturing (AM) techniques, which can produce complex component geometries, microstructures, and compositions, are ideal. The improved process monitoring and control that AM can provide are ideal for ensuring and reducing material variability, which will be particularly important as standards committees pursue regulations for AM components. However, gaining these benefits requires overcoming the substantial barrier of qualifying AM processes and the resulting materials and components for supporting research campaigns and eventually nuclear service.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Mechanical Properties of Aged A709

A709 plate is in the process of being developed and qualified through a collaboration by Argonne National Laboratory (ANL), Idaho National Laboratory (INL), and Oak Ridge National Laboratory (ORNL). The goal is to qualify A709 plate in Section III, Division 5 of the American Society of Mechanical Engineers (ASME) Boiler and Pressure Vessel Code (BPVC). This would permit the construction of A709 plate for fast-reactor structural applications. A tradeoff between creep and creep-fatigue properties was established in prior work. A processing route was identified as providing the optimal balance between creep-rupture and elevated-temperature cyclic properties for the solution annealed condition. This condition, however, resulted in a shorter than desired creep-rupture life. Aging is probed to evaluate its potential at further improving mechanical properties. Aging statically precipitates the solutes in solution prior to service. The processing routes identified as providing the best creep-rupture properties and best balance in mechanical properties are investigated. This report discloses the results from tensile, creep, and elevated-temperature cyclic testing performed at INL on the aged material. The aged properties are compared to solution annealed properties. A709 offers improvement in performance compared to 316H particularly at high temperatures; 316H is a material qualified in Section III, Division 5 of the ASME BPVC. For certain high-temperature fast-reactor design conditions, 316H cannot be used while A709 can.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Developing New Fuels for High Performance Research Reactors

The National Nuclear Security Administration (NNSA) Material Management and Minimization (M3) program works globally to minimize the civilian use of highly enriched uranium (HEU), a weapon-usable nuclear material. Supporting this effort, M3’s Office of Reactor Conversion and Uranium Supply is developing new fuels capable of converting research reactors from HEU fuel to high-assay low-enriched uranium (HALEU) fuel. Some of the remaining research and test reactors (RTRs) operating on HEU today have unique designs, fuel configurations, and demanding performance requirements that cannot be met with an existing regulatory-approved low-enriched uranium (LEU) fuel. M3, DOE’s national laboratories, and other industry partners are qualifying new high-density LEU fuels to convert these RTRs while maintaining their unique capabilities supporting a wide variety of science and technology research in areas such as medicine, industry, defense, education, and training. Current efforts are focused on two options for the remaining US high-performance research reactor conversions: a monolithic uranium 10wt% molybdenum (U-10Mo) fuel form and a dispersion uranium silicide fuel form. This paper reviews the history and status of M3’s fuel qualification efforts for the U-10Mo LEU fuel form.

Montgomery, Rose [ORNL] (ORCID:0000000286038936)↗

DOE OSTI2023

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↗

DOE OSTI2023

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

36 MATERIALS SCIENCE↗

DOE OSTI2020

Progress Report on the Assessment of the Material Performance for TCR Applications

The objective of Argonne’s materials research activities for the Transformational Challenge Reactor (TCR) program is to improve the understanding of material properties from additive manufacturing with the focus on understanding the creep and fatigue properties of additively manufactured materials. The material work conducted by Argonne provides support in developing and qualifying advanced materials and manufacturing processes to allow for innovative reactor design and licensing for the TCR. In this report, we present the creep data at temperatures of 550, 600 and 650°C and stresses between 175 and 300 MPa for 316L stainless steel produced by a laser powder bed fusion process. We conducted five different post-build heat treatments, namely 650°C/1h, 750°C/1h, 800°C/1h, 900°C/1h and 1050°C/1h. Creep tests of the heat-treated specimens were performed under the same test condition, 550°C/275 MPa to evaluate and understand the effect of post-build heat treatment on the creep behavior of additively-manufactured 316L SS. Creep tests were conducted to ASME NQA-1 or its lab equivalent for quality assurance.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2025

A simple centrifuge cell method for ex situ quantification of electrical conductivity of slurry electrode materials

We present the design, experimental procedure, and experimental evaluation of a system for fast, simple, and ex situ characterization of electrical conductivity of slurry electrode materials. The system uses a custom-designed electrochemical cell compatible with centrifugation in a swing-bucket centrifuge. The cell features cylindrical graphite electrodes that are partially sheathed so as to expose only 2 mm of the electrode surface to the bottom region of the packed particulate pellet. Also presented is a conduction model that provides a shape factor for estimating effective conductivity. We tested aqueous solutions of carbon black (CB), activated carbon (AC), and mixtures thereof. These particles were dispersed in 0.0 and 0.5 M NaCl solutions. Measurements show that the effective conductivity initially increases linearly with pellet mass and then saturates at higher masses. Notably, CB exhibited a fivefold increase in conductivity than AC at equal pellet masses. CB/AC mixtures at a fixed pellet mass were tested with CB mass fractions of 0 to 100%. Interestingly, the mixture conductivity was found to be a non-monotonic function of CB mass fraction, with a maximum conductivity at about 60 % CB mass fraction. At this maximum, the mixture conductivity is approximately 30 % higher than pure CB. NaCl concentration in the slurry solution had no effects on conductivity. These results highlight the interactions between slurry electrode composition and compaction, offering insights for optimizing slurry electrodes. Furthermore, the system and results may also be applicable to evaluation of particulate materials (including slurries) used for Li-ion batteries, capacitive deionization, fuel cells, and flow electrodes.

Capacitive deionization↗