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Powder metallurgy hot isostatic pressing (PM-HIP) Microreactor Project presentation for the 2023 Advanced Reactor Technology (ART) program review.
Section III, Division 5 of the American Society of Mechanical Engineers Boiler and Pressure Vessel Code covers construction rules for elevated-temperature nuclear components. Microreactor developers have expressed a need for advanced manufacturing processes to fabricate microreactor components to reduce manufacturing costs. Components fabricated using manufacturing processes other than conventional techniques are not currently qualified in Section III, Division 5. An expeditious approach to qualifying an advanced manufacturing process for alloys whose wrought-product form is already qualified in Division 5 is to demonstrate the resultant properties from the advanced manufacturing process are equivalent or superior to the wrought-product form. Powder metallurgy-hot isostatic pressing (PM-HIP) is a mature technology that offers many advantages that are attractive to the microreactor industry. Preliminary data show that the elevated-temperature creep-fatigue properties of PM-HIP 316H stainless steel (SS) are reduced compared to the Wrought 316H SS, which is qualified in Section III, Division 5. Work is ongoing to identify the mechanisms responsible for the reduced creep-fatigue properties and to establish acceptance criteria to confirm the adequacy of the component for service.
The Advanced Materials and Manufacturing Technologies (AMMT) program operating under the Department of Energy Office of Nuclear Energy is accelerating the qualification and deployment of additively manufactured materials in advanced reactor environments. Laser powder bed fusion (LPBF) has emerged as a promising additive manufacturing technique to fabricate complex components with the potential of tailored material properties. In the nuclear industry, metal additive manufacturing can offer numerous advantages, such as reduced lead times, streamlined quality assurance, and cost-effective low-volume production of new and replacement components with conventional or novel materials and geometries. The rapid and effective qualification of the effect of processing variability on the performance and degradation of additively manufactured materials is essential for the deployment of these components into advanced reactor environments. As part of this effort, AMMT is performing irradiation and corrosion testing of several materials built by LPBF, including 316L and 316H stainless steels. Our efforts encompass neutron irradiation testing, ion irradiation testing, and advanced modeling to provide a robust technical basis for understanding the effect of process variability on materials degradation and developing a sound methodology for accelerated ion irradiation testing. We develop focused irradiation test plans that align well with risk-informed and technologically inclusive approaches to licensing. We will also discuss our plans and specific concerns for corrosion testing additively manufactured material, with a primary focus on molten salt and liquid sodium environments.
The advanced non-light water reactor designs (Gen IV reactors), including molten salt/ very high temperature/ sodium-cooled and lead-cooled fast reactors, typically operate at higher temperatures and more extreme radiation conditions than light water reactors. An intrinsic part of the deployment and progress of Gen IV reactor designs is selecting the most suitable structural material for a specific application. Additive manufacturing (AM), a fairly new process of making physical, three-dimensional objects from a computer design file, is going to completely change the way of design, build and certify nuclear systems. It offers a range of opportunities to produce complex geometries from existing materials, offers new routes for processing of previously difficult to process materials, allows for design of new high-performance materials, and finally facilitates hybridization of dissimilar materials. This emerging technology has successfully produced cars, wind turbine blade molds and even live cells. It could also open up big opportunities for the nuclear industry to quickly deploy technologies at a fraction of the cost. So far, AM techniques have been preliminarily applied in the field of nuclear reactors, including the classical parts such as the pressure vessel of a small reactor with 508-III steel, the bottom nozzle of a fuel assembly with 304L steel, the fuel cladding with zirconium alloy and the integrated impeller of a pump and the multi-channel valve body with 316L steel [6,7]. The AM applications for operating nuclear reactors started in auxiliary plant components and have slowly migrated to metallic reactors and core components, but many of these are not safety critical components. Although many parts used for nuclear reactors have been fabricated by AM techniques, practical applications in engineering are still a long way off due to the uncertainty factors focused on the processing, material properties, analysis methods and application standards, which feeds the safety and life-cycle of the nuclear reactor. Due to rapid, repeated heating and cooling during production, a high dislocation density was present in the AM material. This microstructure feature is unstable at elevated temperature while high temperature is one of the typical operation environments for nuclear reactors. Thus, it is important to understand the thermal effect on the microstructure of AM material. The objectives of this study are to investigate the effect of heat treatment on the microstructure and mechanical properties of 316L stainless steel produced by laser powder bed fusion additive manufacturing, and to determine an appropriate heat treatment practice that will be applied to the lightweight AM lattice-structured material with the same chemistry. The heat treatment study consisted of annealing the samples at a temperature range of 800 to 1200 oC with a 50 oC increment for different times (1-24 hours), followed by vacuum or air cooling. Microstructural characterization was carried out by Scanning Electron Microscope (SEM). Grain size and crystallographic orientation were investigated by Electron Backscatter Diffraction (EBSD). Vickers hardness tests with a 0.5 kg load were employed to determine the hardness of samples after different heat treatments. After heat treatment, the random crystallographic orientation was preserved, and the volume fraction of high-angle grain boundaries (grain boundary misorientation =15 oC) remained the same. The dislocation density decreased with annealing temperature due to recovery. The fine subgrain structures in the as-printed specimen were quite stable up to 1200 oC. Minimal recrystallization was observed up to 1200 oC. Recrystallization initiated only after 8.5 hours at 1200 oC. The SEM images did not show obvious dependence of microstructure on cooling rate. The hardness of the specimens decreased with increasing annealing temperature as a result of the decrease in dislocation density. It is interesting to note that the AM material showed very similar hardness to the wrought material when annealing at similar temperature, although the microstructures are very different. Annealing at 1050 oC for 1 hour followed by air cooling was selected as the heat treatment procedure for the lattice designed lightweight AM 316L material.
The project established a Tight Oil Field Laboratory to address technical challenges in developing stacked unconventional reservoirs in the Powder River Basin. Key activities included data compilation, subsurface mapping, drilling, logging, coring, deployment of fiber optics and microseismic, completion and stimulation optimization, and well performance evaluation.
A. Idaho National Laboratory (INL) is developing a microreactor to produce electrical power utilizing a small nuclear core and Stirling engines under the Microreactor Application Research Validation and Evaluation (MARVEL) program. This procurement specification defines the requirements for procurement of the B4C Powder. B. Any conflict between this specification and referenced Codes and Standards, or any supplementary specifications in the procurement documents requires written clarification from the Contractor prior to proceeding with any work. Any deviation from the procurement documents requires approval by the Contractor with the change request process.
Laser powder bed fusion additive manufacturing (LPBF-AM) of a low-alloy, high-performance AF-9628 steel results in exceptionally high strength and good ductility. The reasons for such mechanical properties are investigated through detailed microscopy performed at several length scales. Thus, the characterization of melt pool, porosity, grain morphology, phases, and dislocations is performed in the as-printed material. The as-printed material consists of only 0.004 vol% of uniformly distributed porosity, single-phase martensitic laths with an average lath size of ≈2.5 μm, the absence of carbides indicating interstitial trapping of C atom, and high dislocation density in the martensitic laths. Experimental data through microscopy are then fed in analytical models for calculating strengthening contributions from various strengthening mechanisms. Calculated yield strength agrees well with experimentally determined value, and therefore, activation of various strengthening mechanisms is established in as-printed AF-9628.
Although a few binder-free and self-supported single-atom electrodes have been reported, achieving mechanically robust, defect-engineered, and reproducible films that preserve atomic dispersion under electrochemical operation remains challenging. This work addresses this limitation by presenting a versatile and generalizable strategy to transform powders into standalone, defect-engineered thin films hosting atomically dispersed Ni centers within conductive 2D frameworks. The physicochemical and electronic properties of these materials are thoroughly characterized using a comprehensive set of spectroscopic and microscopic techniques and confirmed the homogeneous dispersion and monoatomic nature of the Ni centers (0.94 wt.%) on the electrode films. Electrochemical testing via cyclic voltammetry and electrochemical impedance spectroscopy under a range of experimental conditions revealed that integration of Ni single atoms markedly enhanced performance and stability compared to carbon nanotube-only electrodes, maintaining integrity after 15 h of continuous operation. This improvement is accompanied by a notable reduction in charge transfer resistance (30.50 Ω) and an increase in double-layer capacitance (295.45 µF). Post-electrochemical analyses corroborated the structural integrity and robustness of the electrodes. Overall, this work bridges atomically precise catalysis and device-level electrochemistry, opening a route toward reproducible and scalable single-atom electrodes for sensing and energy conversion.
Abstract A Mn(II) salt and A + CN − under anaerobic conditions react to form 2‐D and 3‐D extended structured compounds of A m Mn II n (CN) m+2n stoichiometry. Here, the creation and characterization of this large family of compounds, for example AMn II 3 (CN) 7 , A 2 Mn II 3 (CN) 8 , A 2 Mn II 5 (CN) 12 , A 3 Mn II 5 (CN) 13 , and A 2 Mn II [Mn II (CN) 6 ], where A represents alkali and tetraalkylammonium cations, is reviewed. Cs 2 Mn II [Mn II (CN) 6 ] has the typical Prussian blue face centered cubic unit cell. However, the other alkali salts are monoclinic or rhombohedral. This is in accord with smaller alkali cation radii creating void space that is minimized by increasing the van der Waals stabilization energy by reducing ∠Mn−N≡C, which, strengthens the magnetic coupling and increases the magnetic ordering temperatures. This is attributed to the non‐rigidity of the framework structure due the significant ionic character associated with the high‐spin Mn II sites. For larger tetraalkylammonium cations, the high‐spin Mn sites lack sufficient electrostatic A + ⋅⋅⋅NC stabilization and form unexpected 4‐ and 5‐coordinated Mn sites within a flexible, extended framework around the cation; hence, the size, shape, and charge of the cation dictate the unprecedented stoichio‐metry and unpredictable cation adaptive structures. Antiferromagnetic coupling between adjacent Mn II sites leads to ferrimagnetic ordering, but in some cases antiferromagnetic coupling of ferrimagnetic layers are compensated and synthetic antiferromagnets are observed. The magnetic ordering temperatures for ferrimagnetic A 2 Mn II [Mn II (CN) 6 ] with both octahedral high‐ and low‐spin Mn II sites increase with decreasing ∠Mn−N≡C. The crystal structures for all of the extended structured materials were obtained by powder diffraction.
Cookoff experiments of powdered and pressed TATB-based plastic bonded explosives (PBXs) have been modeled using a pressure-dependent universal cookoff model (UCM) in combination with a micromechanics pressurization (MMP) model described in a companion paper. The MMP model is based on the accumulation of decomposition gases at nucleation sites that load the surrounding TATB crystals and binder. This is the first cookoff model to use an analytical mechanics solution for compressibility and thermal expansion to describe internal pressurization caused by both temperature and decomposition occurring within closed-pore explosives. This approach produces more accurate predictions of ignition time and pressurization within high-density explosives than simple equation-of-state models. The current paper gives details of the reaction chemistry, model parameters, predicted uncertainty, and validation using experiments from multiple laboratories with errors less than 6 %. The UCM/MMP model framework gives more accurate thermal ignition predictions for high density explosives that are initially impermeable to decomposition gases.
Abstract Part quality manufactured by the laser powder bed fusion process is significantly affected by porosity. Existing works of process–property relationships for porosity prediction require many experiments or computationally expensive simulations without considering environmental variations. While efforts that adopt real-time monitoring sensors can only detect porosity after its occurrence rather than predicting it ahead of time. In this study, a novel porosity detection-prediction framework is proposed based on deep learning that predicts porosity in the next layer based on thermal signatures of the previous layers. The proposed framework is validated in terms of its ability to accurately predict lack of fusion porosity using computerized tomography (CT) scans, which achieves a F1-score of 0.75. The framework presented in this work can be effectively applied to quality control in additive manufacturing. As a function of the predicted porosity positions, laser process parameters in the next layer can be adjusted to avoid more part porosity in the future or the existing porosity could be filled. If the predicted part porosity is not acceptable regardless of laser parameters, the building process can be stopped to minimize the loss.
Austenite reversion and intermetallic precipitation are two key phase transformations in maraging steels which determine the strength and ductility. Usually, an optimum aging temperature/time is determined using trial and error approach with inputs from thermodynamic databases and a-posteriori microscopy/hardness evaluations. In this study, a thermo-kinetic model is developed to predict the precipitation and austenite reversion kinetics during various post-fabrication heat treatments in a Ti-free variant of grade 300 maraging steel manufactured using laser powder bed fusion. The thermo-kinetic model was based on the principles of Scheil solidification and the classical nucleation theory. The predictions from the thermo-kinetic model were verified using suitable microscopy techniques, and the results from the thermo-kinetic model agree well with the experimental measurements. Overall, results highlight the fact that an Integrated Computational Materials Engineering approach can be used to predict the precipitation and austenite reversion kinetics, and be used as an input for an efficient design of heat treatments for achieving optimum mechanical properties.
Here, the cracking behavior of a high γ' volume fraction CoNi-base superalloy fabricated via laser powder bed fusion (LPBF) is studied in relation to the content of carbon and boron. Severe cracking occurred with the increase in boron content from 0.08 to 0.16 at. pct (0.015 to 0.029 wt pct), while compositions with 0.1 to 0.36 at. pct C (0.02 to 0.076 wt pct) and 0.08 at. pct B exhibited minimal cracking. Assessment of cracks in the high-boron composition shows a variation in crack density with printing parameters, and alignment of the cracks with the build direction. Scanning electron microscopy (SEM) of the crack surfaces shows evidence of a solidification cracking mode. Differential thermal analysis (DTA) reveals a decreased incipient melting temperature for the high-boron composition, and atom probe tomography (APT) is used to measure the enrichment at grain boundaries, revealing distinct boron segregation. Scheil-Gulliver solidification simulations for the different C and B levels are consistent with the incipient melting behavior observed with DTA. Evaluation of the solidification cracking susceptibility from the simulations allow for comparison of the CoNi alloy behavior to Ni-base superalloys studied for LPBF fabrication and displays how such metrics may aid in the design of new precipitation-strengthened superalloys for additive manufacturing (AM).
The simulation and modeling of part-level distortion and residual stress in diverse metal additive manufacturing (AM) geometries has great potential to enable the rapid adoption of this technology in engineering design. Moreover, the use of additive manufacturing component libraries (CLs) offer a computationally efficient means of quantifying these part-level defects resultant from AM processing. We report on how the individual simulations of simple shapes, potential entries in a CL, can be superimposed to provide an indication of distortion and residual stresses in complex geometries. Laser powder bed fusion AM was used to construct test geometries of varied shapes and their combinations in the form of CLs in an effort to characterize location-dependent and feature-dependent distortion distributions. Blue light scanning was used to experimentally measure 3D distortions in order to investigate the interaction between the component shapes and local boundary conditions. Overall, part-level distortions were highly dependent on test component geometry, local boundary conditions, and shape combination. Commercial finite element software was used to verify experimental trends and to make predictions of distortion. The use of CLs resulted in over 20 times savings in computational cost while reproducing overall trends in distortion for test geometry assemblies. Therefore, it is anticipated that the use of CLs for L-PBF AM geometries has demonstrated potential to facilitate efficient simulations of full component AM assemblies, thereby reducing the need for costly trial-and-error-type experimental analysis.
The utilization of additive manufacturing (AM) techniques for refractory materials in high-temperature environments has significantly expanded because of the ability to fabricate geometrically complex components. Electron beam powder bed fusion (EB-PBF), which provides lower residual stress, a cleaner vacuum environment, and better efficiency for high melting point, is one of the best-suited AM methods to produce advanced refractory components. However, the property variation attributed to the heterogeneous microstructure and process-induced defects has hindered the widespread adoption of EB-PBF-produced material like tungsten. While numerous in-situ monitoring and defect detection methods have been demonstrated for EB-PBF, a workflow that compares and evaluates process-induced abnormalities from different imaging perspectives is still limited. This study examines a feature-embedded tungsten component manufactured via the EB-PBF process to demonstrate the defect detection capabilities of a multimodal defect imaging workflow. The predefined and process-induced defects are evaluated by harnessing various imaging techniques, including in-situ electron imaging, layerwise near-infrared (NIR) imaging, post-build high-energy x-ray computed tomography (CT), and conventional destructive metallography. The results highlight the strengths and limitations of distinctive defect imaging techniques concerning specific defect types, sizes, and conditions. It was found that electron imaging can provide more abnormal detection capabilities while maintaining a higher measuring accuracy, against the conventional metallography in this case study, compared with NIR and CT imaging techniques.
Laser shock peening is a mechanical surface treatment which can induce large compressive residual stresses and microstructural changes in the material by using repetitive shocks from laser pulses. In this work, the surface integrity (surface microstructure, topography, hardness and residual stress) of a laser shock peening treated powder metallurgy Ni-based superalloy was investigated. Laser shock peening treatment introduces large plastic deformation especially at a depth of about 100 μm from the surface, which increases the local hardness. The residual stress from the surface to the interior of the sample was investigated by synchrotron X-ray diffraction. The maximum compressive stress reaches 400 MPa at the surface, while the depth of the compressive stress is about 0.7 mm. Lastly, the oxidation behavior of the treated and untreated samples was evaluated by thermal exposure at 700°C for 312 h. The LSP treatment decreased the thickness of oxide layer, thereby showing improved oxidation resistance.
The near-net fabrication capabilities of laser powder-bed fusion (LPBF) offer the potential to manufacture tools with complex cooling channels that can improve the production efficiency of the tools with reduced greenhouse gas emissions. High strength, toughness, and wear resistance are some of the key properties required by the tooling industries to qualify tools. While strength can be increased through appropriate heat treatments, the increase in strength comes with an associated ductility loss. Here, we show that the non-equilibrium conditions inherent to LPBF can suppress the transformation-induced plasticity effect to room temperature in a Ti-free version of grade 300 maraging steel (G300MS), which is commonly not observed at room temperature in G300MS manufactured using conventional methods. The presence of retained austenite along with Ni-rich regions was found to increase the kinetics for austenite reversion during aging, thereby enabling the transformation of austenite into ε martensite during tensile deformation at room temperature, in turn increasing the strength with minimal ductility loss.
Here, the isothermal and cyclic oxidation behavior of Haynes 282 (H282) processed by laser powder bed fusion and electron beam melting was compared to its cast counterpart during exposures in air at 800 and 950°C. The specific microstructure of the AM alloys compared to coarse-grain cast 282 resulted in differences in oxidation rates, internal oxidation and spallation behavior. At 800°C, faster Ti diffusion to the surface due to the smaller grain size of the AM alloys led to Ti doping of the Cr 2 O 3 scale and faster oxidation rates. The higher density of grain boundaries also resulted in more pronounced internal oxidation. At 950°C, a duplex Cr 2 O 3 scale was observed with a dense inner layer and porous cracked outer layer with embedded TiO 2 particles. The impact of the external and internal oxide compositions and oxidation-induced elemental depletions on the oxidation lifetime, creep properties and spallation behavior is discussed.