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Analysis of Deformation and Fracture Mechanisms in the Harvested High-Dose Baffle-Former Bolt with Stress-Corrosion Cracks Formed While in Service

This report presents the results of advanced mechanical testing conducted on miniature tensile specimens excised from an irradiated baffle-former bolt, a commercial pressurized water reactor component. The specimens were extracted from the midsection of the bolt shank, where the estimated damage dose reached 23 displacements per atom. The mechanical testing included the following tests: (1) conventional tensile testing at room temperature, augmented by digital image correlation (DIC) to enable noncontact strain measurements, and (2) in situ tensile testing within a scanning electron microscopy (SEM) instrument equipped with energy-dispersive x-ray spectroscopy (EDS) and electron backscatter diffraction (EBSD) detectors to evaluate active deformation and fracture mechanisms. Additionally, SEM fractographic analysis revealed alterations in the fracture mechanism from a predominantly ductile fracture in nonirradiated steel to a mixed fracture mode (still dominating ductile and minor cleavage spots) in irradiated specimens derived from the baffle bolts. The findings indicate a complex strain localization behavior for in-service irradiated steel specimens. Beyond conventional necking at the macro scale and defect-free channel formation at the micro scale, DIC results identified the presence of deformation bands approximately 100 μm in width. These bands consist of chains of grains exhibiting elevated local strain levels and may be considered an intermediate or mesoscale level of strain localization. These bands become discernible near the yield stress as localized hot spots, areas of elevated strain, persisting throughout most of the experiment. The formation of mesoscale deformation bands as a strain localization mechanism may exacerbate the defect-free channel formation in irradiated materials, further promoting irradiation-assisted stress corrosion crack initiation.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

FAST Irradiations, Postirradiation Examinations, and Modeling of U-Mo for Light Water Reactor Applications

Many next generation light water reactor (LWR) concepts, such as mobile small modular reactors, are seeking to use smaller core dimensions than conventional reactor types. Smaller reactor cores require an increase in fissile material to maintain reactivity. For non-proliferation purposes, enrichment increases are limited to less than 20% (high assay low enriched uranium, [HALEU]) and so higher uranium density fuels than UO 2 must be considered. To this end, uranium-molybdenum alloys were tested using the Fission Accelerated Steady-state Test (FAST) approach. The experiment test matrix is focused on identifying the temperature transition between low swelling and high fission gas retention to break away swelling and low fission gas retention. This paper documents the results of irradiation tests and post-irradiation examinations (PIE) including neutron radiography, rodlet profilometry, fission gas collection analysis, and optical metallography. The results of these tests showed that unconstrained U-Mo fuels (solid, Na-bonded rodlets) have a swelling threshold between 400-450°C with minimal fission gas release below this point. Higher temperature solid fuel showed microstructural zoning with small pore networks while lower temperature solid fuels have a uniform microstructure with large pore networks. U-Annular Mo fuels where swelling had some self-constraint imposed upon it, were shown to have much reduced swelling compared to their solid counterparts as well as very low fission gas release for irradiation temperatures up to 500°C. These initial results show that the use of U-Mo in constrained fuel geometries could be used as a high uranium density HALEU fuel for LWRs.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Demonstration of Scaled-Production of Rare Earth Oxides and Critical Materials from U. S. Coal-Based Sources (Final Report)

The project objective was to demonstrate scaled production of high purity rare earth oxides (REO), nominally exceeding 90% grade, from coal refuse sources using innovative technologies that reduce cost and improve environmental outcomes relative to traditional rare earth processing technologies. The project utilized a critical material pilot plant constructed and tested as part of a previous U.S. Department of Energy project. Target performance criteria was a 50% reduction in production cost based on previous optimum values, 150% increase in recovery and greater than 2% concentrates of rare earth oxides, cobalt and manganese. Concentrate production goals were to produce a rare earth mix oxide product at a rate of 200 grams per day having a minimum purity of 50% as well as products of cobalt and manganese having a minimum purity of 2%. A previous pilot plant investigation identified acid cost as the major contributor to an operating cost that made the recovery of rare earth and other critical metals from bituminous coal sources economically challenging. As such, acid cost reduction was a major target using bio-oxidation reactors to produce sulfuric acid from naturally occurring coal pyrite. Based on laboratory data, a bio-oxidation circuit was designed for the pilot plant to produce 7.5 l/min of acid using two 11-m3 (3000 gallon) reactors equipped with 40 hp aerators for air dispersion. The pilot-scale tests revealed that acid concentration equivalent to as high as 1.0 M sulfuric acid could be continuously produced. However, the bio-acid contained exceptionally high iron concentrations, which complicated downstream processing of the pregnant leach solution (PLS). A TEA of the bio-oxidation circuit showed that production cost was approximately $0.13 per kg acid equivalent if produced using a four-day retention time in the reactors. This value represents a 48% reduction from that of purchased bulk sulfuric acid. Calcination (or roasting) studies were conducted on coarse refuse from West Kentucky No. 13 and Fire Clay coal seam sources. The test results revealed the potential to increase recovery by nearly 100% using temperatures between 500°C to 700°C with light REE recovery value being the most improved. Acid baking of the calcined products using sulfuric acid at 250°C increased heavy rare earth recovery from around 40% to 80% while decreasing the acid requirements by over 50%. The existing pilot plant was upgraded for the pilot scale demonstration of REE and CM recovery. The primary feedstocks were West Kentucky No.13 and heap leach pregnant leach solution (PLS) while a secondary feedstock was a lignite waste material from a construction sand operation. The pilot scale operation started with PLS generation through leaching followed by iron and aluminum removal, nominally at 3.3 and 4.5 pH, respectively. Leaching lixiviants used for the test were industrial grade sulfuric acid or bio-acid generated at the pilot scale facility. For most of the tests, the solid feed rate was 200 lb/hr whereas lixiviant was added at 2 gpm to provide an optimal residence time of 45 minutes. Following the contaminant removal step, several different process schematics were tested with the goal of maximizing REE recovery and purity. In the first test, direct processing of aluminum precipitation raffinate for REE recovery using oxalic acid at pH 1.5 was investigated. Overall REE recovery was approximately 45%. Unfortunately, elevated calcium content in the PLS significantly impacted the RE-Oxide product grade. Similarly, high calcium content decreased both the product purity and grades of CM products. As such, a new flowsheet was tested with the same initial process schematic but different precipitation stages for REEs and CMs at pH 6.0 and 9.0, respectively. It was noted that the overlapping precipitation behavior of Co, Ni and Zn with REEs limited the applicability of this process schematic. While this change increased the RE-Oxide grade from 36% in the first test to 87%, the loss of critical metals to the REE cake and bypass of the REEs to the CM cake significantly impacted the recovery of both REEs and CMs. Therefore, the modified process flowsheet combined oxalic acid precipitation stage raffinate and redissolved CM cake filtrate to maximize both the recovery and purity of the products. Consequently, a RE-Oxide product with 85% purity and CM cakes with over 19% Co, 38% Ni, 14% Zn and 9% Mn content were generated with significantly higher recoveries. While the modified process flowsheet improved recoveries and grades, elemental losses observed in separate precipitation and redissolution losses inspired the adaptation of a single precipitation stage at pH 9.0 for both REEs and CMs. This change was anticipated to maximize the REE recovery while minimizing the costs associated with separated redissolution and processing stages. As expected, REE recovery in this new circuit arrangement was over 56% with a product grade of over 87% RE-Oxide content. Similarly, Co, Ni, Mn, and Zn recoveries of 54%, 40%, 67%, and 66%, respectively, were achieved. Unfortunately, the elevated calcium content present in the solution due to its precipitation at pH 9.0 caused a decrease in the CM cake quality. Therefore, the final process flowsheet involved the addition of calcium oxalate precipitation following the oxalic acid precipitation stage, which effectively eliminated calcium contamination of the CM products. Finally, the pilot scale experiments conducted using bio-acid achieved comparable REE leaching recoveries to the conventional sulfuric acid leaching. Elevated iron concentration in the solution caused the co-precipitation of REEs with the iron and aluminum cake, resulting in the REE losses. Furthermore, elevated iron content bypassing the iron and aluminum precipitation stages contaminated the metal sulfide and manganese cake, respectively. A techno-economic analysis was performed based on a commercial facility capable of treating 500 tph of coal-based material. The production cost for West Kentucky No. 13 coarse refuse material ranged from approximately $500-$700/kg of total rare earth oxide whereas the lignite source had significantly lower production cost of $100-$300/kg. The significant difference in cost was due to the easier leaching characteristics of the lignite material and the higher feed concentrations. All process scenarios resulted in a negative net present value (NPV). For the lignite feedstock, laboratory REE leach recovery values were about 30% higher than the pilot plant data. Using the lab leach results, a positive net present value was achieved and the production cost decreased from $100-$300 $/kg to less than $150/kg of total REO.

01 COAL, LIGNITE, AND PEAT↗

Analysis of attenuation data from the decommissioned ZIon unit 1 reactor pressure vessel beltline weld

In order to examine the attenuation of radiation damage through the thickness of an irradiated reactor pressure vessel (RPV), four segments were acquired from the Zion Unit 1 power plant RPV after the plant was decommissioned. The Zion Unit 1 RPV Beltline Weld Segment 1 was cut into seven blocks, consisting of five base metal and two beltline welds from the high fluence region of the segment. Through-wall test specimens were machined and tested. Specimens included those used for Charpy impact, Master Curve fracture toughness testing, and chemical analysis. The observed through-thickness ductile-to-brittle transition temperatures in the beltline weld deviated significantly from the expected behavior based on the attenuation of fast fluence as a function of depth into the RPV. Beginning at the inside surface, the 41-J Charpy transition temperature was either flat or slightly increasing until the ¾ -T location. The results of a simple, model-based analysis of the Zion beltline weld material that included the irradiation conditions and material chemistry were generally consistent with industry trend curves and the standard attenuation model, rather than the observed data. Although there was no archive material from the RPV available to permit measurement of the unirradiated properties, fracture toughness specimens fabricated from archive surveillance weld were used to obtain an estimate of the initial through-thickness values of the Charpy transition temperature. The Charpy shifts obtained using this approach were similarly in disagreement with the predictions of the US NRC Regulatory Guide 1.99, Rev. 2. However, testing of irradiated Charpy specimens taken from the RPV following post-irradiation annealing (10 hr. at 500 °C) provided a quite different estimate of the unirradiated properties which improved the agreement between the inferred through-thickness Charpy shifts and exponential attenuation model included in Regulatory Guide 1.99/2. In conclusion, the analysis of the Zion data and data obtained in previous post-mortem examinations of decommissioned RPVs indicates that more work is needed to understand the through-thickness properties of RPV materials in order to properly assess through-wall damage attenuation.

Charpy impact↗

Application of FARM to an IES scenario within the FORCE ecosystem

The FARM (Feasible Actuator Range Modifier) software module is a component of the RAVEN-based FORCE framework for analysis of Integrated Energy Systems (IES). FARM supports the HERON software module in the evaluation of the optimal dispatch by evaluating feasible set-points for the different IES unit components. Set-points are required to satisfy limits on both production variables (i.e., the variables to be optimized such as the electrical power, the hydrogen production rate, etc.) and process variables tied to the service life of equipment (e.g., steam flowrate, vessel pressure, turbine firing temperature, etc.). This problem is addressed by adopting a two-stage approach. First, the HERON power dispatcher determines set-points that meet the constraints on the former variables (e.g., power levels and power ramp rate limits). These constraints are called explicit constraints. Then, FARM adjusts these set-points to ensure the respect of the limits on the latter variables given the knowledge of the system physics acquired through machine learning algorithms. These constraints are called implicit constraints. From this standpoint, FARM constitutes a bridge between the HERON power dispatcher that adopts a simplified description of the IES unit (low-resolution physics) and the HYBRID high-fidelity models (high-resolution physics). The original version of the FARM software module (FARM-Alpha) was released by Argonne National Laboratory in January 2021. In the latest version of the code released in July 2022 (FARM-Delta), the Reference Governor (RG) algorithm was upgraded to a Multi-Input Multi-Output version from its original Single-Input Single-Output form. The RG algorithm acts to enforce constraints. With this improvement an IES unit is now treated as a single dynamic system from the standpoint of control. The crosstalk among components in an IES unit is now fully considered thereby ensuring a true optimization is obtained for those units that have multiple set-points. In this report, the capabilities of FARM-Delta operating within the FORCE ecosystem are demonstrated for an IES test case. The specific configuration of IES unit for this case was selected by the IES team with consultation from the Advanced Reactor IES Expert Group. A full TEA analysis that invoked HERON, HYBRID, FARM, and RAVEN was performed and serves to demonstrate how the latest modification to FARM algorithms (i.e., state variable selection, state-space matrices derivation, set-point verification) can shape setpoints that might otherwise compromise the health of equipment through accelerated wear and tear. In this specific test case, it was demonstrated that these algorithms ensure a more efficient utilization of steam resources to be shared by two different subsystems, namely Balance of Plant (BOP) and High-Temperature Steam Electrolysis (HTSE). Finally, some code improvements that can further enhance the user-friendliness are suggested.

97 MATHEMATICS AND COMPUTING↗

Simplified inelastic constitutive models for ASME Section III, Division 5 design by inelastic analysis

This report describes the development of simplified, universal constitutive model that captures the high temperature monotonic and cyclic behavior of a range of commonly-used high temperature materials. The goal of the work is to provide a simple, universal constitutive model to replace the current bespoke models for Grade 91, 316H, and Alloy 617 included in Nonmandatory Appendix HBB-Z of the ASME Boiler & Pressure Vessel Code, and to extend this model to cover Alloy 800H. We initiated this work in response to feedback from reactor vendors and other Code users requesting simplified models, compared to the current models, that are easier to implement and use in commercial finite element analysis software. This report describes the completion of this effort by developing a model to correct the defects in standard model forms presently used for high temperature material modeling, described in past work, developing and implementing new numerical methods to train this model against test data, and then actually training the model for the four materials. The report provides a complete mathematical description of the model along with the tabulated material coefficients for the four materials. The final step will be to formulate an ASME Code change to introduce the new models into the Code.

36 MATERIALS SCIENCE↗

Microstructure of Neutron-Irradiated Al 3 Hf-Al Thermal Neutron Absorber Materials

A thermal neutron-absorbing metal matrix composite (MMC) comprised of Al 3 Hf particles in an aluminum matrix was developed to filter out thermal neutrons and create a fast flux environment for material testing in a mixed-spectrum nuclear reactor. Intermetallic Al 3 Hf particles capture thermal neutrons and are embedded in a highly conductive aluminum matrix that provides conductive cooling of the heat generated due to thermal neutron capture by the hafnium. These Al 3 Hf-Al MMCs were fabricated using powder metallurgy via hot pressing. The specimens were neutron-irradiated to between 1.12 and 5.38 dpa and temperatures ranging from 286 °C to 400 °C. The post-irradiation examination included microstructure characterization using transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy. This study reports the microstructural observations of four irradiated samples and one unirradiated control sample. All the samples showed the presence of oxide at the particle–matrix interface. The irradiated specimens revealed needle-like structures that extended from the surface of the Al 3 Hf particles into the Al matrix. An automated segmentation tool was implemented based on a YOLO11 computer vision-based approach to identify dislocation lines and loops in TEM images of the irradiated Al-Al 3 Hf MMCs. This work provides insight into the microstructural stability of Al 3 Hf-Al MMCs under irradiation, supporting their consideration as a novel neutron absorber that enables advanced spectral tailoring.

36 MATERIALS SCIENCE↗

Fabrication and Testing of Solid-Solution Strengthened Corrosion Resistant Alloys For Service in Molten Fluoride Environments

The demand for higher system thermal efficiencies requires the operation of power generation cycles and heat conversion systems at progressively higher temperatures. As the system operating temperature increases, existing materials may not provide adequate mechanical properties or environmental compatibility or both. There is an increasing commercial interest in the development and deployment of liquid-fueled Molten Salt Reactors (MSRs). Hastelloy®N, the highest performing candidate MSR structural alloy, is not capable of operations at temperatures above 700°C, thus limiting the performance of these systems. Using an Integrated Computational Materials Engineering (ICME)-approach and small laboratory scale heats, ORNL developed a class of patented alloys covered by U.S. Patent 9, 435, 011 B2, “Creep-resistant, Cobalt-free alloys for high temperature, liquid-salt heat exchanger systems,” similar to Hastelloy®N in that they are primarily solid solution strengthened. In contrast to precipitation strengthened alloys, the microstructure of solid solution alloys and hence the high temperature mechanical properties are stable for extended periods of time allowing long reactor operating life. The new alloys have shown to possess good resistance to liquid fluorides at temperatures up to 850°C and have significantly improved creep properties when compared to Hastelloy®N. The purpose of the CRADA project was for ORNL to collaborate with Haynes International- a materials producer, MetalTek International- a foundry, and Kairos Power – an advanced reactor developer – to scale-up selected alloys, evaluate their properties, and identify one solid solution strengthened alloy that can meet the property requirements for the reactor being developed by Kairos Power and other similar liquid fluoride-salt cooled reactors. As part of the project, eight alloys were down-selected and fabricated in larger industrial scale heats by Haynes International. Resistance to molten salt was evaluated in flowing FLiNaK and FLiBe by Kairos Power using their Rotating Cage Loop (RCL) system. Accounting for iron deposition during these tests, the new alloys displayed very low net mass change showing excellent corrosion performance in molten salt. Creep properties evaluated at ORNL were found to be better than that of Hastelloy®N and 316 stainless steel. Long-term stabilities of the alloys evaluated by Haynes International showed that these alloys have excellent thermal stability in the temperature range 704.4-815.6°C, with the change in strength and ductility being less than 10-15% after a 4000-hour exposure at 815.6°C. Autogenously Gas Tungsten Arc Welding (GTAW) welded samples showed less than 10% change in yield strength / ultimate tensile strength / total elongation compared to the basemetal, indicating that the alloys have excellent weldability. Three parts were successfully investment-cast using one alloy with very little voiding showing feasibility of fabricating parts using the casting process. This project enabled extensive interaction between the material producer Haynes International, casting supplier MetalTek, and reactor developer Kairos Power. This facilitated testing of materials and components produced using the newly developed alloys by the end-user. This allowed the generation of critical dataset required for down-selection of a few promising alloys for further development. This data is also currently being shared with other reactor designers for them to evaluate the suitability of this alloy for their reactor design. The availability of this alloy will ultimately enable the design and development and deployment of MSRs with increased temperature of operation and thus, improved efficiencies.

99 GENERAL AND MISCELLANEOUS↗

Fabrication and Testing of Solid-Solution Strengthened Corrosion Resistant Alloys For Service in Molten Fluoride Environments

The demand for higher system thermal efficiencies requires the operation of power generation cycles and heat conversion systems at progressively higher temperatures. As the system operating temperature increases, existing materials may not provide adequate mechanical properties or environmental compatibility or both. There is an increasing commercial interest in the development and deployment of liquid-fueled Molten Salt Reactors (MSRs). Hastelloy®N, the highest performing candidate MSR structural alloy, is not capable of operations at temperatures above 700°C, thus limiting the performance of these systems. Using an Integrated Computational Materials Engineering (ICME)-approach and small laboratory scale heats, ORNL developed a class of patented alloys covered by U.S. Patent 9,435,011 B2, “Creep-resistant, Cobalt-free alloys for high temperature, liquid-salt heat exchanger systems,” similar to Hastelloy®N in that they are primarily solid solution strengthened. In contrast to precipitation strengthened alloys, the microstructure of solid solution alloys and hence the high temperature mechanical properties are stable for extended periods of time allowing long reactor operating life. The new alloys have shown to possess good resistance to liquid fluorides at temperatures up to 850°C and have significantly improved creep properties when compared to Hastelloy®N. The purpose of the CRADA project was for ORNL to collaborate with Haynes International- a materials producer, MetalTek International- a foundry, and Kairos Power – an advanced reactor developer – to scale-up selected alloys, evaluate their properties, and identify one solid solution strengthened alloy that can meet the property requirements for the reactor being developed by Kairos Power and other similar liquid fluoride-salt cooled reactors. As part of the project, eight alloys were down-selected and fabricated in larger industrial scale heats by Haynes International. Resistance to molten salt was evaluated in flowing FLiNaK and FLiBe by Kairos Power using their Rotating Cage Loop (RCL) system. Accounting for iron deposition during these tests, the new alloys displayed very low net mass change showing excellent corrosion performance in molten salt. Creep properties evaluated at ORNL were found to be better than that of Hastelloy®N and 316 stainless steel. Long-term stabilities of the alloys evaluated by Haynes International showed that these alloys have excellent thermal stability in the temperature range 704.4-815.6°C, with the change in strength and ductility being less than 10-15% after a 4000-hour exposure at 815.6°C. Autogenously Gas Tungsten Arc Welding (GTAW) welded samples showed less than 10% change in yield strength / ultimate tensile strength / total elongation compared to the basemetal, indicating that the alloys have excellent weldability. Three parts were successfully investment-cast using one alloy with very little voiding showing feasibility of fabricating parts using the casting process. This project enabled extensive interaction between the material producer Haynes International, casting supplier MetalTek, and reactor developer Kairos Power. This facilitated testing of materials and components produced using the newly developed alloys by the end-user. This allowed the generation of critical dataset required for down-selection of a few promising alloys for further development. This data is also currently being shared with other reactor designers for them to evaluate the suitability of this alloy for their reactor design. The availability of this alloy will ultimately enable the design and development and deployment of MSRs with increased temperature of operation and thus, improved efficiencies.

36 MATERIALS SCIENCE↗

Radically Engineered Modular Air Separation System with Tailored Oxygen Sorbents

The commercial energy sector relies heavily on fossil fuel conversion, and in the process releases a significant amount of CO 2 . A promising technology to utilize fossil fuels with relatively affordable CO 2 capture is gasification. However, it requires a pure oxygen stream. The current state of the art method to produce oxygen is cryogenic air separation, which supercools air to a liquid, and then using distillation columns to separate the components. While this method has been thoroughly studied, it only has a 25% efficiency from a second law standpoint and therefore requires a significant amount of energy (and associated emissions) for oxygen production. This, then, lowers the incentive for carbon capture within a plant, so alternative methods need to be investigated. One potential method, chemical looping air separation (CLAS), is a promising method to replace state of the art oxygen generation technologies. CLAS utilizes a cyclic redox scheme with an oxygen sorbent to create pure oxygen streams. This approach typically utilizes a dual reactor scheme where the oxygen deficient sorbent enters the first reactor and is subjected to high oxygen partial pressures to re-oxidize the sorbent. Then the sorbent is sent to the reducing reactor, where it is subjected to low oxygen partial pressure (steam or vacuum) to releases oxygen. The overarching objective of this project was to discover the principles for rational design and optimization of oxygen sorbents and process design to ensure the process is a viable replacement for cryogenic air separation, especially in the context of modular gasification systems. This was done through development, characterization, testing, and analyses of (a) high temperature mixed composite oxides; (b) low temperature doped perovskite oxides (A1 x A2 1-x B1 y B2 1-y O 3 ); (c) scale up synthesis and testing of the optimized sorbent particles; (d) process design and analyses of the CLAS system in the context of modular gasification applications.

01 COAL, LIGNITE, AND PEAT↗

Critical heat flux on zircaloy and accident tolerant fuel cladding under prototypical conditions of pressurized and boiling water reactors

First of a kind high spatial and temporal resolution temperature measurements of Pressurized Water Reactor and Boiling Water Reactor simulated fuel pins (high heat flux cosine profile heaters) in annular rod type geometry during nucleate boiling, departure from nucleate boiling and re-wetting has been performed. Distributed fiber optic measurements of the cladding axial temperature with spatial resolutions down to 2.5 mm axially at up to three equally spaced azimuthal locations per rod have demonstrated the similarities and differences of the different accident tolerant fuel cladding materials. These experiments show the performance of accident tolerant cladding with a precise measurement of the location and evolution of dryout followed by the re-wetting phenomena (see supplementary time history of a critical heat flux event). Experimental parameters varied coolant mass fluxes from 1695 to 2712 kg/m 2 s, pressures from 10 to 20 MPa, and inlet subcooling from 10 to 55 °C. It was found that the coatings and different material have little effect on the value of the critical heat flux. Any discrepancies between the local critical heat flux verified among the cladding material are attributed to different departure from nucleate boiling phenomena captured during the experiment with the high-resolution optical fiber temperature data. Substantial differences in the performance of the different cladding material to survive a critical heat flux event were however observed by post-test X-ray and optical inspection. External evident damage and internal cracks to the simulated fuel pin having the bare zircaloy cladding were observed in regions associated with the occurrence of the critical heat flux for longer periods. Such damages were associated with zirconium oxidation, and not noticed on the Cr coated zircaloy or FeCrAl claddings. These results indicate that the use of FeCrAl or a Cr coated zircaloy as cladding in Pressurized Water Reactor and Boiling Water Reactor may increase the survivability of the cladding material for short transients.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

Preliminary Feasibility of Printing, Microstructure Analysis and Mechanical Performance of a Down Selected Ni Alloy

This report is submitted as completion of a Milestone 3 deliverable under work package ORNL CT-23OR1304051 in support of the Advanced Materials and Manufacturing Technologies (AMMT) program. The AMMT program is aiming at the faster incorporation of new materials and manufacturing technologies into complex nuclear-related systems. An integrated approach, combining advanced characterization, high-throughput and accelerated testing, modeling and simulation including machine learning and artificial intelligence will be employed. While 316H (Fe-16-18Cr-10-14Ni-2-3Mo-0.04-0.1C) has been identified as a key alloy to be integrated into the AMMT accelerated alloy qualification approach due its relevance for many current and future nuclear energy reactors, many other alloys could be considered for the advanced fabrication of innovate high-performance nuclear components. ANL, INL, ORNL and PNNL are collaborating on identifying the most promising alloy candidates relevant for the AMMT program. A selection criteria matrix was established to evaluate the alloys considering their relative importance and technological readiness levels for nuclear energy applications, with a focus on laser powder bed fusion (LPBF). Due to the broad range of potential candidate alloys, ORNL and INL focused on Ni-based alloys, while ANL and PNNL mainly evaluated Fe-based alloys. PNNL previously published materials scorecards reports on several key alloys and this report is providing a broader overview of Ni-based candidate alloys, expending beyond alloys well-known to the nuclear community. Of particular interest are alloys that are currently commercially available in powder form due to the growing demand from other industries that have invested heavily in additive manufacturing. Among these alloys, Haynes 282 (Fe-20Cr-20Co-8Mo) was selected due to its superior strength at high temperature compared to the code-qualified alloy 617 (Ni-20-24Cr-10-15Co-8-10Mo). To assess the integration of this new alloy into the AMMT digital manufacturing framework, we performed the rapid optimization of alloy 282 printing parameters on a Renishaw 250 machine, the fabrication of sufficient materials for extensive characterization and mechanical testing both at ORNL and INL, and added the printing data into the digital platform via the Peregrine software. A detailed analysis of the LPBF 718 alloy was also conducted, with creep specimens being tested at 600-650°C and characterized by advanced electron microscopy. The alloy superior mechanical strength and great printability associated with the extensive database that has already been generated highlight the promising potential of LPBF 718 as a candidate alloy for the AMMT program. INL, ANL and PNNL have generated similar reports and all the information will be compiled into a final M2 milestone report to provide the AMMT leadership team with clear recommendations on the down selection of reactor materials, as well as establish a roadmap for the qualification of these selected alloys.

36 MATERIALS SCIENCE↗

Burst and oxidation behavior of Cr-coated Zirlo during simulated LOCA testing

We report Cr-coated Zr-alloys are a near-term cladding concept to improve reactor safety during accident scenarios. Burst and steam oxidation behavior of bare and Cr-coated Zirlo claddings were examined under simulated loss-of-coolant accident conditions. The 4.4 µm coating had no substantial effect on ballooning or opening geometry but did increase burst temperatures at higher pressures. The coating reduced steam oxidation of the cladding compared to bare specimens, but in regions of high strain, the coating developed through-cracks allowing rapid underlying zirconia formation.

36 MATERIALS SCIENCE↗

Report on Initial Tribological Studies of Graphite in Dry Argon and Molten Salt Environment

This report documents completion of the Advanced Reactor Technologies (ART) Level 2 Milestone M2TG-24OR0501081: “Complete report on initial tribological studies within molten salt environment”, due January 31, 2024. This milestone is a carryover milestone from FY23 M2TG-23OR0501091. The report summarizes the initial studies on tribological characterization of the graphite–graphite sliding interface in a dry argon and molten FLiNaK salt environment. The experiments were conducted on a high-temperature multifunctional tribometer placed in a glovebox. This configuration enables probing the wear and friction properties at high temperatures in an inert environment. The worn surfaces were analyzed using high-resolution microscopy and white-light profilometry to determine the wear modes and wear rates. This report discusses the previous wear and friction studies on 316H stainless steel (SS) sliding against graphite in molten salt for different temperatures, sliding speeds, and salt amount. Moreover, key tribological parameters of pebble-on-pebble interaction in gas-cooled and molten salt reactors (MSRs) are analyzed and used to design an experimental test matrix for future studies. The outcomes of this project could provide key information about the tribological behavior of graphite pebbles in gas-cooled and MSRs, thereby contributing to safer operation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Development of Accelerated High Temperature Mechanical Testing Techniques

The Advanced Materials and Manufacturing Technologies (AMMT) Program focuses on advancing materials and manufacturing techniques for nuclear energy applications, particularly in the qualification of materials for high-temperature structural use. This report presents work on refining the creep testing of small specimen geometries. Efforts include the development of a new specimen geometry for sub-sized specimens, which were subjected to uniaxial creep tests. The results contribute to the understanding of material behavior under stress at elevated temperatures and offer potential improvements in creep data collection methods. These findings support ongoing advancements in material qualification processes essential for nuclear reactor applications.

36 MATERIALS SCIENCE↗

SMR Containment Cable and Electrical Penetration Assembly System

GAIN Project CRADA Number NFE-21-08839, entitled “SMR Containment Cable and EPA System” was initiated by the partnership of Oak Ridge National Laboratory (ORNL) and Engineered Solutions Group (ESG) to test an ESG-designed Electrical Penetration Assembly and Containment Cabling System Qualified for not only SMR technologies, but also Advanced Reactors design. An Electrical Penetration Assembly (EPA) is a component used to allow electrical power and signal conductors as well as optical fiber through the nuclear reactor’s containment structure while maintaining a pressure barrier. The EPA ensures the containment's integrity both during the normal operation and also accident conditions by providing a sealed passage for power and signals. This project was undertaken to fill the equipment gap of EPA and Cabling Systems that require much more severe environmental requirements than legacy plant applications present due to their smaller containment volumes that result in high energy densities compared to legacy designs. This high energy density results in severe accident environments and also more severe normal operating conditions.This document describes cost effective approaches to qualify a unique EPA for Small Modular Reactor (SMR) technologies as legacy LWR EPA technologies will likely have inherent material performance insufficiencies. The DBA profiles for SMRs (and some Advanced Reactor Technologies) are more severe than the legacy qualification requirements making the design of the qualification testing system challenging as the temperatures and pressures can approach the limits permitted by ASME Pressure Vessel Code, as well as accident temperatures exceeding the capability of polymeric gaskets and dielectrics. Small Modular Reactors are designed to have, as the name suggests, modularity which implies sized for factory fabrication and subsequent assembly at the power plant site. SMR containment is much smaller than a legacy Light Water Reactor containment. The containment walls are likely to be comprised of stainless steel. Qualifying Electrical Penetration Assemblies (EPAs) through these steel vessels are of interest in this work. Methods are presented here that discuss critical safety and cost effectiveness for these SMR EPA’s test systems.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Report on Properties and Microstructure of 3D Printed Inc-718

The report presents the microstructure and mechanical properties of 3D printed Inconel 718 to assess its potential use as a structural material for the Transformation Challenge Reactor (TCR). The structural components near the outlet of the core will experience significant neutron fluxes and outlet coolant temperatures from the hot standby temperature of 300°C to nearly 550°C at the center of the part. These components must support the core in appropriate loading conditions and require structural analysis at relevant temperatures. Strong spatial and chemical heterogeneity was found in as-built (ASB) Inconel 718. Three heat treatments were designed and conducted to simplify the microstructure and determine how each precipitating phase contributed to the overall strength. Baseline mechanical properties were measured from uniaxial tensile tests on subsize SS-J2 specimens at room temperature and at elevated temperatures of 300, 450, and 600°C. Microstructure electron microscopy was performed on ASB Inconel 718 and heat treated to correlate the observed mechanical properties with nanoscale features. Homogenization of the microstructure led to a highly ductile Inconel with lower strength compared with wrought Inconel 718. The tensile properties of additively manufactured 718 using a standard ASTMrecommended heat treatment were consistent with literature and with the ASTM for the properties of this alloy. A higher fraction of the δ phase led to shorter uniform elongation without altering other engineering properties.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Pilot Testing of a Highly Efficient Pre-combustion Sorbent-based Carbon Capture System

TDA developed and demonstrated a highly efficient pre-combustion carbon capture system. The overall objective of this work was to develop a new sorbent-based pre-combustion carbon capture technology for Integrated Gasification Combined Cycle (IGCC) power plants. In this project our goal was to demonstrate the techno-economic viability of the new technology by 1) demonstrating it in large-scale slipstream tests, and 2) carrying out a high fidelity engineering and cost analysis. TDA’s process used an advanced physical adsorbent that selectively removes CO 2 from coal-derived synthesis gas above the dew point of the gas at temperatures as high as 300°C. The sorbent consists of a mesoporous carbon whose surface was grafted with functional groups that remove CO 2 via a well-known acid-base interaction. As documented in bench-scale experiments and field tests with actual coal gas, the sorbent achieved a very high capacity for CO 2 at temperatures as high as 300°C. The sorbent bound CO 2 more strongly than common physical adsorbents, providing the chemical potential needed for the high temperature operation. However, because CO 2 does not form a true covalent bond with the surface sites (as is the case with chemical absorbents), the sorbent regeneration could be carried out with only a very small energy input. The heat input to regenerate our sorbent was only 4.9 kcal per mol of CO 2 , which is much lower than that for chemical absorbents (e.g., 29.9 kcal/mol CO 2 for sodium carbonate) and was similar to the requirements of physical solvents (e.g., 4 kcal/mol CO 2 for Selexol TM ). Because the sorbent operates above the dew point of the synthesis gas (unlike the Selexol TM process), a higher power cycle efficiency can be achieved. With previous DOE/NETL funding (Contract No. DE-FE-0000469), we demonstrated the techno-economic viability of the technology in bench-scale tests and slipstream demonstrations at the National Carbon Capture Center (NCCC), Wilsonville, Alabama and Wabash River IGCC plant in Terra Haute, Indiana. We demonstrated a stable working CO 2 capacity for over 11,650 cycles with simulated synthesis gas. We also evaluated its performance with actual synthesis gas in two test campaigns at the Wabash River IGCC Plant, Terre Haute, IN and the National Carbon Capture Center (NCCC), Wilsonville, AL. The slipstream tests clearly showed that the actual coal gas constituents and potential contaminants (e.g. trace metals, halides, tars) had no effect on the sorbent’s ability to remove CO 2 (the same sorbent beds were used in both field tests with no sign of deactivation for 2,000 cycles with over 26,750 SCF of gas treated). As expected, due to the high temperature CO 2 removal capability and low energy needed to regenerate the sorbent, the power cycle efficiency with our process was greater than 34% on a higher heating value (HHV) basis; in comparison, the same IGCC plant equipped with the Selexol TM solvent for carbon capture can only achieve 31.4% HHV efficiency. The capital cost for an IGCC system with TDA’s process is estimated as $2,417/kW e , which is 12% lower than that of the IGCC/ Selexol TM process. The levelized cost for electricity including the transport, storage and monitoring (TS&M) cost for CO 2 was calculated as $\$ $92.9/MWh (lowest reported to our knowledge), which is much better than the $105.2/MWh estimated for the IGCC/ Selexol TM process. In this project (DE-FE0013105), TDA Research, in collaboration with our partners Gas Technology Institute (GTI), Illinois Clean Coal Institute (ICCI), University of California, Irvine (UCI), University of Alberta (UOA), Siemens, NCCC and Sinopec advanced the technical maturity of the technology; scaling it up by a factor of 100. We optimized the reactor design using computational fluid dynamics (CFD); using adsorption modeling we improved the pressure swing adsorption (PSA) cycle sequence. We carried out two field test campaigns with a fully-equipped 0.1 MW e prototype unit (for a total of 844 hours) using actual synthesis gas to prove the viability of the new technology. A successful 30 day (707 hrs) evaluation was completed at NCCC under air blown gasification conditions. We demonstrated 97.3% carbon capture at 1,500 SLPM, 93% carbon capture at 1,800 SLPM, and 90% carbon capture at 2,100 SLPM in the NCCC tests. We also demonstrated the system for 137 hours at a Sinopec petrochemical plant under oxygen blown gasification, demonstrating 86% carbon capture at 2,660 SLPM. In collaboration with University of California, Irvine (UCI), we completed a techno-economic analysis (TEA) for TDA’s warm gas cleanup technology integrated to IGCC power plant. The net plant efficiencies (on a coal HHV basis) for the warm gas cleanup cases were estimated to be 34.0% for E-GasTM gasifier, 34.4% for GE gasifier, 33.4 for the Shell gasifier and 34.2 for the TRIG TM gasifier (Cases 2, 4, 6 and 8 in this study) with a catalytic combustor for CO 2 purification, which are significantly higher than those for the Cold Gas Case, or an increase of as much as 12% in the heat rate for Case 2, 6% for Case 4, 9% for Case 6, and 9% for Case 8. The 1st year cost of electricity with the transport, storage and monitoring (TS&M) costs for the CO 2 included was $\$ $129.2/MWh for the E-GasTM gasifier Warm Gas Cleanup Case, $\$ $131.9/MWh for the GE gasifier Warm Gas Cleanup Case, $\$ $146.8/MWh for the Shell Gasifier Warm Gas Cleanup Case, and $\$ $129.9/MWh for the TRIG TM gasifier Warm Gas Cleanup Case. For comparison, the costs for the baseline Cold Gas CO 2 removal with Selexol for the different gasifiers were: $\$ $146.6/MWh for the E-Gas TM gasifier, $\$ $142.2/MWh for the GE gasifier, $\$ $159.0/MWh for the Shell gasifier and $\$ $144.3/MWh for the TRIG TM gasifier. In summary, the costs for our system were 7 to 12% lower than the corresponding Cold Gas Cleanup cases. The results of this techno-economic analysis suggested that TDA’s high temperature PSA-based Warm Gas Clean-up Technology can make a substantial improvement in the IGCC plant thermal performance for achieving near zero CO 2 emissions for E-Gas TM , GE, Shell and TRIG TM gasifier based IGCC power plants. The capital expenses were estimated to be lower than that of Selexol’s™. Taken together, the higher net plant efficiency and lower capital and operating costs resulted in substantial reduction in the cost of carbon capture for the IGCC plant equipped with TDA’s high temperature PSA-based carbon capture system. Finally, in collaboration with Gas Technology Institute (GTI) we completed the environmental health and safety assessment for TDA’s warm gas carbon capture technology.

01 COAL, LIGNITE, AND PEAT↗