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At least 37 records · Page 2

Key results from examinations of seven high burnup pressurized water reactor spent nuclear fuel rods

At present, spent nuclear fuel (SNF) assemblies discharged from US commercial power plants are placed into dry storage following a short cooling time (<10 years) in the plant’s spent fuel pool. The process of packaging the spent fuel into dry-storage canisters includes a drying step to remove residual water from the canister. During the drying process, the fuel rod cladding may reach temperatures as high as 400°C. Oak Ridge National Laboratory (ORNL) is performing destructive examinations of high burnup (HBU) (>45 GWd/MTU) SNF rods to address knowledge and data gaps related to extended interim storage and eventual transportation for disposal. The rods examined include four different kinds of fuel rod cladding: standard Zircaloy-4 (Zirc-4), low-tin (LT) Zirc-4, ZIRLO, and M5. Three rods were subjected to a thermal transient to assess the effects of decay-heat-driven high temperatures expected during vacuum drying of the fuel as it is prepared for interim dry storage. The examinations focus on the composite fuel rod performance, as compared with the performance of defueled rod cladding, and establish the baseline mechanical properties of a fuel rod before interim dry storage. The key results of these examinations are presented, including the measured mechanical and fatigue properties, observations of cladding hydrogen pickup and hydride reorientation effects on rod performance, effects of the simulated drying temperatures on rod performance, and general conclusions of SNF performance in extended interim dry storage and transport. The rods were found to be strong and durable in the expected loading conditions, even considering the formation of radial hydrides associated with vacuum drying. The combined testing provides a broad body of data supporting extended interim storage and transportation performance of HBU spent fuel.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Extending the family of reduced [Mn 12 O 12 (O 2 CR) 16 (H 2 O) x ] n- complexes, and their sensitivity to environmental factors

Here, the family of reduced [Mn 12 O 12 (O 2 CR) 16 (H 2 O) 4 ] n- (n = 1, 2) single-molecule magnets (SMMs) has been expanded with the synthesis of new members using I - as a stoichiometric one-electron reducing agent of the neutral n = 0 complexes. Electrochemical data, 1 H NMR spectra of the [Mn 12 O 12 (O 2 CCH 2 Cl) 16 (H 2 O) 3 ] 0,-,2- salts, and the crystal structures of two complexes, (PPh 4 )[Mn 12 O 12 (O 2 CCHCl 2 ) 16 (H 2 O) 4 ] and (PPh 4 ) 2 [Mn 12 O 12 (O 2 CCH 2 Cl) 16 (H 2 O) 3 ] have been obtained. For (PPh 4 ) 2 [Mn 12 O 12 (O 2 CCH 2 Cl) 16 (H 2 O) 3 ], the data confirm an S = 10 ground state, and magnetization vs dc field scans on a pristine crystal exhibit hysteresis loops possessing steps due to quantum tunneling of magnetization (QTM). In addition, two forms of the cluster have been identified in the crystal with distinctly different relaxation barriers, with the faster-relaxing form being the majority one in pristine crystals from mother liquor, and the slower-relaxing one becoming the majority one in vacuum-dried samples. Similar behavior is seen for (PPh 4 )[Mn 12 O 12 (O 2 CCHCl 2 ) 16 (H 2 O) 4 ] with an S = 19 / 2 ground state, which shows three forms to be present in the hysteresis loops of a pristine crystal, all converting to a slow-relaxing form on vacuum-drying. High-frequency EPR spectra of the latter confirm a high axial anisotropy with $\mathcal{D}$ = -0.477 cm -1 and rationalize its effective relaxation barrier U eff = 57 K. The combined work emphasizes a high sensitivity of such ultra-small nanomagnets to environmental influences, affecting their properties significantly, especially their quantum properties that are so important to many potential new 21st century applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Solvent-Free Manufacturing of Lithium-Ion Battery Electrodes via Cold Plasma

Slurry casting has been used to fabricate lithium-ion battery electrodes for decades, which involves toxic and expensive organic solvents followed by high-cost vacuum drying and electrode calendering. This work presents a new manufacturing method using a nonthermal plasma to create inter-particle binding without using any polymeric binding materials, enabling solvent-free manufacturing electrodes with any electrochemistry of choice. The cold-plasma-coating technique enables fabricating electrodes with thickness (>200 μm), high mass loading (>30 mg cm -2 ), high peel strength, and the ability to print lithium-ion batteries in an arbitrary geometry. This crosscutting, chemistry agnostic, platform technology would increase energy density, eliminate the use of solvents, vacuum drying, and calendering processes during production, and reduce manufacturing cost for current and future cell designs. Here, lithium iron phosphate and lithium cobalt oxide were used as examples to demonstrate the efficacy of the cold-plasma-coating technique. It is found that the mechanical peel strength of cold-plasma-coating-manufactured lithium iron phosphate is over an order of magnitude higher than that of slurry-casted lithium iron phosphate electrodes. Full cells assembled with a graphite anode and the cold-plasma-coating-lithium iron phosphate cathode offer highly reversible cycling performance with a capacity retention of 81.6% over 500 cycles. For the highly conductive cathode material lithium cobalt oxide, an areal capacity of 4.2 mAh cm -2 at 0.2 C is attained. We anticipate that this new, highly scalable manufacturing technique will redefine global lithium-ion battery manufacturing providing significantly reduced plant footprints and material costs.

25 ENERGY STORAGE↗

TRANSIENT THERMAL MODELING OF THE HIGH BURNUP DEMONSTRATION RESEARCH PROJECT CASK USING STAR-CCM+ AND COBRA-SFS

The Department of Energy in collaboration with the Electric Power Research Institute is in the process of conducting the High Burnup Demonstration Project. Where the objective is to characterize the performance of high-burnup fuel in long term storage. As part of this demonstration, a TN-32B dry storage cask was instrumented and loaded with spent nuclear fuel at North Anna Nuclear Generating Station in November 2017. The project cask provides a unique opportunity to gain information on spent fuel and cask performance from an in-service operational system. The cask was instrumented with thermocouples inside of the fuel assemblies, then loaded and dried using normal procedures. After the drying process a thermal soak period where the cask was left indoors was used to obtain steady temperatures for model comparison along with surface temperatures. This paper details thermal modeling validation work that was done to model both the steady state and transient cases. Two modeling tools were used to predict temperatures in the cask. The general purpose CFD and heat transfer code STAR-CCM+ was used with both a detailed pin-by-pin model was used along with a more efficient k-effective simplification. The other code is COBRA-SFS, a purpose-built detailed thermal modeling tool developed and maintained at PNNL. Results from all the modeling tools were compared blind to the test data. Each model utilized general design information and compared reasonably well to the blind steady state data using convection and surface temperature boundary conditions. Post-test adjustments were later made to better reflect the “as built” conditions of the cask. Based on lessons learned from the steady state analysis the vacuum drying process was modeled in both codes. Utilizing the measured loading conditions the transient models were able to compare very well with the measured data. Overall the project showed an ability to model spent fuel storage conditions very well and future work is planned to generalize the methodology used for vacuum drying.

Thermal Analysis, Spent Fuel, Dry Storage↗

Update on the Investigation of Commercial Drying Cycles Using the Advanced Drying Cycle Simulator

The purpose of this report is to document updates on the apparatus to simulate commercial vacuum drying procedures at the Nuclear Energy Work Complex at Sandia National Laboratories. Validation of the extent of water removal in a dry spent nuclear fuel storage system based on drying procedures used at nuclear power plants is needed to close existing technical gaps. Operational conditions leading to incomplete drying may have potential impacts on the fuel, cladding, and other components in the system during subsequent storage and disposal. A general lack of data suitable for model validation of commercial nuclear canister drying processes necessitates well-designed investigations of drying process efficacy and water retention. Scaled tests that incorporate relevant physics and well-controlled boundary conditions are essential to provide insight and guidance to the simulation of prototypic systems undergoing drying processes. This report documents a new test apparatus, the Advanced Drying Cycle Simulator (ADCS). This apparatus was built to simulate commercial drying procedures and quantify the amount of residual water remaining in a pressurized water reactor (PWR) fuel assembly after drying. The ADCS was constructed with a prototypic 17×17 PWR fuel skeleton and waterproof heater rods to simulate decay heat. These waterproof heaters are the next generation design to heater rods developed and tested at Sandia National Laboratories in FY20. This report describes the ADCS vessel build that was completed late in FY22, including the receipt of the prototypic length waterproof heater rods and construction of the fuel basket and the pressure vessel components. In addition, installations of thermocouples, emissivity coupons, pressure and vacuum lines, pressure transducers, and electrical connections were completed. Preliminary power functionality testing was conducted to demonstrate the capabilities of the ADCS. In FY23, a test plan for the ADCS will be developed to implement a drying procedure based on measurements from the process used for the High Burnup Demonstration Project. While applying power to the simulated fuel rods, this procedure is expected to consist of filling the ADCS vessel with water, draining the water with applied pressure and multiple helium blowdowns, evacuating additional water with a vacuum drying sequence at successively lower pressures, and backfilling the vessel with helium. Additional investigations are expected to feature failed fuel rod simulators with engineered cladding defects and guide tubes with obstructed dashpots to challenge the drying system with multiple water retention sites.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

BWR Spent Nuclear Fuel Acquisition and Testing to Support DOE-NE High Burnup Spent Fuel Data Project

The Office of Spent Fuel and Waste Disposition (SFWD) within the US Department of Energy (DOE) Office of Nuclear Energy (NE) established the Spent Fuel and Waste Science and Technology (SFWST) campaign to conduct research and development (R&D) activities related to the storage, transportation, and disposal of spent nuclear fuel (SNF) and high-level radioactive waste. The SFWST program was created within SFWD to address issues of extended or long-term SNF storage and transportation. Some near-term objectives of SFWST are to use a science-based, engineering-driven approach to: Support the enhancement of the technical bases to support the continued safe and secure dry storage of SNF for extended periods; Support the enhancement of the technical bases for retrieving SNF after extended dry storage; Support the enhancement of the technical bases for transporting high burnup (HBU) fuel and transporting low burnup fuel and HBU fuel after dry storage DOE-NE, in partnership with the Electric Power Research Institute, developed the High Burnup Spent Fuel Data Project to perform a large-scale demonstration and laboratory-scale testing of HBU pressurized water reactor (PWR) fuels (exceeding 45 gigawatt-days per metric ton of uranium [GWd/MTU]). Under this project, 25 sister rods—which are rods that have the same design, power histories, and other characteristics—were removed from assemblies at the North Anna Nuclear Power Station and sent to Oak Ridge National Laboratory (ORNL) in January 2016. ORNL performed detailed nondestructive examination (NDE) on all 25 rods. The NDE consisted of visual examinations, gamma and neutron scanning, profilometry and rod length measurements, and eddy current examinations. After completing the NDE, 10 of the sister rods were delivered to Pacific Northwest National Laboratory (PNNL) in a NAC International, Inc. legal-weight truck cask in September 2018 for destructive examination (DE). To date, SFWD work has focused on the PWR fuel that is part of the Sister Rod Test program. No boiling water reactor (BWR) fuel has been tested in the program, and the data needs that were identified for the PWR fuel have not been collected for BWR fuel. The goal to obtain six to nine BWR rods and test them at ORNL will support closing this important data gap. BWR fuel comprises approximately 56% of the total fuel assemblies currently in storage at nuclear power plants in the United States. BWR nuclear fuel and cladding designs and manufacturing are significantly different from PWRs. Differences include the following: BWR fuel pellets are larger than PWR pellets; Variations of Zircaloy-2 (including liners) are used instead of the Zircaloy-4 cladding materials used in PWRs; Clad manufacturing and stress-relief processes are different between PWRs and BWRs; The fuel rod dimensions are different because larger rod diameters and thicker cladding are used in BWRs; BWR fuel typically has lower internal rod pressures and sees vastly different operating conditions than PWR fuel (i.e., two-phase flow); BWR assemblies are “canned,” meaning each assembly is surrounded by a metal fuel channel; BWR cladding is often composed of an inner pure Zr liner that has widely different mechanical properties than the Zircaloy-2 alloy and exhibits a stronger affinity for hydrogen; The BWR SNF generally has more total hydrogen in the cladding/liner than typical PWR fuel; The construction of the PWR and BWR assemblies is vastly different; BWR rods are solidly attached to the assembly nozzles and experience a much different vibration and shock load than PWR rods, which are “floating” within a grid system attached to guide tubes, and the rods sit loosely on the bottom end plates. These numerous differences will affect the way the BWR SNF responds under dry storage preparation processes (e.g., vacuum drying) and during transportation. The results collected in the PWR experimental program must be compared with a subset of similar data collected on BWR SNF to establish a technical basis for whether the larger PWR database is sufficient to bound the BWR SNF end-of-life conditions as is currently assumed for several fuel/clad properties. Changes that occur in both fuel types at HBU could exacerbate any mechanical property differences. As the fuel burnup increases, several changes occur that might affect the performance of the fuel, cladding, and assembly hardware in storage and transportation. These changes include increased cladding corrosion layer thickness, increased cladding hydrogen content, increased cladding creep strains, increased fission gas release, and the formation of the HBU structure at the surface of the fuel pellets. The Nuclear Regulatory Commission (NRC) limits the current maximum rod-averaged burnup to 62 GWd/MTU due to these changes and the lack of data at higher burnups.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Quantification of Residual Water in Spent Fuel Dry Storage Canisters Using Mass Spectrometry

The purpose of this report is to document updates on the apparatus to simulate commercial vacuum drying procedures at the Nuclear Energy Work Complex at Sandia National Laboratories. Validation of the extent of water removal in a dry spent nuclear fuel storage system based on drying procedures used at nuclear power plants is needed to close existing technical gaps. Operational conditions leading to incomplete drying may have potential impacts on the fuel, cladding, and other components in the system during subsequent storage and disposal, such as fuel degradation; cladding corrosion, embrittlement, or breaching; and the creation of a flammable environment via radiolysis of water. A general lack of data suitable for model validation of commercial nuclear canister drying processes necessitates well-designed investigations of drying process efficacy and water retention. Scaled tests that incorporate relevant physics and well-controlled boundary conditions are essential to provide insight and guidance to the simulation of prototypic systems undergoing drying processes. This report documents details on the quantification of residual water in the Advanced Drying Cycle Simulator (ADCS), an apparatus built to simulate commercial drying procedures and quantify the amount of residual water remaining in a pressurized water reactor (PWR) fuel assembly after drying. The ADCS was constructed with a prototypic 17×17 PWR fuel skeleton and waterproof heater rods to simulate decay heat. The ADCS is outfitted with thermocouples to measure the thermal response of the ADCS to simulated decay heats and internal helium fill pressures relevant to commercial drying procedures. The ADCS is also instrumented with pressure transducers to measure the pressures and vacuum levels observed during simulated commercial drying. The most unique instrumentation used for quantifying residual water in the ADCS is a Hiden Analytical HPR-30 mass spectrometer (MS), which measures gas compositions of the ADCS internal free volume, based on partial pressures calculated from relative proportions of gas molecules detected by the MS. This report details the methodology used to implement MS measurements in quantifying residual water in the ADCS. This methodology includes the calibration of the HPR-30 MS to a Buck Research Instruments CR-4 chilled mirror hygrometer, which itself is calibrated to a NIST-traceable standard. Data collected by both the MS and the chilled mirror hygrometer from water/helium mixtures ranging from 150 to 500,000 ppmv water in helium were used to generate calibration curves, establishing a source of verification of MS measured water contents. Details regarding water content measurement uncertainties are included in this report, defining the accuracy and verifiability of the HPR-30 MS in measuring residual water content in simulated dry storage canister environments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Response of a Pressurized Water Reactor Dashpot Region to Commercial Drying Cycles

The purpose of this report is to document updates to the simulation of commercial vacuum drying procedures at the Nuclear Energy Work Complex at Sandia National Laboratories. Validation of the extent of water removal in a dry spent nuclear fuel storage system based on drying procedures used at nuclear power plants is needed to close existing technical gaps. Operational conditions leading to incomplete drying may have potential impacts on the fuel, cladding, and other components in the system. A general lack of data suitable for model validation of commercial nuclear canister drying processes necessitates additional, well-designed investigations of drying process efficacy and water retention. Scaled tests that incorporate relevant physics and well-controlled boundary conditions are essential to provide insight and guidance to the simulation of prototypic systems undergoing drying processes. This report documents testing updates for the Dashpot Drying Apparatus (DDA), an apparatus constructed at a reduced scale with multiple Pressurized Water Reactor (PWR) fuel rod surrogates and a single guide tube dashpot. This apparatus is fashioned from a truncated 5×5 section of a prototypic 17×17 PWR fuel skeleton and includes the lowest segment of a single guide tube, often referred to as the dashpot region. The guide tube in this assembly is open and allows for insertion of a poison rod (neutron absorber) surrogate.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Preliminary Simulations of Commercial Drying Cycles Using the Advanced Drying Cycle Simulator

The purpose of this report is to document updates on the apparatus to simulate commercial vacuum drying procedures at the Nuclear Energy Work Complex at Sandia National Laboratories. Validation of the extent of water removal in a dry spent nuclear fuel storage system based on drying procedures used at nuclear power plants is needed to close existing technical gaps. Operational conditions leading to incomplete drying may have potential impacts on the fuel, cladding, and other components in the system during subsequent storage and disposal. A general lack of data suitable for model validation of commercial nuclear canister drying processes necessitates well-designed investigations of drying process efficacy and water retention. Scaled tests that incorporate relevant physics and well-controlled boundary conditions are essential to provide insight and guidance to the simulation of prototypic systems undergoing drying processes. This report documents fiscal year 2023 (FY23) updates on the Advanced Drying Cycle Simulator (ADCS). This apparatus was built to simulate commercial drying procedures and quantify the amount of residual water remaining in a pressurized water reactor (PWR) fuel assembly after drying. The ADCS was constructed with a prototypic 17×17 PWR fuel skeleton and waterproof heater rods to simulate decay heat. These waterproof heaters are the next generation design to heater rods developed and tested at Sandia National Laboratories in FY20. In FY23, a series of four simulated commercial drying tests was completed. This report presents the temperature and pressure histories of the drying tests as well as axial temperature profiles that can be compared to data from the Electric Power Research Institute (EPRI) High Burnup Demonstration TN-32B cask. Water content measurements and dew point calculations from a Hiden Analytical HPR-30 mass spectrometer are also presented in this report. Due to familiarization with this first-of-a-kind system, refinements to equipment calibration and test procedures have been identified to better match commercial drying cycles for future simulated tests. However, the presented data demonstrate the successful construction and operation of a viable research platform for quantifying residual water content closely approaching that expected in dry storage canisters during commercial drying procedures.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Update on the Simulation of Commercial Drying of Spent Nuclear Fuel

The purpose of this report is to document improvements in the simulation of commercial vacuum drying procedures at the Nuclear Energy Work Complex at Sandia National Laboratories. Validation of the extent of water removal in a dry spent nuclear fuel storage system based on drying procedures used at nuclear power plants is needed to close existing technical gaps. Operational conditions leading to incomplete drying may have potential impacts on the fuel, cladding, and other components in the system. A general lack of data suitable for model validation of commercial nuclear canister drying processes necessitates additional, well-designed investigations of drying process efficacy and water retention. Scaled tests that incorporate relevant physics and well-controlled boundary conditions are essential to provide insight and guidance to the simulation of prototypic systems undergoing drying processes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Effects of Residual Water on Storage Canister Internal Components

This report describes an evaluation of the spent nuclear fuel cladding and canister internal materials’ corrosion/oxidation due to (inadvertent) residual free water inside a dry storage canister post-dryout. Drying of spent nuclear fuel (SNF) and the impact of (inadvertent) residual water in a SNF canister is being addressed under the DOE-NE Spent Fuel and Waste Science and Technology (SFWST) program to ensure the safe extended dry storage and transportation of commercial SNF. A long-standing understanding has been that the amount of residual water in a storage canister after vacuum drying is not expected to be much more than trace amounts of 0.43 gram mole. However, recent findings from the High Burnup Demonstration project, and an Integrated Research Project show that residual free water well above the amount of approximately 0.43 gm-moles that had been assumed for a 3 torr rebound pressure, may remain within an SNF canister following prototypic drying. In fact, an NRC-NMSS sponsored study considered residual water amount as high as 55 moles. Considering the recent findings and the NRC-sponsored work, this present work was conducted to study the effects of unspecified amount of residual water on oxidation and corrosion of canister internals, i.e., it was assumed that the residual water amount is not limiting. It was assumed that the spent nuclear fuel content in the canister is not exposed to the internal environment, i.e., the packaged canister does not contain any damaged (breached) fuel.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Drying Spent Magnox Fuel for Interim Dry Storage

Spent Magnox fuel is usually stored under water for shielding and cooling following use in-reactor, but the storage water can react with Magnox clad fuel and cause corrosion and forms a sludge which generates a secondary waste product. One option to prevent unwanted corrosion and avoid expensive waste management is to dry the wet fuel. This project aims to test a drying process which will convert wet and corroded Magnox fuel to a stable form to demonstrate viability for conversion from wet to dry storage. Samples of corroded Magnox supplied by National Nuclear Laboratory. Corrosion product retrieved by various methods including dry scraping, ultrasonic treatment to form sludge and sludge drying to isolate suspension. TGA undertaken on Sample 1 and Sample 2, with brucite and hydromagnesite for comparison. Both samples showed ∼10% mass loss up to 250 deg. C attributable to water held in sample. Mass loss from dehydroxylation which liberates further water in both samples. TGA data plotted alongside chemically pure brucite and hydromagnesite shows expected similarities/differences between Sample 1(mostly brucite) and Sample 2 (brucite/hydromagnesite mixture). Following treatment, dried samples observed to slowly gain mass in ambient conditions. Presumed to be hygroscopic absorption of air water vapour as effect is reversible, with similar effect observed for hydromagnesite and brucite. Etched Magnox vacuum dried for 3.5 h at 90 deg. C to test for reaction with residual water - some discoloration but no noticeable corrosion observed. Drying etched Magnox metal to observe surface effects/corrosion during drying process.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Development of Mockups and Instrumentation for Spent Fuel Drying Tests

The purpose of this report is to provide updates on the experimental components, methodology, and instrumentation under development for use in advanced studies of realistic drying operations conducted on surrogate spent nuclear fuel. Validation of the extent of water removal in a dry spent nuclear fuel storage system based on drying procedures used at nuclear power plants is needed to close existing technical gaps. Operational conditions leading to incomplete drying may have potential impacts on the fuel, cladding, and other components in the system. Water remaining in canisters upon completion of drying procedures can lead to cladding corrosion, embrittlement, and breaching, as well as fuel degradation. Additional information is needed on the drying process efficacy to help evaluate the potential impacts of water retention on extended longterm dry storage. A general lack of data suitable for model validation of commercial nuclear canister drying processes necessitates additional, well-designed investigations. Smaller-scale tests that incorporate relevant physics and well-controlled boundary conditions are essential to provide insight and guidance to the simulation of prototypic systems undergoing drying processes. This report describes the implementation of moisture monitoring equipment on a pressurized, submersible system employing a single waterproof, electrically heated spent fuel rod simulator as a demonstration of analytical capabilities during a drying process. A mass spectrometer with specially designed inlets was used to monitor moisture and other gases at 150 kPa to 800 kPa for a test simulating a forced helium dehydration procedure and below 1 torr for tests mimicking a vacuum drying process. The dew point data from the mass spectrometer was found to be in good agreement with a solid-state moisture probe. A distinct advantage of the mass spectrometer system was the capability to directly sample from the hightemperature (>200 °C) head space expected in a prototypic scale experiment where a solid-state moisture probe would suffer considerable loss of accuracy or fail altogether. The operational and analytical experiences gained from this test series are poised to support an expansion to assembly-scale tests at prototypic length. These assemblies are designed to feature prototypic assembly hardware, advanced diagnostics for in situ internal rod pressure monitoring, and failed fuel rod simulators with engineered cladding defects to challenge the drying system with waterlogged fuel.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Rapid Evaluation of Amine-Functionalized Solvents for Biomass Deconstruction Using High-Throughput Screening and One-Pot Enzymatic Saccharification

Efficient and sustainable pretreatment of lignocellulosic biomass is critical for biofuel and biochemical production, yet its optimization is often hindered by slow, labor-intensive experimental methods. Here, we report the first demonstration of a custom-built, miniaturized, high-throughput screening platform integrated with one-pot enzymatic saccharification, enabling parallel evaluation of solvent type, feedstock, and temperature with minimal material use and high reproducibility. As a proof-of-concept, the HTX platform was used to screen five amine-functionalized solvents, including isopropanolamine, butylamine, N-methylbutylamine, ethanolamine, and ethanolamine acetate across three bioenergy crops (sorghum, poplar, and switchgrass) and pretreatment temperatures ranging from 80 to 140 °C. Vacuum drying successfully removed more than 99% of the solvents from the pretreated biomass, eliminating the need for water washing prior to saccharification. Isopropanolamine and N-methylbutylamine yielded the highest glucose (70–80%) and xylose (58–67%) release, with trends reflecting feedstock recalcitrance. The produced hydrolysates supported robust growth of an engineered strain of the yeast Rhodosporidium toruloides, confirming biocompatibility. This high-throughput platform provides a scalable, feedstock-agnostic framework for rapid pretreatment screening, accelerating solvent–feedstock pairing and process optimization. Its ability to integrate pretreatment, solvent removal, saccharification, and microbial conversion in a miniaturized format offers significant advantages for cost-competitive biorefinery development.

Biomass↗

Electrochemical Investigation of Moisture Byproducts in Molten Calcium Chloride

Residual water in molten CaCl 2 reacts to form different byproducts, such as HCl, which can impact the corrosivity of the salt and efficiency of electrochemical operations, such as electrolytic oxide reduction and electrorefining. The ability to detect and quantify these byproducts electrochemically can provide feedback on the efficacy of vacuum drying and other purification methods, as well as the impact of these byproducts on process operations. An electrochemical signal’s association with the production of H 2 is verified and characterized using cyclic voltammetry (CV) and residual gas analysis. CV estimated a 2-electron exchange process associated with H 2 production. CV detected trace quantities of an oxidized species containing hydrogen in the salt on the order of 10 ppm. Different salt handling methods were compared for their impact on the hydrogen electrochemical signal. It was found that 30 min of exposure of CaCl 2 in a beaker to low-humidity air (<20%) had minimal impact on the H 2 production signal.

Electrochemistry↗

Sister Rod Destructive Examinations (FY23) Appendix F3: Uncertainty and Conservative Bias in the Cyclic Integrated Reversible-Bending Fatigue Test

The development and application of the Cyclic Integrated Reversible-Bending Fatigue Tester (CIRFT) has been documented over the past 10 years. The CIRFT system was developed in collaboration with the U.S. Nuclear Regulatory Commission (NRC) to address the concern that high-burnup fuel rod fatigue performance was degraded compared to cladding-only behavior. Fatigue data measured by CIRFT on high-burnup fuel rods were then used by the NRC to develop a fatigue response curve for pressurized water reactor fuel rods with Zircaloy-4 cladding in NUREG-2224. Subsequently, CIRFT has been used in the sister rod project to test whether reoriented hydrides associated with vacuum drying influenced the fatigue lifetime, to extend the fatigue testing database to include fuel rods with ZIRLO cladding, and to add to the experience on both Zircaloy-4 and M5 cladding. These data will be used as a reference for subsequent characterization of fuel rods removed from the high-burnup demonstration cask to better understand the effects of long-term dry storage, which can be thought of as a multiyear elevated temperature anneal. The objective of fatigue testing is to provide data that can be used to develop a best-estimate fatigue curve and a conservative fatigue design curve that accounts for uncertainty and can be compared with actual transportation conditions. The process for defining a design fatigue curve for commercial used fuel rods was developed by Oak Ridge National Laboratory (ORNL) in FY22. One issue noted in the fatigue evaluation was that the calculated combined uncertainty in the strain amplitude values determined from the measured data was large. It was proposed then to directly measure the uncertainty in the strain amplitude to either validate the calculated combined uncertainty or update the uncertainty based on the measurement data. Thus, the purpose of this appendix is to document the measured uncertainty in the strain amplitude data. In the process, it was determined that there has been a conservative bias in the calculated strain amplitude that is small enough to be within the measurement uncertainty. This observation is discussed herein, and a case is made to continue to include the conservative bias in the data.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗