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Sister Rod Destructive Examinations (FY23) Appendix I: SNF Aerosols Released During Rod Fracture

This report documents work performed under the Spent Fuel and Waste Disposition’s Spent Fuel and Waste Science and Technology program for the US Department of Energy (DOE) Office of Nuclear Energy (NE). This work was performed to fulfill Level 3 Milestone M3SF-23OR010201026, “FY23 M3 draft report on results from testing in FY23,” within work package SF-23OR01020102 and is an updated to the work reported in M2SF-23OR010201024, M2SF-22OR010201047, M2SF-21OR010201032, M2SF-19ORO010201026, and M2SF-19OR010201028. As a part of the DOE NE High Burnup Spent Fuel Data Project, Oak Ridge National Laboratory (ORNL) is performing destructive examinations (DEs) of high burnup (HBU) (>45 GWd/MTU) spent nuclear fuel (SNF) rods from the North Anna Nuclear Power Station operated by Dominion Energy. The SNF rods, called sister rods or sibling rods, are all HBU and include four different kinds of fuel rod cladding: standard Zircaloy-4 (Zirc-4), low-tin Zirc-4, ZIRLO, and M5. The DEs are being conducted to obtain a baseline of the HBU rods’ condition before dry storage and are focused on understanding overall SNF rod strength and durability. Fuel rods and defueled cladding will be tested to derive material properties. Although the data generated can be used for multiple purposes, one primary goal for obtaining the post-irradiation examination data and the associated measured mechanical properties is to support SNF dry storage licensing and relicensing activities by (1) addressing identified knowledge gaps and (2) enhancing the technical basis for post-storage transportation, handling, and subsequent disposition.This report documents the status of the ORNL Phase 1 DE activities related to the collection of SNF aerosol particles released during fuel rod fracture in 4-point bending in Phase 1 of the sister rod test program.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Comet flyby sample return experiment

Dust from several comets can be returned to earth with minimum propulsion effort after a high-speed encounter. The collection concept involves the capture of individual dust particles by condensation in a cell after vaporization by a thin diaphragm. This collection concept has been validated in laboratory tests. To compensate for the slower laboratory velocities in a two-stage light-gas gun, higher-density metals (Zn and Cd) have been used for particles and diaphragms to simulate hypervelocity vaporization. Teflon has proved to be a suitable material for the collection cell; more than 50 percent of the vaporized projectile material has been recovered by chemical etching from such cells. Hypervelocity-impact parameters (such as diaphragm-to-projectile ratio, hole size, and plume angles) determined by tests permit the modification of existing analytical models. These new findings are necessary for flyby cometary experiments.

Tsou, P.↗

Window Cooling Studies and Disk Vibration Testing on a Subset of Mo-100 Disks

Production of metastable Technetium-99 (Tc-99m), a radioactive tracer that emits gamma rays, is vital to the medical imaging community. Tc-99m is extracted from the decay of Molybdenum-99 (Mo-99) which has a half-life of about 2-3 days. The work presented in this report is part of the NNSA’s mission to produce Mo-99 commercially, within the US, without the use of highly enriched uranium (HEU) in support of nonproliferation and global security. Los Alamos National Laboratory (LANL) is working with NorthStar Medical Radioisotopes (NMR) on their efforts to produce Mo-99 through the irradiation of Mo-100 targets using an electron beam. The NMR target comprises a stack of approximately 60-70 Mo-100 disks with diameter 24 mm and thickness 0.74 mm held in stainless steel laminations, each separated using 0.25 mm thick stainless-steel spacers. The symmetric target stack is housed in an Inconel vessel with two Inconel windows on either side. Two electron accelerators are used to produce 40 MeV, 3.16 µA electron beams each that penetrate the Inconel windows and irradiate the Mo-100 disks. Approximately 90% of the total 250 kW beam power is deposited in the NMR target during the irradiation process, with a smaller percentage adding up to 2.2 kW of heat deposited on the Inconel window. During irradiation, pressurized helium gas flows through thin gaps between the disks cooling the beam window, target disks, disk laminations and spacers. Both NMR and LANL have found during cold testing of the target system (no heat deposition) that the Mo 100 disks undergo significant mass loss and disk breakage due to vibrations induced by the flowing helium gas. The mass loss is not only undesirable due to monetary loss from reduced final quantities of Mo-99, but also due to the hazards associated with radioactive material trapped in the cooling lines and particle filters. The effect of flow rate and target geometry on the flow induced vibrations need to be quantified, and recommendations provided to minimize this mass loss. LANL has previously also tested NMR’s Inconel beam window by heating the window, while flowing pressurized helium, using the average heat deposited on the window. However, the NMR beam is pulsed with a duty cycle of 12.5%, which introduces oscillation in temperature around the nominal 600 °C steady state value with each pulse. Available fatigue curves for Inconel are few, established for room temperature, and they are based on mechanical strain cycles not thermally induced strain as in the NMR target. The effect of pulsed beam heating on the Inconel window therefore needs to be quantified. This report details the experiments conducted to assess the factors that lead to mass loss in the NMR target disks as well as to understand the effect of a pulsed beam on NMR’s Inconel window. This work describes LANL’s experimental characterization of the flow induced vibrations and disk mass loss in a reduced scale set-up containing 5 to 10 Mo-100 disks. We use high speed imaging, displacement measurements and microphone measurements combined with signal processing to estimate the vibration frequency of each disk. The effect of disk thickness, target fit and duration of testing on the mass loss is described. We find that in the current configuration of NMR targets, the vibrations and mass loss on the first disk are minimized, while those in the adjacent disks are highest. The microphone and high-speed image data show that increased flow rates and increased duration of testing increases vibration frequency and mass loss. The mass loss is due to both disk rotation and back and forth motion. There are visible wear marks on the disks with the highest mass loss. We also note that the current NMR window gap reduces flow induced vibrations compared to the previous smaller gaps. Improved target holders significantly reduce disk mass loss to almost negligible quantities. This work finds that the larger window to first disk gap and improved target holder geometry should allow NMR to successfully conduct irradiations with minimal mass loss. The window tests were conducted to understand the effect of a pulsed beam on both the window longevity and to estimate the window temperature and displacement during pulsing. The experiments presented here were performed at significantly low power, due to the limitations of the induction heating system. The window temperature rose to approximately 73 °C with a significantly reduced power of 45 W without beam pulsing. With a 5 Hz pulse rate, 12.5% duty cycle, the window temperature remained constant at 26 °C. These experiments will be repeated with improved coil geometry and reported in upcoming journal papers.

42 ENGINEERING↗

The particle size of Martian aeolian dunes

The effective particle size of unconsolidated materials on the Martian surface can be determined from thermal inertia, due to a pore size dependence of thermal conductivity at Martian atmospheric pressures. Because dunes consist of a narrow range of well-sorted, unconsolidated particles, they provide for a test of the relationship between particle size and thermal inertia calculated from midinfrared emission data for the Martian surface. Two independent approaches are used. First, thermal inertia data indicate that Martian dunes have an average particle size of about 500 +/-100 microns, or medium to coarse sand. Second, expected dune particle sizes are determined from grain trajectory calculations and the particle size transition from suspension to saltation. On earth, the transition occurs for a grain when the ratio of the terminal fall velocity to the wind friction speed, u*(t) is near unity; for grains at u*(t) this occurs at about 52 microns. Terrrestrial dune sands have a mean of 250 microns and are composed entirely of grains greater than 52 microns. The corresponding Martian transition grain size is about 210 microns, suggesting that Martian dunes should be significantly coarser than terrestrial dunes. Grain saltation path length as a function of particle size also shows that, under Martian conditions, larger grains than on earth will become suspended. Both approaches indicate that Martian dune sand should be coarser than terrestrial dune sand. These results closely match the grain sizes determined from thermal inertia models, providing the first direct test of the validity of these models for actual Martian surface materials.

Edgett, Kenneth S.↗

NLR CSP Optical Facilities: Illuminating the Path Forward Through Innovation and Impact: Agreement 38490

This initiative is a multi-faceted project at the National Laboratory of the Rockies (NLR) aimed at strengthening its Concentrating Solar Power (CSP) Optical Facilities to advance the development of low-cost, high-performance materials for solar and other applications. The project's strategy is built on three pillars: strategic stakeholder engagement, diligent facility maintenance and utilization, and the development of new research capabilities. The overarching goal is to ensure the facilities remain state-of-the-art resources for industry and academia, thereby accelerating the conversion of concentrated sunlight into energy. A key driver of the project is an international Advisory Board, which provides critical guidance on research priorities and industry needs, leading to new collaborations and secured funding. This external engagement, combined with proactive outreach to industry partners, ensures the lab's work remains aligned with real-world challenges, including materials durability and performance certification. Significant efforts in facility maintenance have addressed challenges with aging infrastructure. Notable achievements include the complete refurbishment of the hail-damaged Ultra-Accelerated Weathering System (UAWS) and the successful replacement of a failing 15-year-old Lambda 1050 spectrophotometer with a new-generation model, substantially upgrading material characterization capabilities. These maintenance activities were complemented by achieving a prestigious ISO 9001:2015 certification for the Advanced Optical Materials Labs, formally recognizing the quality and reliability of NLR's measurement capabilities. Despite these successes, challenges remain, including high demand for the High Flux Solar Furnace (HFSF) and intermittent failures of other key instruments. The project has delivered major advancements in research techniques and capabilities. At the Flatirons campus, a new indoor laboratory, was established to house advanced deflectometry and photogrammetry systems for heliostat characterization. For on-sun testing, a novel, actively cooled turning mirror was developed for the HFSF, enabling more realistic testing of particle receivers and components. A collaboration with Virginia Tech successfully demonstrated the high-temperature durability of a new solar absorber coating through extensive cyclic testing. Concurrently, new modeling took place to better predict material degradation on rough, fractal surfaces. In summary, this project has systematically enhanced NLR's CSP Optical Facilities through strategic upgrades, rigorous maintenance, and stakeholder-guided research. By overcoming equipment failures, budgetary constraints, and logistical hurdles, the project has reinforced NLR's role as a central hub for CSP innovation and materials testing. Future work will focus on securing diverse funding, expanding collaborations, and continuing to provide the critical infrastructure needed to accelerate the development and deployment of next-generation technologies.

14 SOLAR ENERGY↗

Design of a Thermal Precipitator for the Characterization of Smoke Particles from Common Spacecraft Materials

A thermal precipitator (TP) was designed to collect smoke aerosol particles for microscopic analysis in fire characterization research. Information on particle morphology, size and agglomerate structure obtained from these tests supplements additional aerosol data collected. Modeling of the thermal precipitator throughout the design process was performed with the COMSOL Multiphysics finite element software package, including the Eulerian flow field and thermal gradients in the fluid. The COMSOL Particle Tracing Module was subsequently used to determine particle deposition. Modeling provided optimized design parameters such as geometry, flow rate and temperatures. The thermal precipitator was built and testing verified the performance of the first iteration of the device. The thermal precipitator was successfully operated and provided quality particle samples for microscopic analysis, which furthered the body of knowledge on smoke particulates. This information is a key element of smoke characterization and will be useful for future spacecraft fire detection research.

Smoke↗

Contamination control in hybrid microelectronic modules. Part 2: Selection and evaluation of coating materials

The selection, test, and evaluation of organic coating materials for contamination control in hybrid circuits is reported. The coatings were evaluated to determine their suitability for use as a conformal coating over the hybrid microcircuit (including chips and wire bonds) inside a hermetically sealed package. Evaluations included ease of coating application and repair and effect on thin film and thick film resistors, beam leads, wire bonds, transistor chips, and capacitor chips. The coatings were also tested for such properties as insulation resistance, voltage breakdown strength, and capability of immobilizing loose particles inside the packages. The selected coatings were found to be electrically, mechanically, and chemically compatible with all components and materials normally used in hybrid microcircuits.

Himmel, R. P.↗

Exploratory investigation on the use of low-cost alternative media for ultrafine grinding of coal

In this study, the energy efficiency of three alternative grinding media including, coarse silica beads, fine silica beads, and granular sand, were evaluated and compared against standard stainless steel. Stirred mill test results show that both silica beads and granular sand were more efficient than stainless steel in producing ultrafine particles following the order of coarse silica beads>granular sand>fine silica beads>stainless steel. The finest product size corresponding to a P 80 value of 2.33 μm was generated by coarse silica beads with a nominal size of 420×1190 μm, which also consumed the least amount of grinding energy. The specific energy input was reduced by almost 50% as opposed to that of stainless steel, while the operating work index was reduced by 87%. Overall, the test data indicate that grinding media density, media particle size and shape all play a role in determining the optimized grinding behavior of the coal material.

01 COAL, LIGNITE, AND PEAT↗

Impact of Silicon Impurity on the Hydrometallurgical Recovery of NCM622 Cathode

Hydrometallurgy is one of the best approaches to date for recycling LIBs due to its high efficiency, low energy usage, and industrial scalability. However, impurities have always been a thorny issue because they could have unintended impacts on the recovered cathode materials. This research marks the first systematic investigation into the influence of silicon impurity on the LiNi 0.6 Co 0.2 Mn 0.2 O 2 (NCM622) cathode obtained from hydrometallurgical recycling. Here we find that silicon nanoparticles will be nucleated at the center of the precursor particles during co-precipitation synthesis, and the silicon core will slowly dissolve in the surrounding ammonia, creating a special hollow structure in the particle. More importantly, the dissolution of silicon impurity will eventually lead to the deposition of silicates in the cathode material, which is an unfavorable result. Test data indicate that NCM622 cathode with 5 at% silicon has a capacity of 148.8 mAh g −1 after 100 cycles at 1/3 C, approximately 10 mAh g −1 lower than the virgin. Despite being relatively mild, the adverse influence of silicon impurity in hydrometallurgical recycling still requires attention.

25 ENERGY STORAGE↗

Effect of carbide size, area, density on rolling-element fatigue

A carbide parameter that can be used to predict rolling element fatigue life was developed.The parameter is based on a statistical life analysis and incorporates the total number of particles per unit area, particle size, and percent carbide area. These were determined from quantimet image analyzing computer examinations of random samples selected from eight lots of material previously tested in rolling fatigue. The carbide parameter is independent of chemical composition, heat treatment, and hardening mechanism of the materials investigated.

Chevalier, J. L.↗

Reducing Airborne Debris In Wind Tunnels

In proposed technique to trap airborne particles during normal wind-tunnel testing, large sections of single-backed adhesive paper or cloth mounted with adhesive side exposed to flow. Adhesive material securely installed on flow vanes, walls, or other surfaces of wind tunnel in manner facilitating replacement. Installed or replaced anytime permissible to enter tunnel. Provides safe, inexpensive, rugged, passive, continuous, and otherwise inert cleansing action suitable for wind tunnel of any size. Also applied to specialized clean-room environments and to air-conditioning systems in general.

Sleeper, Robert K.↗

Space Environmental Effects on the Optical Properties of Selected Transparent Polymers

Transparent polymer films are currently considered for use as solar concentrating lenses for spacecraft power and propulsion systems. These polymer films concentrate solar energy onto energy conversion devices such as solar cells and thermal energy systems. Conversion efficiency is directly related to the polymer transmission. Space environmental effects will decrease the transmission and thus reduce the conversion efficiency. This investigation focuses on the effects of ultraviolet and charged particle radiation on the transmission of selected transparent polymers. Multiple candidate polymer samples were exposed to near ultraviolet (NUV) radiation to screen the materials and select optimum materials for further study. All materials experienced transmission degradation of varying degree. A method was developed to normalize the transmission loss and thus rank the materials according to their tolerance of NUV. Teflon(Tm) FEP and Teflon(Tm) PFA were selected for further study. These materials were subjected to a combined charged particle dose equivalent to 5 years in a typical geosynchronous Earth orbit (GEO). Results from these NUV screening tests and the 5 year GEO equivalent dose are presented.

Edwards, David L.↗

Testing the Solar Probe Cup, an Instrument Designed to Touch the Sun

Solar Probe Plus will be the first, fastest, and closest mission to the sun, providing the first direct sampling of the sub-Alfvenic corona. The Solar Probe Cup (SPC) is a unique re-imagining of the traditional Faraday Cup design and materials for immersion in this high temperature environment. Sending an instrument of this type into a never-seen particle environment requires extensive characterization prior to launch to establish sufficient measurement accuracy and instrument response. To reach this end, a slew of tests for allowing SPC to see ranges of appropriate ions and electrons, as well as a facility that reproduces solar photon spectra and fluxes for this mission. Having already tested the SPC at flight like temperatures with no significant modification of the noise floor, we recently completed a round of particle testing to see if the deviations in Faraday Cup design fundamentally change the operation of the instrument. Results and implications from these tests will be presented, as well as performance comparisons to cousin instruments such as those on the WIND spacecraft.

Whittlesey, Phyllis L.↗

Testing the Solar Probe Cup, An Instrument Designed to Touch The Sun

Abstract: Solar Probe Plus will be the first, fastest, and closest mission to the Sun, providing the first direct sampling of the sub-Alfvénic corona. The Solar Probe Cup (SPC) is a unique re-imagining of the traditional Faraday Cup design and materials for immersion in this high temperature environment. Sending an instrument of this type into a never-seen particle environment requires extensive characterization prior to launch to establish sufficient measurement accuracy and instrument response. To reach this end, a slew of tests are created for allowing SPC to see ranges of appropriate ions and electrons, as well as a facility that reproduces solar photon spectra and fluxes for this mission. Having already tested the SPC at flight-like temperatures with no significant modification of the noise floor, we recently completed a round of particle testing to see if the deviations in Faraday Cup design fundamentally change the operation of the instrument. Results and implications from these tests will be presented, as well as performance comparisons to cousin instruments such as those on the WIND spacecraft.

solar physics↗

Monolithic ATF MiniFuel Sample Capsules Ready for HFIR Insertion

Several advanced nuclear fuel concepts are being considered throughout the nuclear industry. Implementation of these concepts could increase accident tolerance or enhance performance beyond the capabilities of the UO₂-based nuclear fuel currently in use. Qualification and deployment of any new fuel requires rigorous irradiation testing to demonstrate performance under representative normal and off-normal operating conditions. The traditional approach for qualifying new fuels requires exhaustive execution of many integral fuel tests. However, due to the long timeframe for executing these integral tests and the limited number of available materials test reactors, this approach is becoming impractical. To accelerate fuel qualification, Oak Ridge National Laboratory developed the MiniFuel irradiation vehicle for use in conducting accelerated separate effects irradiation testing of a wide range of nuclear fuel materials in the High Flux Isotope Reactor (HFIR). The first MiniFuel irradiations performed in the facility tested sol gel–derived uranium nitride kernels and tristructural isotropic (TRISO)-coated particle fuels. This report describes the preparation and assembly of the first set of monolithic MiniFuel irradiations conducted to support accident-tolerant fuel (ATF) development and accelerated fuel qualification. Two irradiation targets containing a variety of UO₂ and U₃Si₂ disk fuel specimens were fabricated and assembled for irradiation to burnups of 8-10 and 28-40 MWd/kg U. The target irradiation temperature is 450-550°C. Irradiation of U₃Si₂ will provide new data regarding the irradiation performance of a candidate ATF to complement current ATF-1 integral experiments being performed in the Advanced Test Reactor. UO₂ samples were included as a reference so that the results from the MiniFuel experiments can be compared with the extensive UO₂ fuel performance database. The monolithic MiniFuel capsules were successfully assembled, welded, and tested per HFIR requirements and are ready for insertion into the reactor. Pictures of the assembly process are included in this report. The experiment is planned for insertion into the HFIR during cycle 487 in April 2020.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Solid spherical glass particle impingement studies of plastic materials

Erosion experiments on polymethyl methacrylate (PMMA), polycarbonate, and polytetrafluoroethylene (PTFE) were conducted with spherical glass beads impacting at normal incidence. Optical and scanning electron microscopic studies and surface profile measurements were made on specimens at predetermined test intervals. During the initial stage of damage to PMMA and polycarbonate, material expands or builds up above the original surface. However, this buildup disappears as testing progresses. Little or no buildup was observed on PTFE. PTFE is observed to be the most resistant material to erosion and PMMA the least. At low impact pressures, material removal mechanisms are believed to be similar to those for metallic materials. However, at higher pressures, surface melting is indicated at the center of impact. Deformation and fatigue appear to play major roles in the material removal process with possible melting or softening.

Rao, P. V.↗

Material Response Analysis of PICA-NuSil at the Hypersonic Materials Environmental Test System

Phenolic impregnated carbon ablator (PICA) is a thermal protection system (TPS) that gained heritage during the Stardust mission and is the baseline TPS material for expeditions to Mars (e.g., Mars Science Laboratory and Mars 2020).1 PICA is friable; therefore, a polysiloxane resin (NuSil CV-1144-0) is deposited onto the surface of flight hardware before assembly, test, and launch operations (ATLO) to mitigate particle shedding. Furthermore, the Mars Science Laboratory (MSL) and Mars 2020 heatshields were instrumented with an array of thermocouple plugs (MEDLI Integrated Sensor Plugs or MISP) designed to measure the in-depth thermal response of PICA during flight. Post-flight analysis of MISP data suggests that recession was lower than predicted, and NuSil is suspected as a reasonable cause. NuSil primarily consists of a copolymer blend of dimethyl and diphenyl-substituted polysiloxane resin. Four decades of research in the field of polymer-derived ceramics demonstrate that polysiloxane resins form oxidation-resistant silicon oxycarbide materials at pyrolysis temperatures as low as 800 °C. -2 Furthermore, silicon oxycarbide materials exhibit excellent thermal stability at relatively high-temperatures (< 1200 °C) but eventually decompose via carbothermal reduction. -3 Therefore, it is reasonable to suggest that NuSil forms an oxidation-resistant thermal barrier coating on the TPS surface and influences the material response during atmospheric entry. Evidence for this notion was observed during prior arc-jet testing at both the Aerodynamic Heating Facility (AHF) and the Panel Test Facility (PTF) at the NASA Ames Research Center. Articles of PICA were subjected to testing in airflow, and a temperature discontinuity was recorded at the surface of coupons coated with NuSil. A glassy coating was observed to form at the surface in shear flow configurations (wedge and panel) under moderate heat fluxes. Furthermore, state-of-the-art material response models have yet to account for the underlying physics and chemistry of the temperature discontinuity. To this end, a pathfinder test campaign was executed at the Hypersonic Materials Environmental Test System (HyMETS) to enhance the fundamental understanding of PICA-NuSil ablation phenomena and provide a preliminary data set to aid in the development of material response models.

PICA↗

Vacuum Ultraviolet Radiation and Atomic Oxygen Durability Evaluation of HST Bi-Stem Thermal Shield Materials

Bellows-type thermal shields were used on the bi-stems of replacement solar arrays installed on the Hubble Space Telescope (HST) during the first HST servicing mission (SMI) in December 1993. These thermal shields helped reduce the problem of thermal gradient- induced jitter observed with the original HST solar arrays during orbital thermal cycling and have been in use on HST for eight years. This paper describes ground testing of the candidate solar array bi-stem thermal shield materials including backside aluminized Teflon(R)FEP (fluorinated ethylene propylene) with and without atomic oxygen (AO) and ultraviolet radiation protective surface coatings for durability to AO and combined AO and vacuum ultraviolet (VOV) radiation. NASA Glenn Research Center (GRC) conducted VUV and AO exposures of samples of candidate thermal shield materials at HST operational temperatures and pre- and post-exposure analyses as part of an overall program coordinated by NASA Goddard Space Flight Center (GSFC) to determine the on-orbit durability of these materials. Coating adhesion problems were observed for samples having the AO- and combined AO/UV-protective coatings. Coating lamination occurred with rapid thermal cycling testing which simulated orbital thermal cycling. This lack of adhesion caused production of coating flakes from the material that would have posed a serious risk to HST optics if the coated materials were used for the bi-stem thermal shields. No serious degradation was observed for the uncoated aluminized Teflon(R) as evaluated by optical microscopy, although atomic force microscopy (AFM) microhardness testing revealed that an embrittled surface layer formed on the uncoated Teflon(R) surface due to vacuum ultraviolet radiation exposure. This embrittled layer was not completely removed by AO erosion, No cracks or particle flakes were produced for the embrittled uncoated material upon exposure to VUV and AO at operational temperatures to an equivalent exposure of approximately five years in the HST environment. Uncoated aluminized FEP Teflon(R) was determined to be the most appropriate thermal shield material and was used on the bi-stems of replacement solar arrays installed on HST during SMI in December 1993. The SMI -installed solar arrays air scheduled to be replaced during MST's fourth servicing mission (SM3B) in early 2002.

Dever, Joyce↗