INL Carbon Characterization Lab
What goes into AGC Graphite Characterization
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.
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Photographic combustion characterization of LOX/hydrocarbon type propellants
Single element injectors and two fuels were tested with the aim of photographically characterizing observed combustion phenomena. The three injectors tested were the O-F-O triplet, the transverse like on like (TLOL), and the rectangular unlike doublet (RUD). The fuels tested were RP-1 and propane. The hot firings were conducted in a specifically constructed chamber fitted with quartz windows for photographically viewing the impingement spray field. All LOX/HC testing demonstrated coking with the RP-1 fuel leaving far more soot than the propane fuel. No fuel freezing or popping was experienced under the test conditions evaluated. Carbon particle emission and combustion light brilliance increased with Pc for both fuels although RP-1 was far more energetic in this respect. The RSS phenomena appear to be present in the high Pc tests as evidenced by striations in the spray pattern and by separate fuel rich and oxidizer rich areas. The RUD element was also tested as a fuel rich gas generator element by switching the propellant circuits. Excessive sooting occurred at this low mixture ratio (0.55), precluding photographic data.
Judd, D. C.↗
Advancing radioactive material research method: the development of a novel in situ particle-attached microfluidic electrochemical cell
This study aims to develop a microgram-scale microfluidic electrochemical cell (E-cell) for investigating the redox behavior of uranium oxide (UO 2 ). The traditional bulk electrochemical methods may require shielded facilities to investigate the hazardous materials, e.g., spent nuclear fuel, due to high radiation levels. Microfluidic E-cells offer advantages such as reduced radiation exposure, control over fluid flow rates, and high-throughput capabilities. Methods: The design of the E-cell considers electrode morphology, adhesion to a thin membrane, electrode configuration, and vacuum compatibility. Three techniques, including FIB-SEM lift-out, Au coating, and polyvinylidene fluoride (PVDF) binder, are explored for fabricating and attaching microgram quantities of UO 2 as working electrodes. The PVDF binder method proves to be the most effective, enabling the creation of a vacuum-compatible microfluidic E-cell. Results and discussion: The PVDF binder method demonstrates successful electrochemical responses and allows for real-time monitoring of UO 2 electrode behavior at the microscale. It offers chemical imaging capabilities using in situ SEM/EDS analysis. The technique provides consistent redox outcomes similar to bulk electrochemical analysis. Conclusion: The development of a microgram-scale microfluidic electrochemical cell using the PVDF binder technique enables the investigation of UO 2 redox behavior. It offers a low-risk approach with reduced radiation exposure and high-throughput capabilities. The technique provides real-time monitoring and chemical imaging capabilities, making it valuable for studying spent nuclear fuel systems and material characterization.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Spatiotemporal energy infrastructure datasets for the United States: A review
Not Available
Tavakkoli, Sakineh↗
Preparation and evaluation of advanced catalysts for phosphoric acid fuel cells
The platinum electrocatalysts were characterized for their crystallite sizes and the degree of dispersion on the carbon supports. One application of these electrocatalysts was for anodic oxidation of hydrogen in hot phosphoric acid fuel cells, coupled with the influence of low concentrations of carbon monoxide in the fuel gas stream. In a similar way, these platinum on carbon electrocatalysts were evaluated for oxygen reduction in hot phosphoric acid. Binary noble metal alloys were prepared for anodic oxidation of hydrogen and noble metal-refractory metal mixtures were prepared for oxygen reduction. An exemplar alloy of platinum and palladium (50/50 atom %) was discovered for anodic oxidation of hydrogen in the presence of carbon monoxide, and patent disclosures were submitted. For the cathode, platinum-vanadium alloys were prepared showing improved performance over pure platinum. Preliminary experiments on electrocatalyst utilization in electrode structures showed low utilization of the noble metal when the electrocatalyst loading exceeded one weight percent on the carbon.
Stonehart, P.↗
Characterization, Operation and Analysis of Test Motors Containing Aluminized Hybrid Fuels
NASA Marshall Space Flight Center's Materials and Processes Department, with support from the Propulsion Systems Department, has renewed the development and maintenance of a hybrid test bed for exposing ablative thermal protection materials to an environment similar to that seen in solid rocket motors (SRM). The Solid Fuel Torch (SFT), operated during the Space Shuttle program, utilized gaseous oxygen for oxidizer and an aluminized hydroxyl-terminated polybutadiene (HTPB) fuel grain to expose a converging section of phenolic material to a 400 psi, 2-phase flow combustion environment. The configuration allows for up to a 2 foot long, 5 inch diameter fuel grain cartridge. Wanting to now test rubber insulation materials with a turn-back feature to mimic the geometry of an aft dome being impinged by alumina particles, the throat area has now been increased by several times to afford flow similarity. Combined with the desire to maintain a higher operating pressure, the oxidizer flow rate is being increased by a factor of 10. Out of these changes has arisen the need to characterize the fuel/oxidizer combination in a higher mass flux condition than has been previously tested at MSFC, and at which the literature has little to no reporting as well. Testing for fuel regression rate comprised a two-level, full factorial design available over Aluminum loading level, mass flow rate, pressure, and diameter. The data taken significantly surpasses the previous available data on regression rate of aluminized HTPB fuel burning with gaseous oxygen. It encompasses higher mass fluxes, and appears to generate more consistent data. The good test article and facility design and testing work of the Penn State HPCL combined with careful analysis of the data and good planning has made this possible. This should be able to assist with developing rate laws that are useful both for research planning and for developing flight system sizing relationships that can help optimize hybrid rocket concepts for trade studies. The successful approach of this DOE and test setup is applicable to other propellant combinations as well.
Kibbey, Timothy P.↗
Characterization, Operation and Analysis of Test Motors Containing Aluminized Hybrid Fuels
NASA Marshall Space Flight Center's Materials and Processes Department, with support from the Propulsion Systems Department, has renewed the development and maintenance of a hybrid test bed for exposing ablative thermal protection materials to an environment similar to that seen in solid rocket motors (SRM). The Solid Fuel Torch (SFT), operated during the Space Shuttle program, utilized gaseous oxygen for oxidizer and an aluminized hydroxyl-terminated polybutadiene (HTPB) fuel grain to expose a converging section of phenolic material to a 400 psi, 2-phase flow combustion environment. The configuration allows for up to a 2 foot long, 5 inch diameter fuel grain cartridge. Wanting to now test rubber insulation materials with a turn-back feature to mimic the geometry of an aft dome being impinged by alumina particles, the throat area has now been increased by several times to afford flow similarity. Combined with the desire to maintain a higher operating pressure, the oxidizer flow rate is being increased by a factor of 10. Out of these changes has arisen the need to characterize the fuel/oxidizer combination in a higher mass flux condition than has been previously tested at MSFC, and at which the literature has little to no reporting as well. Testing for fuel regression rate comprised a two-level, full factorial design available over Aluminum loading level, mass flow rate, pressure, and diameter. The data taken significantly surpasses the previous available data on regression rate of aluminized HTPB fuel burning with gaseous oxygen. It encompasses higher mass fluxes, and appears to generate more consistent data. The good test article and facility design and testing work of the Penn State HPCL combined with careful analysis of the data and good planning has made this possible. This should be able to assist with developing rate laws that are useful both for research planning and for developing flight system sizing relationships that can help optimize hybrid rocket concepts for trade studies. The successful approach of this DOE and test setup is applicable to other propellant combinations as well.
Kibbey, Timothy P.↗
Characterization and Detailed Analysis of Regression Behavior for HTPB Solid Fuels Containing High Aluminum Loadings
NASA Marshall Space Flight Center's Materials and Processes Department, with support from the Propulsion Systems Department, has renewed the development and maintenance of a hybrid test bed for exposing ablative thermal protection materials to an environment similar to that seen in solid rocket motors (SRM). The Solid Fuel Torch (SFT), operated during the Space Shuttle program, utilized gaseous oxygen for oxidizer and an aluminized hydroxyl-terminated polybutadiene (HTPB) fuel grain to expose a converging section of phenolic material to a 400 psi, 2-phase flow combustion environment. The configuration allows for up to a 2 foot long, 5 inch diameter fuel grain cartridge. Wanting to now test rubber insulation materials with a turn-back feature to mimic the geometry of an aft dome being impinged by alumina particles, the throat area has now been increased by several times to afford flow similarity. Combined with the desire to maintain a higher operating pressure, the oxidizer flow rate is being increased by a factor of 10. Out of these changes has arisen the need to characterize the fuel/oxidizer combination in a higher mass flux condition than has been previously tested at MSFC, and at which the literature has little to no reporting as well. For (especially) metalized fuels, hybrid references have pointed out possible dependence of fuel regression rate on a number of variables: mass flux, G - oxidizer only (G0), or - total mass flux (Gtot), Length, L, Pressure, P, and Diameter, D.
Kibbey, Timothy P.↗
Time-resolved spray characterization via unified optical flow and binarization technique
This work leverages an unsupervised machine learning and advanced image processing techniques to characterize the breakup of fuel sprays in a small-scale combustor under reacting conditions, providing valuable insights into near-nozzle flow phenomenology. The proposed methodology integrates an improved optical flow model on a convolutional neural network to extract flow vectors with a binarization technique to assess droplets’ size and shape across the region of interest. The velocimetry approach demonstrates superior performance compared to a state-of-the-art optical flow model when applied to high-speed X-ray phase contrast spray images, achieving more accurate and reliable flow predictions. Moreover, breakup processes are quantified by breakup length and sphericity in accordance with velocity estimations, allowing a more complete characterization of the flow. This study establishes a robust methodology for analyzing spray morphology and primary breakup in compact combustors, contributing valuable means of understanding and optimizing fuel spray behavior in advanced combustion systems.
42 ENGINEERING↗
Investigation of Sooting in Microgravity Droplet Combustion: Fuel-Dependent Effects
Kumagai and coworkers first performed microgravity droplet combustion experiments [Kumagai, 1957]. The primary goal of these early experiments were to validate simple 'd(sup 2)-law models [Spalding, 1954, Godsave, 1954] Inherent in the 'd(sup 2) -law' formulation and in the scope of the experimental observation is the neglect of sooting behavior. In fact, the influence of sooting has not received much attention until more recent works [Choi et al., 1990; Jackson et al., 1991; Jackson and Avedisian, 1994; Choi and Lee, 1996; Jackson and Avedisian, 1996; Lee et al., 1998]:. Choi and Lee measured soot volume fraction for microgravity droplet flames using full-field light extinction and subsequent tomographic inversion [Choi and Lee, 1996]. In this investigation, soot concentrations were measured for heptane droplets and it was reported that soot concentrations were considerably higher in microgravity compared to the normal gravity flame. It was reasoned that the absence of buoyancy and the effects of thermophoresis resulted in the higher soot concentrations. Lee et al. [1998] performed soot measurement experiments by varying the initial droplet diameter and found marked influence of sooting on the droplet burning behavior. There is growing sentiment that sooting in droplet combustion must no longer be neglected and that "perhaps one of the most important outstanding contributions of (micro)g droplet combustion is the observation that in the absence of asymmetrical forced and natural convection, a soot shell is formed between the droplet surface and the flame, exerting an influence on the droplet combustion response far greater than previously recognized." [Law and Faeth, 1994]. One of the methods that we are exploring to control the degree of sooting in microgravity is to use different fuels. The effect of fuel structure on sooting propensity has been investigated for over-ventilated concentric coflowing buoyant diffusion flames. (Glassman, 1996]. In these investigations, the fuel flowrate was increased until smoke was observed to escape from the "luminous visible flame" [Glassman, 1996]. A total of 29 fuels were used in order to characterize relative sooting propensity. The sooting propensity of a particular fuel was assessed by comparing the flowrates for soot emission from the tip of the flame. It was reported that the sooting tendency for diffusion flames increased for fuels with higher rates of pyrolysis. Randolph and Law [1986 and not 1994] also examined the effect of fuel structure on droplet sooting behavior. In their experiments the droplets were separated from the bulk gas stream and quenched with nitrogen prior to gravimetric measurements. A variety of fuels were studied, namely aromatics, phenyl-alkanes and alkanes. The results were in qualitative agreement with the work of Glassman [1986]. Vander Wal et al. [1994] performed relative soot concentration measurements using laser-induced incandescence for heptane and decane fuel droplets burning under normal-gravity conditions. It was found that soot volume fractions for decane was more than a factor of two larger than that for heptane. Although the normal-gravity investigations have provided some important insights regarding the influence of fuel structure on the sooting behavior of droplet flames, results cannot be easily extrapolated for microgravity studies since increased residence times and thermophoretic effects must be considered in greater detail. Several studies have compared sooting behavior of different fuel droplets burning under microgravity conditions [Card and Choi, 1990; Jackson et al., 1991; Jackson and Avedisian, 1994], however, detailed quantitative results were not provided. In all of these previous studies, the degree of sooting was only visually assessed from an incandescent backlighted image of the soot containing region. Such techniques can provide misleading results regarding sooting behavior [Choi, 1996].
Manzello, Samuel L.↗
Can Water-Injected Turbomachines Provide Cost-Effective Emissions and Maintenance Reductions?
An investigation has been performed to evaluate the effect of water injection on the performance of the Air Force Research Laboratory (AFRL, Wright-Patterson Air Force Base (WPAFB)) experimental trapped vortex combustor (TVC) over a range of fuel-to-air and water-to-fuel ratios. Performance is characterized by combustor exit quantities: temperature and emissions measurements using rakes, and overall pressure drop, from upstream plenum to combustor exit. Combustor visualization is performed using gray-scale and color still photographs and high-frame-rate videos. A parallel investigation evaluated the performance of a computational fluid dynamics (CFD) tool for the prediction of the reacting flow in a liquid fueled combustor (e.g., TVC) that uses water injection for control of pollutant emissions and turbine inlet temperature. Generally, reasonable agreement is found between data and NO(x) computations. Based on a study assessing the feasibility and performance impact of using water injection on a Boeing 747-400 aircraft to reduce NO(x) emissions during takeoff, retrofitting does not appear to be cost effective; however, an operator of a newly designed engine and airframe might be able to save up to 1.0 percent in operating costs. Other challenges of water injection will be discussed.
Hendricks, Robert C.↗
An Initial Microstructurally Informed Model of High Burnup Structure Formation in UO 2 Fuel
The microstructure of a UO 2 fuel pellet changes as burnup increases, impacting fuel performance. Predicting and characterizing high burnup structure (HBS) and dark zone formation is a key part of supporting burnup limit extensions for light water reactors. This paper describes a model developed through fitting radially resolved pellet data obtained from recently published microstructural characterization data. The model predicts grain size and grain character, in addition to pore density and size, with fitting dependencies on power history variables. Separately fitting power history variables to microstructural parameters allows for insight into the underlying physical phenomena for future model development. Additionally, experimental data have been correlated to an HBS fraction to facilitate the development of a model capable of predicting a total fuel restructured fraction at the engineering scale. In conclusion, this two-step approach provides a coupling from reactor power history to microstructural data to fractional HBS and creates a basis to model HBS-dependent parameters in a fuel performance code.
High burnup structure↗
Characterization of Mk-IV and EBR-II X441A Metallic Fuel Pins for the THOR-C-2 and THOR-M-TOP-1 Experiments: Results from Post-Transient Neutron Tomography of THOR-C-2 Capsule and Pre-transient Non-Destructive and Destructive Examination of DP 36 and DP 40 (Rev.1)
Current interest in sodium-cooled fast reactor designs, such as TerraPower’s Natrium Reactor, has highlighted the need for advanced-reactor fuel technology development. A Fuel Safety Research and Development (FSRD) program for metallic fast reactor fuels has been created to achieve comprehensive safety testing within the re-commissioned Transient Reactor Test (TREAT) facility at the Idaho National Laboratory. Despite over 60 years of metallic fuel irradiation, uncertainties exist in the performance of the fuel system, particularly under anticipated operational occurrences and severe accident scenarios. Throughout historical testing within the Experimental Breeder Reactor (EBR)-II and the Fast Flux Test Facility, fuel behavior has demonstrated benign response to transient reactor conditions; however, accurate predictions of failure thresholds rely heavily on fuel composition and irradiation history. In advancing the FSRD program, two planned transient heating experiments are at various stages of completion. The Temperature Heat sink Overpower Response (THOR)-C-2, fueled with an unirradiated Mk IV U-10Zr pin, has undergone transient irradiation in TREAT and post-transient three-dimensional neutron tomography. Additionally, pre-transient characterization of test and sibling U-19Pu-10Zr pins for THOR-M-TOP-1 was evaluated by both non-destructive and destructive methods. The test and sibling pins were selected from previously irradiated EBR-II experiment X441A. Both pins underwent visual examination, precise gamma spectrometry, two-dimensional neutron radiography, and element contact profilometry while the sibling pin was additionally subjected to sectioning and optical microscopy. THOR-C-2 radiography captured the fuel and cladding relocation during the intermediate transient at the top and bottom of the THOR capsule, allowing key features to be linked to the pin’s measured thermal response. For THOR M TOP 1, a solid baseline for steady-state behavior has been established. No anomalous features were identified in either the test or sibling pin. Defining characteristics and features were recorded for further comparisons.
22 GENERAL STUDIES OF NUCLEAR REACTORS↗
Nuclear waste reduction: Exploring new pathways one step at a time
In my home country of Venezuela, nuclear energy is not a topic that attracts much attention. The government briefly oversaw some nuclear energy programs during the 1950s, but currently there are no active nuclear power facilities in the country. In fact, the Venezuelan government signed and ratified the treaty of the prohibition of nuclear weapons in 2021, which states that Venezuela has never owned, possessed or controlled nuclear weapons or programs of any kind. When I moved to the United States, however, nuclear energy became an extremely relevant topic. In the 1940s, the U.S. government established and oversaw the Manhattan Project to build atomic bombs for use in World War II. After the war, the government encouraged scientists to use this information on nuclear reactions to develop nuclear energy for peaceful civilian purposes instead.1 During these early days of nuclear research, there were no formal regulatory standards for nuclear waste management. Policies usually were self-regulated and often created based on existing policies of disposal for non-nuclear waste.2 As a result, there were instances of nuclear waste leaching into the environment and affecting local communities. So, much research has been conducted since then to characterize and store nuclear waste safely and securely.3 I first became interested in nuclear energy during my undergraduate studies when I worked on a project involving ligand synthesis to help extract actinides from nuclear waste. I then studied electrochemistry in molten salt systems for nuclear energy applications during my Ph.D. As I approached graduation, I started looking into national laboratories that have programs involving nuclear energy and waste management. At Idaho National Laboratory (INL), the focus is more on applied processes and how nuclear energy can be innovated to realize next-generation reactor design and technologies. This focus led me to apply for a Seaborg distinguished postdoctoral position at INL, for which I was chosen based on my proposal of a way to improve nuclear waste recycling. To understand my proposal, we must familiarize ourselves with the makeup of nuclear waste. After uranium dioxide is used as nuclear fuel in a reactor, the fuel matrix is then characterized by various fission products, including rare earth elements, alkali and alkaline earths, and actinides. Some of these fission products can potentially be recovered through pyroprocessing, 4 which involves the electrochemical dissolution of the used nuclear fuel in a molten chloride salt mixture at high temperatures. Though some of the fission products can be easily recovered—for example, uranium is reduced onto an inert cathode by applied potentials—numerous other fission products such as rare earth elements are difficult to recover due to their multivalent oxidation states and side reactions.5 To improve the recovery efficiency of rare earth elements specifically, I proposed investigating the fundamental interactions between rare earth elements in the molten chloride salt and their metallic form (Figure 1). The kinetic pathways and the chemical reactions of these elements, which will be elucidated through spectro-electrochemistry at high temperatures, will give insights on how the recovery efficiency can be improved. Although my research focuses on fundamental science, it will benefit the applied process by generating new scientific knowledge and closing the gap for efficient recycling of the waste: one step at a time.
11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
High Temperature High Vacuum Mechanical Property Assessment of Zirconium Nuclear Fuel Cladding
This report presents the mechanical characterization of a specific Zry-4 cladding batch serving as the foundation for a diverse range of fuel performance research at Oak Ridge National Laboratory (ORNL). This effort supports research needs for the U.S. Department of Energy (DOE), particularly regarding evaluating accident tolerant fuel (ATF) cladding coating concepts, expanding understanding of cladding response to loss-of-coolant accidents (LOCA) transients, refining post-critical heat flux (CHF) limits (t@T), and upcoming irradiation campaigns. The central objective was to define the baseline performance of the substrate Zircaloy-4 (Zry-4) material leveraged across ORNL Advanced Fuel Campaign (AFC) efforts through controlled high-temperature vacuum tensile testing. This work begins to address gaps in existing models where implementation based on nominal heat-treatment labels, such as stress relief annealed (SRA), often fail to capture the interplay of recovery, recrystallization, and grain growth. To quantify this, data was benchmarked against the Pacific Northwest National Laboratory (PNNL) stress strain model to determine where this material falls in comparison to assumed values for materials in the same heat treatment regime. Analysis of the tensile data revealed that this specific SRA batch exhibits a transitional microstructural state best described by an effective cold-work (CW) parameter of 0.09, diverging from the previous estimation of 0.5 for SRA materials. Additionally, comparative testing of Cr coated specimens demonstrated no distinct difference in axial strength relative to the bare substrate. This suggests that the strengthening benefits of Cr coatings observed in burst scenarios are driven by residual stress mechanisms acting solely in the hoop direction.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Chapter Four—MSW characterization and preprocessing for biofuels and bioproducts
The organic fraction of MSW (OFMSW) has a high carbohydrate and lipid content, indicating its good potential as a feedstock for bioethanol and biodiesel production. However, variability in feedstock composition for MSW is a critical challenge for downstream conversion processes such as pyrolysis, gasification, incineration, and biotechnological conversion. MSW characterization is critical to inform and optimize the design of physical handling processes to minimize costs and environmental impacts, and improve the downstream conversion performance of MSW materials. Here, this book chapter focuses on current MSW characterization and preprocessing technologies and discusses the costs, benefits, and environmental impacts associated with MSW preprocessing. Also, the book chapter outlines the potential strategies to increase total revenue and mitigate negative environmental impacts for MSW recycling systems.
09 BIOMASS FUELS↗
Initial results from electron microscopy from AGR 5/6/7 Capsule 1 fuel and
Initial results from electron microscopy from AGR 5/6/7 Capsule 1 fuel and applications of other microanalysis techniques to irradiated TRISO fuel. Includes detail on characterization of particles from AGR 5/6/7 Capsule 1, which include background and motivation, x-ray computed tomography on four particles from compact 1-7-9, SEM/EDS of particles from compacts 1-7-9 and 1-7-4, and Summary. Local thermal conductivity measurement on AGR-2 particles also discussed.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
The U.S. Accident Tolerant Fuels Program — Update on a National Initiative
In 2012 the U.S. Congress directed the Department of Energy’s (DOE) Office of Nuclear Energy to give priority to developing enhanced fuels and cladding for light water reactors to improve safety in the event of accidents in the reactor or spent fuel pools. DOE developed a plan with a goal to insert a Lead Test Assembly (LTA) into a commercial light water reactor by the end of FY 2022. Three of the leading commercial nuclear fuel vendors, in concert with several participating commercial nuclear utilities, are now seriously engaged in this initiative and have exceeded initial expectations by having met DOE’s goal this year, three years ahead of schedule. The early successes of the ATF program are due in part to a strong collaboration by the DOE national laboratories with both commercial nuclear fuel vendors and the U.S. Nuclear Regulatory Commission. This undertaking has recently been expanded to incorporate an effort to extend burnup from the current U.S. regulatory limit of 62 GWD/MTU and increase enrichment as necessary to support routine utilization of fuel at >75 GWD/MTU. This effort provides a critical economic incentive to accelerate the deployment of ATF technologies. This paper reviews the DOE-sponsored, industry-led ATF concepts currently under development and highlights the contributions made by the DOE laboratories in support of these ATF concepts, including: 1) steady-state irradiation testing in the Advanced Test Reactor (ATR) and High Flux Isotope Reactor (HFIR); 2) transient irradiation testing in the Transient Reactor Test Facility (TREAT); 3) fabrication process development and characterization of high density fuels, Cr-coated Zry cladding, FeCrAl cladding, and SiC cladding; and 4) post-irradiation examination of lead test rods irradiated in commercial reactors.
Goldner, Frank J.↗