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Electron microscopy characterization of the fuel-cladding interaction in medium burnup annular fast reactor MOX
In this work, we present electron microscopy data focused on the fuel-cladding interaction layer in annular fast reactor MOX with HT-9 cladding at medium burnup. In agreement with previous literature data, the volatile fission products Cs, Te and I have migrated radially into the extreme fuel periphery and partially interacted with the cladding. The accumulation of Cs has occurred in the outermost rim of the fuel pellet, where grain recrystallization has also been observed. Significant amounts of Pd have been found in the interaction zone, particularly in the sample taken from the upper half of the fissile column where the cladding temperatures are higher. At this axial location, Cr has been enriched at the cladding inner surface and diffused into the fuel. Furthermore, chromium remains mainly in metallic form, but locally formed oxides. The fission products Cs, Te and I are found, with variable composition, in form of nanocrystalline regions dispersed in the metallic Cr-rich layer. The morphology and chemical characteristics of the layer suggest a non-oxidative corrosion mechanism as principal cladding degradation phenomenon occurring in this sample, with local onset of Cr oxidation within the nanocrystalline precipitates.
Detailed characterization of a PWR fuel rod at high burnup in support of LOCA testing
Experimental investigations of the fuel microstructure and volatile fission products along the pellet of a high burnup specimen (local burnup 76 GWd/tHM) have been conducted to support future transient testing. Detailed microscopy examinations have been carried out at different length scales. Transmission electron microscopy has highlighted a significant amount of damage across the entire radius with the formation of networks of dislocations. The optical and scanning electron microscopy determined the formation of three zones in the pellet with different characteristics. An intermediate region with no grain subdivision, lower porosity than the central zone porosity and high retained fission gas in nanometric bubbles and in the matrix was present between r/r0 ˜ 0.55 and 0.8. The high retention of gas in this region might suggest that the region will be prone to fine fragmentation, in addition to the HBS. An abrupt transition in the structure was observed at mid radius, with a third region developing from the mid radius to the pellet center. In this part of the pellet, metallic and grey phases with size between hundreds of nanometers and a few micrometers have formed at grain boundaries. The majority of fission gas has been released from the grain matrix and the original grains have polygonised, forming sub-grain domains separated by low-angle grain boundaries. No final explanation can be given for the polygonization occurring in the center, but on the basis of the irradiation history and the analysis of all the post irradiation examination (PIE) data, it is postulated that the polygonization within the original grains is an effect of dynamic recovery occurring at high temperature in the fuel center.
A fine pore-preserved deep neural network for porosity analytics of a high burnup U-10Zr metallic fuel
Abstract U-10 wt.% Zr (U-10Zr) metallic fuel is the leading candidate for next-generation sodium-cooled fast reactors. Porosity is one of the most important factors that impacts the performance of U-10Zr metallic fuel. The pores generated by the fission gas accumulation can lead to changes in thermal conductivity, fuel swelling, Fuel-Cladding Chemical Interaction (FCCI) and Fuel-Cladding Mechanical Interaction (FCMI). Therefore, it is crucial to accurately segment and analyze porosity to understand the U-10Zr fuel system to design future fast reactors. To address the above issues, we introduce a workflow to process and analyze multi-source Scanning Electron Microscope (SEM) image data. Moreover, an encoder-decoder-based, deep fully convolutional network is proposed to segment pores accurately by integrating the residual unit and the densely-connected units. Two SEM 250 × field of view image datasets with different formats are utilized to evaluate the new proposed model’s performance. Sufficient comparison results demonstrate that our method quantitatively outperforms two popular deep fully convolutional networks. Furthermore, we conducted experiments on the third SEM 2500 × field of view image dataset, and the transfer learning results show the potential capability to transfer the knowledge from low-magnification images to high-magnification images. Finally, we use a pre-trained network to predict the pores of SEM images in the whole cross-sectional image and obtain quantitative porosity analysis. Our findings will guide the SEM microscopy data collection efficiently, provide a mechanistic understanding of the U-10Zr fuel system and bridge the gap between advanced characterization to fuel system design.
Characterization of spent nuclear fuel canister surface roughness using surface replicating molds
In this study we present a replication method to determine surface roughness and to identify surface features when a sample cannot be directly analyzed by conventional techniques. As a demonstration, this method was applied to an unused spent nuclear fuel dry storage canister to determine variation across different surface features. In this study, an initial material down-selection was performed to determine the best molding agent and determined that non-modified Polytek PlatSil23-75 provided the most accurate representation of the surface while providing good usability. Other materials that were considered include Polygel Brush-On 35 polyurethane rubber (with and without Pol-ease 2300 release agent), Polytek PlatSil73-25 silicone rubber (with and without PlatThix thickening agent and Pol-ease 2300 release agent), and Express STD vinylpolysiloxane impression putty. The ability of PlatSil73-25 to create an accurate surface replica was evaluated by creating surface molds of several locations on surface roughness standards representing ISO grade surfaces N 3 , N 5 , N 7 , and N 8 . Overall, the molds were able to accurately reproduce the expected roughness average (R a ) values, but systematically over-estimated the peak-valley maximum roughness (R z ) values. Using a 3D printed sample cell, several locations across the stainless steel spent nuclear fuel canister were sampled to determine the surface roughness. These measurements provided information regarding variability in normal surface roughness across the canister as well as a detailed evaluation on specific surface features (e.g., welds, grind marks, etc.). The results of these measurements can support development of dry storage canister ageing management programs, as surface roughness is an important factor for surface dust deposition and accumulation. This method can be applied more broadly to different surfaces beyond stainless steel to provide rapid, accurate surface replications for analytical evaluation by profilometry.
Characterization of a Sulfonated Poly(Ionic Liquid) Block Copolymer as an Ionomer for Proton Exchange Membrane Fuel Cells using Rotating Disk Electrode
Ionic liquid (IL) additives to both traditional and advanced oxygen reduction reaction (ORR) electrocatalysts have yielded remarkable improvements in catalyst performance and durability. However, incorporating ILs or IL-modified catalysts into the electrodes of a proton exchange membrane fuel cell (PEMFC) membrane electrode assembly (MEA) has proven to be challenging. Sulfonated poly(ionic liquid) block copolymers (S-PILBCP) present an opportunity to incorporate IL functionality directly into the ionomer, orthogonal to protonic conductivity. Here, we use a rotating disc electrode (RDE) to characterize the interface between a S-PILBCP and Pt catalyst in comparison to Nafion. Catalyst thin films prepared with S-PILBCP show an 80% improvement in the ORR activity over those containing Nafion. Thin films of S-PILBCP also show a significantly reduced degree of poisoning sulfonate adsorption on a Pt(111) surface in comparison to Nafion. Furthermore, these half-cell results provide useful insights that help to highlight the source of the impact of the S-PILBCP on PEMFC MEA performance.
Material Characterization Report of EBR II Mark IV Fuel Element
The focus of this report is the characterization of an unirradiated as-built fuel element from the Experimental Breeder Reactor II (EBR-II) Mark IV driver fuel design. The fuel in this element is a metallic uranium-zirconium alloy, and the cladding material is HT9 stainless steel. Both the metallic fuel and cladding materials are characterized, including chemical composition, grain size, morphology, phase composition, precipitate composition, crystallography, density, and hardness.
Advanced Microscopy for Characterization of High Burnup Commercial UO 2 Fuel Before and After LOCA Testing
This report presents the results from the microstructural examination of high burnup UO 2 under pre- and post- loss of coolant accident (LOCA) conditions. The work in this report builds and expands upon work previously conducted on high burnup UO 2 fuel at Oak Ridge National Laboratory (ORNL). This work investigates the microstructural evolution that occurs during steady state irradiation of UO 2 , particularly in high burnup fuel. Several high burnup fuel samples were available from historic fuel shipments to ORNL. Microstructural characterization will aid in understanding why the fuel is susceptible to fuel fragmentation and support future work to investigate the formation mechanisms of certain features that form under irradiation. High burnup UO 2 microstructural data is also needed to improve constitutive models intended to predict high burnup fuel fragmentation (HBFF). This report summarizes the microstructural evaluation of these fuel samples to interpret and analyze high burnup fuel microstructures.
Thermal properties of HfN-MoW surrogate cermet fuel for nuclear thermal propulsion
Here, the thermal properties of MoW-HfN, a surrogate cermet for MoW-UN nuclear thermal propulsion fuel, were characterized over a wide range of elevated temperatures. Thermal diffusivity, coefficient of thermal expansion (CTE), and heat capacity were measured. Optical and scanning electron microscopy were performed to characterize the microstructure and draw structure–property correlations. The thermal diffusivity was obtained using the laser flash method. Diffusivity values ranged from about 0.18 cm 2 /s at 200°C to 0.15 cm 2 /s at 1800°C. The CTE was measured using push-rod dilatometry up to 1600°C, giving values between 6.0 and 9.0 μm/m. A scientific rationalization of the effective material properties is made using the rule-of-mixtures and other effective properties models.
End-of-Life Evaluation of Compressed Natural Gas Vehicle Fuel Tanks
This study evaluated the structural integrity of Type III and Type IV CNG fuel tanks from the Los Angeles (LA) County Metropolitan Transportation Authority to characterize the fuel tank conditions after experiencing a full service life of 15 years in transit bus application. The data produced provide insight about the condition of the CNG fuel tanks at the conclusion of their defined EOL and potential risks of continued operation of the CNG vehicle without replacement of the expired fuel tanks. In addition to physical testing performed on the fuel tanks, a nondestructive evaluation of modal acoustic emission (MAE) was utilized to assess the structural integrity of the tanks. The CNG fuel tanks were evaluated in their received condition and after experiencing artificial damage. The MAE results were then compared to visual inspection results of the procedures defined in the Compressed Gas Association’s (CGA’s) C-6.2 and C-6.4 standards (Compressed Gas Association 2013; 2012) to better understand the effectiveness of the visual inspection and potential safety risks of continued use of the tanks.
Effects of knock intensity measurement technique and fuel chemical composition on the research octane number (RON) of FACE gasolines: Part 2 – Effects of spark timing
The Research and Motor Octane Number (RON, MON) characterize a fuel’s knock resistance by rating the knock intensity of a sample fuel relative to that of Primary Reference Fuels (PRF) in a Cooperative Fuel Research (CFR) Engine. A fuel’s octane number is regulated to prevent damage from autoignition leading to knocking combustion in spark-ignition engines. The operational differences between the standard RON rating and modern engine operation are explored in a three-part publication series. The previous study focused on the effects of lambda and knock characterization. This second study primarily focuses on the effects of spark timing on RON determination. Following the findings from the first publication, the knock intensity was captured by the knockmeter and by the maximum amplitude of pressure oscillations (MAPO) at the lambda of peak knock intensity and stoichiometry. Knock-limited spark advance tests were conducted for a set of seven Fuels for Advanced Combustion Engines (FACE) from the Coordinating Research Council (CRC) with varying chemical composition, PRFs, and Toluene Standardization Fuels (TSFs). For retarded spark timings, pre-spark low-temperature heat release was found for low RON PRFs. Low RON PRFs also showed knocking characteristics before reaching the center of combustion suggesting that the use of knock-limited spark advance (KLSA) was preferred over the knock-limited combustion phasing. Primarily paraffinic fuels tended towards increased pressure oscillations while dominantly aromatic fuels experienced higher pressure rise rates. A MAPO-based KLSA correlated best to Octane Index at a negative K-factor suggesting beyond RON operation despite being at otherwise RON conditions. At stoichiometry, the MAPO-based KLSA did neither correlate to RON nor Octane Index. Finally, good agreement was found between KLSA-based effective RON from this study to the MAPO-based effective RON from the first study.
Oxygen Reduction at PtNi Alloys in Direct Methanol Fuel Cells—Electrode Development and Characterization
Catalyst layers made from novel catalysts must be fabricated in a way that the catalyst can function to its full potential. To characterize a PtNi alloy catalyst for use in the cathode of Direct Methanol Fuel Cells (DMFCs), the effects of the manufacturing technique, ink composition, layer composition, and catalyst loading were here studied in order to reach the maximum performance potential of the catalyst. For a more detailed understanding, beyond the DMFCs performance measurements, we look at the electrochemically active surface area of the catalyst and charge-transfer resistance, as well as the layer quality and ink properties, and relate them to the aspects stated above. As a result, we make catalyst layers with optimized parameters by ultrasonic spray coating that shows the high performance of the catalyst even when containing less Pt than commercial products. Using this approach, we can adjust the catalyst layers to the requirements of DMFCs, hydrogen fuel cells, or polymer electrolyte membrane electrolysis cells.
Automatic information extraction from neutron radiography imaging to estimate axial fuel expansion in $\mathrm{EBR-II}$
Approximately 130,000 metal fuel pins were irradiated in the Experimental Breeder Reactor II (EBR-II) during its 30 years of operation to develop and characterize existing and prospective fuels. For many of the metal fuel irradiation experiments, neutron radiography imaging was performed to characterize fuel behavior, like fuel swelling. However, due to the lack of technology or resources, many of the images have not been processed or were processed manually through visual examination. This paper represents first-attempt to develop an image processing algorithm capable of automatically extracting information regarding the degree of fuel swelling from neutron radiography imaging. The algorithm was applied to 120 images of three different metallic fuel pin compositions—U-10Zr, U-8Pu-10Zr, and U-19Pu-10Zr. The algorithm performs operations of image intensity adjustment, image binarization, region finding, and labeling to extract information about fuel swelling. The average growth for U-10Zr was found to be 8.49% with 95% Confidence Interval (CI) [8.33 –8.66%], for U-8Pu-10Zr — 7.50% with 95% CI [7.23 – 7.78%], and for U-19Pu-10Zr — 3.15%, with 95% CI [2.40 – 3.91%]. The results obtained by applying this automatic image processing algorithm are consistent with previously reported studies of the same types of fuels. The automatic image processing algorithm will be expanded to include thousands of available neutron radiography images and different types of fuels to investigate empirical dependencies of fuel swelling, which can be subsequently applied to advanced fuel modeling. Results from this study can later be compared to BISON simulations to further benchmark modeling efforts and develop assessment cases.
Qualification and Quantification of Porosity at the Top of the Fuel Pins in Metallic Fuels Using Image Processing
Approximately 130,000 metal fuel pins were irradiated in the Experimental Breeder Reactor II (EBR-II) during its 30 years of operation to develop and characterize existing and prospective fuels. For many of the metal fuel irradiation experiments, neutron radiography imaging was performed to characterize fuel behavior, such as fuel axial expansion. While several fuel expansion results obtained from neutron radiography imaging have been published, the analysis of neutron radiography for the purpose of describing statistical properties of porous matter formed on top of the fuel pins, also referred to as fluff in previous publications, is significantly less represented in the literature with just a single paper so far. This study aims to validate and augment results reported in previous publications using automated image processing. The paper describes the statistical properties of the porous matter in terms of nine parameters derived from radiography images and correlates those parameters with such fuel properties as composition, expansion, temperature, and burnup. The reported results are based on 1097 fuel pins of eight different fuel compositions. For three major fuel types, U-10Zr, U-8Pu-10Zr, and U-19Pu-10Zr, a clear negative correlation is found between the Pu content and five parameters describing the amount of porous matter generated. The parameters describing granularity properties, however, showed either negative correlation or nonlinear dependency from fuel composition. The parameters describing the amount showed a positive correlation with fuel axial expansion, while granularity parameters showed a negative correlation with axial expansion. The dependency on cladding temperature was found to be weak. A positive correlation is demonstrated for volume parameters and fuel burnup. In general, reported results confirm and validate findings published in previous studies using a much larger number of pins and automated processing techniques, which easily lend themselves to reproducibility, thus avoiding subjective bias.
Microstructure, Thermal, and Mechanical Properties Relationships in U and UZr Alloys (Final Report)
Uranium-zirconium (U-Zr) alloys are candidate fuel systems for transmutation based reactors that can be used to burn long-lived minor actinides and fission products in fast spectrum reactors. Metallic fuels have also been gaining more recent attention for applications as accident tolerant fuels, as well as for use in small modular reactors. This research focused on a “science-based” approach to capture the connections between U and U-Zr alloys’ three-dimensional (3-D) microstructure, thermal properties, and mechanical properties through closely coordinated experiments and modeling efforts from the unirradiated to the irradiated fuels. Advanced characterization and modeling techniques were used to understand irradiation-induced microstructural evolution and its direct impact on the thermal and mechanical properties of U and U-Zr fuel. Closely coordinated experiments and modeling were performed to provide crucial data that does not currently exist. Overall, this research spanned multiple length and time scales within the models and experiments. The scope of the research encompassed the understanding of the irradiation effects in U and various U-Zr alloys with particular attention paid to three task areas: (1) microstructural evolution, (2) in-situ/ex-situ thermal and mechanical properties, and (3) multiscale modeling connections to microstructure, thermal, and mechanical properties. This research resulted in (1) the 3-D characterization of neutron irradiated U-Zr fuel in multiple phase regions to better understand fission gas swelling and constituent redistribution, (2) development of a microstructural model linking thermal and mechanical properties via in situ Raman and nanoindentation, (3) and mesoscale phase field modeling was coupled with the AEH method in the MOOSE framework was used to calculate the effective thermal conductivities of U-Zr fuels consisting of α-U and δ-UZr 2 heterogeneous microstructures.
Data Mining – Image Analysis of Radiography for Zr Redistribution
The research effort described in this report represents a first attempt to investigate the radial redistribution of Zr in ternary fuel alloys U-xPu-10Zr (x = 0, 8, 19) irradiated in the in-reactor fuel experiments during the operation of the U.S. Department of Energy’s (DOE’s) Experimental Breeder Reactor II (EBR-II) at Idaho National Laboratory (INL) using methods of image processing on post-irradiation neutron radiographs. Approximately 130,000 metal fuel pins were irradiated in EBR-II during its 30 years of operation to develop and characterize existing and prospective fuels. For many of the metal fuel irradiation experiments, neutron radiography imaging was performed historically now allowing application of modern image analysis techniques to characterize fuel behavior, such as fuel swelling, fluff formation, and now, fuel alloy constituent redistribution. The redistribution of fuel components depends on the temperature field, radially, within the fuel. Specifically, Zr is expected to redistribute radially towards the center of the pin, as well as towards the outer zones. Currently, direct imaging of a pin cross-section through optical methods or scanning electron microscopy (SEM) is used to study the constituents’ redistribution, which is very time-consuming and can only be applied to a limited number of pins. An automated image processing technique allowing for the investigation of fuel radial redistribution zones would significantly accelerate data analysis. In general, if the fuel temperature is hot enough, three redistribution zones are expected, corresponding to the main fuel components (e.g., U, Pu, Zr). While more assessment will be performed in fiscal year (FY)-2023, it seems possible to differentiate the pins according to their fuel composition using image analysis techniques on neutron radiographs of metallic fuel pins based on the analysis to date.
Transmission electron microscopy study of a high burnup U-10Zr metallic fuel
To support the development of U-10 wt.% Zr (U-10Zr) metallic fuel for Gen IV sodium-cooled fast reactors, we analysed a solid, Na-bonded, U-10Zr (by weight percent) fuel cross section that was irradiated to a burnup of ~ 12.4 % at.% at the Fast Flux Test Facility (FFTF). Advanced characterization techniques, including site specific sample preparation by focused ion beam (FIB) and phase/chemical determination by transmission electron microscopy (TEM), were used to reveal the constituent redistribution of Zr, characterize the fuel phases and the secondary phases (such as solid fission products) present at the end of life. It is shown that the fuel pin cross section is divided into three major concentric zones: a Zr-rich central region, a Zr-lean intermediate region, and a Zr intermediate peripherical region. The phase characterization revealed that the irradiation environment enhanced the development and stabilization of phases not predicted by the standard equilibrium U-Zr phase diagrams. Comparing the current results with the ones from previous studies, it is reaffirmed that the irradiation temperature and the time spent in the reactor, rather than the fuel burnup, are the two factors that most influence the formation of redistribution zones and their extension along the fuel cross section. Various solid fission products precipitated inside the fission gas pores, such as lanthanides, ZrRu, BaTe, CsI, and Ba and Sr oxides. Here, this study provides unprecedented nanoscale understandings in the U-10Zr fuel system that may benefit fuel performance modelling and advanced fuel development.
Thermal Conductivity Degradation in High Burnup U-Pu-Zr Fuel
Recent advancements in the characterization of irradiated U-Pu-Zr fuels have revealed complexities that challenge existing understanding of constituent redistribution. Traditionally, models have proposed three concentric regions within the fuel, each characterized by distinctive phases and porosity. However, through detailed analysis of high burnup U-Pu-Zr, we discovered the presence of four distinct constituent redistribution regions. Particularly novel is the observation of significant Pu redistribution, a previously unreported phenomenon that necessitates a reevaluation of current models. This work aims to delve deeper into these findings, seeking to correlate mesoscale measurements of thermal diffusivity and respective thermal conductivity with the phases present in each redistribution region. To achieve this objective, we employed mesoscale thermoreflectance methods using the unique, Idaho National Laboratory (INL) developed, Thermal Conductivity Microscope (TCM) at INL’s Irradiated Materials Characterization Laboratory. The TCM employs two tightly focused lasers: one for heating to generate periodic thermal waves in the substrate, and another spatially separated probe laser to detect changes in the optical reflectivity of the gold-coated substrate resulting from thermal wave diffusion. We conducted several thermal diffusivity measurements within each region of constituent redistribution of a U-19Pu-10Zr fuel pin cross section irradiated to 11 at. % burnup. The TCM measurement positions strategically aligned with transmission electron microscopy (TEM) lift-out locations previously collected from the fuel sample. Complementary microstructural analysis techniques such as optical and scanning electron microscopy (OM/SEM), electron probe microanalysis for chemical compositions, and TEM-based selective area electron diffraction (SAED) analysis for crystallographic insights into each phase were also utilized. This comprehensive approach allowed us to correlate local thermal diffusivity data with microstructural characteristics, enabling the computation of local thermal conductivity at each position. The significance of this contribution lies in its pioneering use of the TCM for ternary fuel mesoscale examination, shedding light on the previously overlooked effects of Pu redistribution on local thermal conductivity. By informing current models capturing constituent redistribution and heat transfer, our findings pave the way for more accurate predictions of metallic fuel performance. Moreover, this work sets the stage for future comparisons with similar TCM examinations on U-19Pu-10Zr fuels at ultra-low burnup, facilitating a comprehensive understanding of thermal property changes across different burnup levels. Ultimately, our study not only enriches our understanding of the thermophysical properties of individual redistribution regions within U-Pu-Zr fuel but also offers valuable insights for the design and operational parameters of proposed next-generation fast reactors.