Results for “Optical Microscopy” — Page 20

NASA NTRSDate not supplied

Advanced TUFROC Thermal Protection System Evolution Under Re-entry like Conditions

Toughened Unipiece Fibrous Reinforced Oxidation-resistant Composite (TUFROC) and its successor, Advanced TUFROC, are state-of-the-art thermal protection systems (TPS) for high temperature reusable applications. Originally designed for use on the wing-leading edge of X-37B, TUFROC is an insulative tiled system consisting of a low-conductivity ceramic base, a carbonaceous cap, and multiple coatings for thermal performance. The improved Advanced TUFROC has demonstrated reusability up to 2900 °F and single use capabilities exceeding 3200 °F. This effort explores the evolution of Advanced TUFROC when exposed to re-entry like conditions via arc jet testing. Chemical reactions and constituent migration resulting from the aerothermal heating are known to occur and are studied in detail. Further, the interaction between the multiple constituents and layers will be discussed as this is believed to have a significant impact on the overall performance. Characterization includes structural analysis via optical microscopy, scanning electron microscopy and energy-dispersive x-ray spectroscopy.

Thermal protection system↗

NASA NTRS2023

Manufacturing and Mechanical Testing of TC1225/LM-PAEK and TC1200/PEEK Thermoplastic Composite Panels

Development of thermoplastic composites (TPCs) for aerospace structures is experiencing renewed enthusiasm attributed to the availability of rapid manufacturing technology, ease of joining through fusion welding processes, and the successful utilization of the material in flight critical structures. Semicrystalline thermoplastics such as polyether ether ketone (PEEK), polyether ketone ketone (PEKK), and polyphenylene sulfide (PPS) have been successfully demonstrated as thermoplastic skins, keel beams, and angle brackets for commercial aircraft. Composite specimens were fabricated from the Toray TC1225 and TC1200 unidirectional prepreg systems and tested to gain confidence with NASA in-house TPC processing as part of the Thermoplastics Development for Exploration Application (TDEA) project. TC1225 is a relatively new material system that uses T700GC fibers and low-melt polyaryl ether ketone (LM-PAEK) resin. TC1200 is the latest version of a material system that has been available for several decades with AS4 fibers and PEEK resin. Results for ultrasonic inspection, optical microscopy, acid digestion, and differential scanning calorimetry establish the quality of the panels. Mechanical test data for unnotched and notched laminate tension and compression as well as compression after impact provide data for equivalency assessment and support material selection in TDEA. Satisfactory equivalence of the TC1225 results and the National Center for Advanced Materials Performance (NCAMP) database was found. The results indicate high-quality manufacturing was achieved, and the resulting mechanical test data are in agreement with that in the literature.

Thermoplastic Composites↗

NASA NTRSDate not supplied

Impact Ice Adhesion at NASA Glenn: Current Experimental Methods and Supporting Measurements

When examining the literature on the adhesion strength of impact ice, there have been a wide range of methodologies tried to measure the required stresses to induce interfacial delamination. Utilizing the Icing Research Tunnel at the NASA Glenn Research Center to generate the impact ice required for this work, several different mechanical tests have been and are being developed to determine the stresses along the interface between ice and coupon. This set of tests includes the technical mature modified lap joint test which has been used to conduct ice adhesion studies through a wide sweep of icing conditions. To conduct in situ ice adhesion measurements inside of the Icing Research Tunnel, several new experiments are currently being developed to make ice adhesion measurements during and immediately after ice accretion. In addition to these experimental methods, several supporting measurement techniques have been developed to allow for a better understanding on the influence of icing cloud conditions on the mechanical behavior of impact ice. Digital image correlation has been successfully implemented to augment the data generated by the modified lap joint test with full field surface displacement and strain measurements which allow for insight into the deformation processes present during a test. Both optical microscopy of impact ice samples along with ice replication techniques have been used to study the grain structure of the impact ice. This has led to a deeper understanding of the results from the modified lap joint method and how the structure of impact ice changes as it is accreted during an icing spray. The freezing process of impact ice generated by supercooled liquid water is not a volume conserving process, which leads to the presence of residual strains along the interface between ice and substrate. These strains have been observed using both a simplified flat geometry and a representative airfoil. The data gathered by these experimental adhesion methods and supporting measurements allows for a comprehensive understanding on the behavior of impact ice which will be critical to the development of future ice shedding models.

Ice Adhesion↗

NASA NTRSDate not supplied

Impact Ice Adhesion at NASA Glenn: Current Experimental Methods and Supporting Measurements

When examining the literature on the adhesion strength of impact ice, there have been a wide range of methodologies tried to measure the required stresses to induce interfacial delamination. Utilizing the Icing Research Tunnel at the NASA Glenn Research Center to generate the impact ice required for this work, several different mechanical tests have been and are being developed to determine the stresses along the interface between ice and coupon. This set of tests includes the technical mature modified lap joint test which has been used to conduct ice adhesion studies through a wide sweep of icing conditions. To conduct in situ ice adhesion measurements inside of the Icing Research Tunnel, several new experiments are currently being developed to make ice adhesion measurements during and immediately after ice accretion. In addition to these experimental methods, several supporting measurement techniques have been developed to allow for a better understanding on the influence of icing cloud conditions on the mechanical behavior of impact ice. Digital image correlation has been successfully implemented to augment the data generated by the modified lap joint test with full field surface displacement and strain measurements which allow for insight into the deformation processes present during a test. Both optical microscopy of impact ice samples along with ice replication techniques have been used to study the grain structure of the impact ice. This has led to a deeper understanding of the results from the modified lap join method and how the structure of impact ice changes as it is accreted during an icing spray. The freezing process of impact ice generated by supercooled liquid water is not a volume conserving process, which leads to the presence of residual strains along the interface between ice and substrate. These strains have been observed using both a simplified flat geometry and a representative airfoil. The data gathered by these experimental adhesion methods and supporting measurements allows for a compressive understanding on the behavior of impact ice which will be critical to the development of future ice shedding models.

Ice Adhesion↗

NASA NTRS2023

Preliminary Examination of Returned Samples From Bennu Using Quantitative Particle Analysis in the Scanning Electron Microscope

The sample of regolith collected from asteroid Bennu by NASA’s OSIRIS-REx spacecraft will land in Utah on September 24, 2023. A 100-mg aliquot of fine Bennu dust adhering to the internal surfaces of the sample return capsule and associated hardware will be collected by curation staff during disassembly and analyzed immediately by members of the sample analysis team in a “Quick-Look” (Q-L) procedure. The Q-L objectives are (1) to provide images for release to the public to inform on the nature of the returned sample, and (2) to perform a reconnaissance investigation of the mineralogic characteristics of the returned material for science purposes. We will determine the minerals that occur in the dust, assess their diversity, and determine relative abundances at the >5% level using a combination of optical microscopy, Fourier-transform infrared spectroscopy, X-ray powder diffraction, and field-emission scanning electron microscopy (SEM). Here we describe the procedures and techniques developed for the Q-L analyses using analog samples analyzed by SEM equipped with energy dispersive X-ray spectroscopy (EDX). To test these techniques, we have applied them to several samples, including powders of the Murchison (Fig. 1) and Orgueil meteorites, as well as simulant samples prepared by the mission.

OSIRIS-REx↗

NASA NTRSDate not supplied

Ignition of Metals in Heated Supersonic Particle Impact with Inert Particulate

The conventional understanding of particle impact ignition characteristic elements relies on the following principles: 1) flammable particulate (except in the case of titanium and aluminum target materials); 2) gas velocity greater than 100 ft/s; 3) Impact point ranging from 45° to perpendicular to the path of the particle [1]; 4) flammable target material. To test assumptions about particulate flammability being necessary for particle impact ignition of less reactive target materials, such as Inconel 718, testing was performed with inert particulate. Supersonic particle impact testing was conducted with heated gas and 1500-µm sapphire particulate on various target materials: 304 stainless steel, wrought and selective laser melted Inconel 718, and Monel 400. Posttest characterization of impact craters was performed on each type of metallic target sample, including surface characterization performed by light optical microscopy and scanning electron microscopy with energy dispersive spectroscopy. Full consumption of the stainless steel and wrought Inconel 718 targets were noted to occur with sequential impacts. The results of testing will be discussed in detail, as well as recommendations for updating the understanding of the particle impact ignition mechanism.

Particle Impact↗

NASA NTRSDate not supplied

Orion Artemis I As Flown MMOD Analysis

Introduction The Lockheed Martin Orion spacecraft conducted the Artemis I flight around the Moon from November 16 through December 11, 2022. After the flight, an engineer from the NASA Johnson Space Center (JSC) Hypervelocity Impact Technology (HVIT) Group performed a Micrometeoroid and Orbital Debris MMOD analysis using the Bumper 3 risk assessment tool to predict the number of small impacts that would likely have occurred during the mission. Separately, a team from the same group inspected the Orion capsule for hypervelocity impact damage features. The results of the inspection were compared to those of the analysis to aid in improving the analysis, including the environment models. Scope of Work The spacecraft geometry model was created by Lockheed Martin during construction of the Artemis I Orion vehicle based on Computer Aided Design (CAD) models of the vehicle. New hypervelocity impact testing was performed to verify Ballistic Limit Equations (BLEs) used in the analysis to link impactor size and damage to the Thermal Protection System (TPS). The exact trajectory flown was recorded during the flight, including vehicle attitude. This data was used in conjunction with the ORDEM 3.2 and MEM 3 environment modeling tools to create models of particle flux impacting the spacecraft throughout the mission. Meteoroid shower forecast information was also included to account for additional particle flux associated with meteoroid showers. Inspection of the Orion capsule included the Backshell thermal tiles and the tape covering it, windows, fabric thermal materials, and small areas of other materials. Potential MMOD damage found was characterized using various techniques, including optical microscopy, computed tomography scanning, and X-ray spectroscopy. Findings The number of craters found in the Backshell tile, and their size distribution, matches well with the Bumper analysis prediction. Tape, window, and other material impacts recorded similarly align to Bumper analysis predictions. Conclusions and Recommendations This comparison of analysis with inspection of the hardware provides valuable insight into the MMOD environment and how accurately analysis tools assess the impact risk to spacecraft. As this was the first large, non-ablative returned surface from a lunar mission, this analysis extends the MMOD community’s insight beyond low Earth orbit into cis-lunar space.

MMOD↗

NASA NTRSDate not supplied

Orion Artemis I As Flown MMOD Analysis

Introduction The Lockheed Martin Orion spacecraft conducted the Artemis I flight around the Moon from November 16 through December 11, 2022. After the flight, an engineer from the NASA Johnson Space Center (JSC) Hypervelocity Impact Technology (HVIT) Group performed a Micrometeoroid and Orbital Debris MMOD analysis using the Bumper 3 risk assessment tool to predict the number of small impacts that would likely have occurred during the mission. Separately, a team from the same group inspected the Orion capsule for hypervelocity impact damage features. The results of the inspection were compared to those of the analysis to aid in improving the analysis, including the environment models. Scope of Work The spacecraft geometry model was created by Lockheed Martin during construction of the Artemis I Orion vehicle based on Computer Aided Design (CAD) models of the vehicle. New hypervelocity impact testing was performed to verify Ballistic Limit Equations (BLEs) used in the analysis to link impactor size and damage to the Thermal Protection System (TPS). The exact trajectory flown was recorded during the flight, including vehicle attitude. This data was used in conjunction with the ORDEM 3.2 and MEM 3 environment modeling tools to create models of particle flux impacting the spacecraft throughout the mission. Meteoroid shower forecast information was also included to account for additional particle flux associated with meteoroid showers. Inspection of the Orion capsule included the Backshell thermal tiles and the tape covering it, windows, fabric thermal materials, and small areas of other materials. Potential MMOD damage found was characterized using various techniques, including optical microscopy, computed tomography scanning, and X-ray spectroscopy. Findings The number of craters found in the Backshell tile, and their size distribution, matches well with the Bumper analysis prediction. Tape, window, and other material impacts recorded similarly align to Bumper analysis predictions. Conclusions and Recommendations This comparison of analysis with inspection of the hardware provides valuable insight into the MMOD environment and how accurately analysis tools assess the impact risk to spacecraft. As this was the first large, non-ablative returned surface from a lunar mission, this analysis extends the MMOD community’s insight beyond low Earth orbit into cis-lunar space.

MMOD↗

NASA NTRS2024

Offset-Stoichiometric Reflowable Composite Bonding Method with Adhesive for Mitigating Strict Faying Surface Tolerances

Inherent susceptibility of adhesive bonds to miniscule quantities of contamination can cause undetectable weakened bonds. For this reason, the Federal Aviation Administration (FAA) places strict regulations on adhesively bonded joints in primary aircraft structures. To meet certification requirements aircraft manufactures resort to redundant load paths in the form of fasteners which inherently add weight to the structure and increase manufacturing time. In prior work, a secondary bonding technique called AERoBOND was developed, which utilized off-stoichiometric epoxymatrix resins to facilitate reflow and diffusion of the resin within the joint interface during a secondary bonding/cure process, thus achieving a bond similar to a co-cured joint. However, the AERoBOND process required tight spatial tolerances between the two parts being joined. This study examined the utilization of conventional adhesive with the AERoBOND method to act as a filler in the joint line, effectively reducing the need for tight tolerances on the joining parts and serving as a flexible alternative for existing manufacturing processes. Ultrasonic inspection, optical microscopy, and ASTM International standard tests were performed to analyze the joints for defects and to quantify the mode-I and mode-II interlaminar fracture toughness and short beam strength of the proposed methodology with varying manufacturing parameters. The comprehensive results indicate that the AERoBOND+ method with and without surface preparation performs comparably to co-cured and conventional, adhesively bonded joints when secondary cured in an autoclave with 791 kPa of pressure. As an example, the AERoBOND+ panel without surface preparation bonded with 791 kPa of pressure (referred to as AB+3 throughout paper) had a mode-I fracture toughness (G Ic ) of 0.643 kJ/m 2 and a mode-II fracture toughness (G IIc ) of 4.000 kJ/m 2 in the non-precracked condition and 4.218 kJ/m 2 in the precracked condition at the adhesive-to-prepreg interface. These results were 96%, 142%, and 217%, respectively, of a co-cured baseline panel (referred to as C1 throughout paper).

Composites↗

NASA NTRS2024

Pull-off Behavior of Stitched Composite T-Joints

T-joints are key structural elements that connect opposing surfaces, thereby providing the load path between flat or curved panels (i.e., upper and lower wing skins) and transverse components (i.e., stiffeners). Due to the low interlaminar strength of polymer matrix composites and their geometrical discontinuities, these joints are vulnerable to pull-off loads. To address these issues, through-thickness reinforcements can be employed to enhance the interlaminar capability of these type of joints. In this study, T-joints were manufactured using through-thickness stitching in dry carbon preforms and cured using the vacuum-assisted resin transfer molding (VARTM) process. Stitched and unstitched T-joints were tested under pull-off loading conditions, and surface strain fields were obtained using a 3D digital image correlation system. The ultimate load, displacement, and absorbed energy of the stitched T-joints were greater than their unstitched counterparts by approximately 16%, 34%, and 58%, respectively. Failure mechanisms were identified by examining fracture surfaces using optical microscopy. Results demonstrate that through-thickness stitching significantly improves the damage tolerance of T-joints, which highlights the effectiveness of stitching to enhance the structural integrity of large aerospace components.

VARTM↗

NASA NTRSDate not supplied

Multiscale and Multifidelity Modeling of a 3D Woven Composite Thermal Protection System

Complex three-dimensional (3D) woven composites have been considered by multiple NASA projects in recent years as a means of offering improved mechanical and thermal performance over traditional laminated composite systems. Parallel efforts have focused on developing simulation capabilities for these systems, which have traditionally and heavily relied on experimental testing to evaluate composite performance. One system is the Heatshield for Extreme Entry Environment Technology (HEEET), which is being considered for the thermal protection system on reentry spacecraft. Optical microscopy was used to characterize the blended carbon and phenolic fiber tows. A section of HEEET insulation layer was imaged with high-resolution micro-computed tomography (microCT) and segmented to separate individual tows, porous matrix, and voids. These data were used to develop multiscale thermomechanical computational models within the NASA Multiscale Analysis Tool (NASMAT). Two NASMAT modeling approaches were considered to capture the details of the 3D woven architecture: a coarse model appropriate for inclusion in multiscale structural analyses and a high-fidelity model created by downsampling the microCT data. Both elastic and thermal properties were computed and compared. The feasibility and challenges associated with modeling complex, hybrid 3D woven composites were also addressed.

NASMAT↗

NASA NTRSDate not supplied

Evaluating Crystallinity in Thermoplastic composites

Polymer matrix composites (PMCs) offer many benefits for the aerospace industry due to their potential for weight reduction when compared to metal or ceramic based materials. Most PMCs currently in flight use thermoset matrices, however, thermoplastic resins are being explored as alternatives due to their ability to be remelted, which is of particular interest due to the potential for in-situ repair and manufacturing required in space. Most thermoplastic resins are semicrystalline polymers. The properties of semicrystalline thermoplastics are largely influenced by their crystallinity, which can vary due to many factors including thermal treatments, environmental conditions, and mechanical deformation. Monitoring the crystallinity of thermoplastic composites is key to ensuring these materials reliably meet the high demands required by space exploration. This talk discusses the use of multiple techniques such as Polarized Light Optical Microscopy and Fourier-Transform Infrared Spectroscopy to characterize the crystallinity in various thermoplastic composites, including carbon fiber reinforced PMCs and novel bio-based Martian and Lunar regolith composites designed for in-situ manufacturing. This work aims to provide the fundamental data necessary to understand the effects of crystallinity on thermoplastic PMCs, which is key to advancing their use in space applications.

Thermoplastics↗

NASA NTRSDate not supplied

Evaluating Crystallinity in Thermoplastic Composites for Aerospace Applications

Polymer matrix composites (PMCs) offer many benefits for the aerospace industry due to their potential for weight reduction when compared to metal or ceramic based materials. Most PMCs currently in flight use thermoset matrices, however, thermoplastic resins are being explored as alternatives due to their ability to be remelted, which is of particular interest due to the potential for in-situ repair and faster production. Most thermoplastic resins are semicrystalline polymers. The properties of semicrystalline thermoplastics are directly influenced by their crystallinity, which can vary due to many factors including thermal treatments, environmental conditions, and mechanical deformation. Within thermoplastic PMC parts, crystallinity gradients can arise due to variations in part geometry, across part thicknesses, and along bonded joints. Monitoring the crystallinity of thermoplastic composites is key to ensuring these materials meet the high demands required for aerospace. Several different analytical techniques exist that can be used to characterize the bulk crystallinity of thermoplastic materials. However, many existing methods lack the specificity required to identify the subtle variations in crystallinity that may play a significant role in the performance and durability of PMC parts. Because of this, a significant amount of work is still required to fully characterize and understand the crystallinity profiles of thermoplastic PMCs and the resulting impact to material properties. This talk discusses the use of multiple techniques such as Differential Scanning Calorimetry, Polarized Light Optical Microscopy, and Fourier-Transform Infrared Spectroscopy to characterize the crystallinity in carbon fiber/thermoplastic composites. Samples of different crystallinity profiles were manufactured using various cooling procedures. This work aims to provide the fundamental data necessary to understand the effects of crystallinity on thermoplastic PMCs, which is key to advancing their use in aerospace applications.

Thermoplastics↗

DOE OSTI2024

Pre-Transient Characterization of Historic EBR-II Pins for Transient Testing

Current interest in sodium-cooled fast reactor (SFR) designs, such as TerraPower’s Natrium Reactor, has highlighted the need for advanced reactor fuel technology development. Modern U-Zr and U- Pu-Zr pin designs are primary candidates to fuel SFRs and boast high fuel utilization capacity, increased fuel-cladding compatibility, and improved safety through inherent feedback mechanisms. Despite over 60 years of metallic fuel irradiation, uncertainties exist in the performance of the fuel system, particularly under transient overpower (TOP) and loss of flow (LOF) scenarios. Throughout historical testing within the Experimental Breeder Reactor II (EBR-II) and the Fast Flux Test Facility (FFTF), fuel behavior has demonstrated benign response to transient reactor conditions; however, accurate predictions of failure thresholds to inform operational limitations rely heavily on fuel composition, burnup, and irradiation history. In expanding TOP and LOF testing, the Transient Heat sink Overpower Response (THOR) Capsule will be used to test modern fuel technologies in a static sodium environment in the Transient Reactor Test (TREAT) Facility. The THOR capsule is highly instrumented and will provide time-dependent thermal behavior of SFR fuel pins subjected to accident conditions within TREAT. The THOR-Metallic (THOR- M) campaign aims to validate and expand historical TOP and LOF testing on high burnup U-Zr and U-Pu- Zr fuel alloys previously irradiated in EBR-II by running the rods to failure. This contribution focuses primarily on the pre-transient engineering-scale destructive and non- destructive characterization that has been conducted on both the test and sibling pins used for the TOP and LOF tests. All pins underwent visual examination, neutron radiography, element contact profilometry, and precise gamma scan. The sibling pins used for each test were further analyzed using gas assay, sampling, and recharge analysis (GASR), and optical microscopy. The results from each technique confirmed that the fuel pins were intact and devoid of any atypical developments when compared to historical data. Additionally, the analyzed measurements establish a baseline for comparison to post-transient analysis. Key fuel behaviors quanitifed include axial elongation of the fuel column, diametral strain of the pin, patterns in fluff structure geometry, changes in axial isotope distribution, evolution of constituent redistribution, porosity, and fission gas release. The pre-transient measurements and changes attributed to transient behavior from post-transient measurement will be compared to historical data to capture the behavioral dependence on composition, burnup, and irradiation history. Results from this work advance the initiatives of the THOR-M campaign, which aid in informing fuel performance models and establishing safety criteria for SFR operational limits. The novel combination of test environment, in-situ instrumentation, and comprehensive suite of characterization methods provides greater understanding of transient fuel behavior. Overall, information on the time and condition of pin failure for high burnup U-Pu-Zr will greatly expand the limited existing TOP and LOF test data.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Pre-Transient Characterization of Historic EBR-II Pins for Transient Testing

Current interest in sodium-cooled fast reactor (SFR) designs, such as TerraPower’s Natrium Reactor, has highlighted the need for advanced reactor fuel technology development. Modern U-Zr and U- Pu-Zr pin designs are primary candidates to fuel SFRs and boast high fuel utilization capacity, increased fuel-cladding compatibility, and improved safety through inherent feedback mechanisms. Despite over 60 years of metallic fuel irradiation, uncertainties exist in the performance of the fuel system, particularly under transient overpower (TOP) and loss of flow (LOF) scenarios. Throughout historical testing within the Experimental Breeder Reactor II (EBR-II) and the Fast Flux Test Facility (FFTF), fuel behavior has demonstrated benign response to transient reactor conditions; however, accurate predictions of failure thresholds to inform operational limitations rely heavily on fuel composition, burnup, and irradiation history. In expanding TOP and LOF testing, the Transient Heat sink Overpower Response (THOR) Capsule will be used to test modern fuel technologies in a static sodium environment in the Transient Reactor Test (TREAT) Facility. The THOR capsule is highly instrumented and will provide time-dependent thermal behavior of SFR fuel pins subjected to accident conditions within TREAT. The THOR-Metallic (THOR- M) campaign aims to validate and expand historical TOP and LOF testing on high burnup U-Zr and U-Pu- Zr fuel alloys previously irradiated in EBR-II by running the rods to failure. This contribution focuses primarily on the pre-transient engineering-scale destructive and non- destructive characterization that has been conducted on both the test and sibling pins used for the TOP and LOF tests. All pins underwent visual examination, neutron radiography, element contact profilometry, and precise gamma scan. The sibling pins used for each test were further analyzed using gas assay, sampling, and recharge analysis (GASR), and optical microscopy. The results from each technique confirmed that the fuel pins were intact and devoid of any atypical developments when compared to historical data. Additionally, the analyzed measurements establish a baseline for comparison to post-transient analysis. Key fuel behaviors quanitifed include axial elongation of the fuel column, diametral strain of the pin, patterns in fluff structure geometry, changes in axial isotope distribution, evolution of constituent redistribution, porosity, and fission gas release. The pre-transient measurements and changes attributed to transient behavior from post-transient measurement will be compared to historical data to capture the behavioral dependence on composition, burnup, and irradiation history. Results from this work advance the initiatives of the THOR-M campaign, which aid in informing fuel performance models and establishing safety criteria for SFR operational limits. The novel combination of test environment, in-situ instrumentation, and comprehensive suite of characterization methods provides greater understanding of transient fuel behavior. Overall, information on the time and condition of pin failure for high burnup U-Pu-Zr will greatly expand the limited existing TOP and LOF test data.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Corrosion Testing Of Additively Manufactured Stainless Steel 316H In Molten Salt Environments

The development of a new ASTM standard for evaluating the corrosion resistance of additive manufactured (AM) stainless steel (SS) 316H in chloride molten salts is critical for the use of these materials in extreme environments such as molten salt reactors (MSRs). This report pertains to a work package of the Advaned Materials and Manufacturing Technologies (AMMT) developing a systematic methodology to link changes in AM fabrication parameters, namely surface finishing, porosity, microstructure, and chemical heterogeneity, to corrosion performance in NaCl-MgCl2 salt, a proposed secondary coolant for MSRs. During Fiscal Year 2024, Idaho National Laboratory investigators in the AMMT program, utilized SS316H bars, fabricated with laser bed powder fusion at Los Alamos National Laboratory, to establish and optimize the workflow for evaluating these process-to-performance relationships. Standard practices for specimen preparation were established using these specimens, with particular focus on descaling and sectioning methods that align with ASTM guidelines. A comprehensive experimental design for static corrosion testing was developed, with pre- and post-exposure analysis utilizing optical microscopy and scanning electron microscopy. So far standard descaling techniques were optimized, one static corrosion test was conducted on the LANL AM SS316H specimens, and pre- and post-corrosion practices were established. In addition, the work package yielded a review paper on corrosion testing gaps for AM materials in nuclear applications and submitted a proposal for a rapid-turnaround experiment to the Nuclear Science User Facilities Program to investigate the combined effects of proton irradiation and corrosion on AM SS316H. This work package establishes a foundation for evaluating processing-to-performance relationships for AM SS316H in harsh conditions, contributing to the safe and efficient design of components for next-generation nuclear reactors. The creation of a standardized methodology and the generation of relevant publications and future research pathways represent significant strides towards integrating AM materials into critical applications where corrosion resistance is paramount.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Examining Constituent Redistribution in U-19Pu-10Zr Fuel as it Evolves with Local Burnup

While constituent redistribution is a known irradiation behavior in U-Pu-Zr fuel, new data have shown it is more complex than our current understanding and predictive capabilities. The size and composition of redistributed rings evolve as a function of pin composition, burnup, geometry, and irradiation temperature. In this work, we extract microstructural information from optical microscopy conducted on U-19Pu-10Zr pins (irradiated between 1.9 at. % and 11.6 at. % peak burnup). Both manual image analysis techniques and machine learning-assisted segmentation are used to quantify the thicknesses of the cladding, fuel-cladding interaction layers, and rings of fuel constituent redistribution in addition to pore distribution. These microstructural features and individual redistributed regions affect local thermomechanical properties, and identifying the relationship between burnup and constituent redistribution will improve accurate prediction of advanced reactor fuel performance.

Constituent Redistribution↗

DOE OSTI2025

Assessing High Burnup U-19Pu-10Zr Fuel Performance against Historical and Modeled Behavior

Advancing the deployment of sodium-cooled fast reactors (SFRs) requires thorough testing of metallic fuel pins under accident conditions to establish safe operational limits of high burnup fuel. To conduct transient testing, a comprehensive understanding of steady-state fuel behavior obtained through both experimental characterization and accurate predictive capabilities is needed. This study comparatively assesses the steady-state irradiation performance of two high burnup U-19Pu-10Zr fuel pins, DP-36 and DP-40, irradiated under prototypic fast reactor conditions in preparation for planned safety testing at the Transient Reactor Test Facility. Since DP-40 was designated for use in the test and DP-36 serves as its sibling pin, non-destructive, engineering-scale post-irradiation examinations (PIE) were conducted on both pins while destructive examinations were performed exclusively on DP-36. The results were then assessed against historical performance data from similar fuel pins irradiated in the Experimental Breeder Reactor-II. Additionally, the steady-state irradiation of each pin was modeled using the BISON fuel performance code to assess the accuracy of current modeling capabilities in predicting the baseline irradiation behavior. Non-destructive examinations included neutron radiography to measure fuel column elongation, gamma scanning to verify pin integrity and fission product migration, and profilometry to assess dimensional changes. Benchmarking against existing PIE data revealed consistent patterns in axial fuel column growth and cladding diametral strain, though both pins exhibited longer low-density “fluff” structures, which can have implications for core reactivity and source term calculations. Destructive examinations on DP-36 included fission gas release analysis and sectioning for optical microscopy, which showed more complex constituent redistribution patterns than the traditionally accepted 3-ring model. The axial evolution of fractional areas and porosities of each of the redistributed zones were quantified and presented. Modeling comparisons showed agreement in fractional fission gas release but consistently overestimated axial and radial swelling and disagreed with measured axial porosity patterns. These conservative overpredictions suggested that the pins would appear closer to failure or operational limits at the start of transient tests, potentially leading to higher strain accumulation during the transient. While conservative estimates provide safety margins, they can negatively impact fuel economics. A review of the swelling models identified areas for improvement in the gaseous swelling, solid swelling, and fuel hot-pressing models when applied to ternary fuel. The results of this study highlight the critical importance of conducting pre-test characterization on both test and sibling pins to accurately capture steady-state fuel behavior, providing a precise baseline for post-test evaluations and essential inputs for transient modeling of the planned experiments. The analysis also revealed significant data gaps that require further investigation to enhance the understanding and prediction of fuel swelling and pore dynamics. Collecting comprehensive data across different irradiation conditions, burnup levels, and fuel compositions are essential for refining existing models and developing mechanistic models for both binary and ternary metallic fuels, ultimately improving the integration of modeling and experimental approaches in accident testing.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗