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DOE OSTI2023

Endowing Polythioester Vitrimer with Intrinsic Crystallinity and Chemical Recyclability

Abstract Technologically important thermosets face a long‐standing end‐of‐life (EoL) problem of non‐reprocessability, a more sustainable solution of which has resolved to nascent vitrimers that can merge the robust material properties of thermosets and the reprocessability of thermoplastics. However, the lifecycle of vitrimers is still finite, as they often suffer from significant deterioration of mechanical performance following multiple reprocessing cycles, analogous to mechanical recycling, and they often show undesired creep under working conditions. To address these two key limitations, we have developed a cross‐linked semi‐crystalline polythioester with both dynamic covalent bonds and intrinsic crystallinity and chemical recyclability, affording a vitrimeric system that exhibits not only reprocessability and crystallinity‐restricted creep but also complete chemical recyclability to initial monomer by catalyzed depolymerization in solution or bulk. Therefore, reported herein is an “infinite” vitrimer system that is empowered with a facile closed‐loop EoL option once serial reprocessing deteriorates performance and the material can no longer meet the application requirements. Specifically, the polythioester vitrimer was constructed by copolymerization of a bicyclic thioester with a bis‐dithiolane, producing dynamically cross‐linked polythioesters with excellent property tunability, from amorphous to semi‐crystalline states and melting transition temperatures from 91 to 178 °C.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1993

An overview of the Evaluation of Oxygen Interaction with Materials-third phase (EOIM-3) experiment: Space Shuttle Mission 46

The interaction of the atomic oxygen (AO) component of the low earth orbit (LEO) environment with spacecraft materials has been the subject of several flight experiments over the past 11 years. The effect of AO interactions with materials has been shown to be significant for long-lived spacecraft such as Space Station Freedom and has resulted in materials changes for externally exposed surfaces. The data obtained from previous flight experiments, augmented by limited ground-based evaluation, have been used to evaluate hardware performance and select materials. Questions pertaining to the accuracy of this data base remain, resulting from the use of long-term ambient density models to estimate the O-atom fluxes and fluences needed to calculate materials reactivity in short-term flight experiments. The EOIM-3 flight experiment was designed to produce benchmark AO reactivity data and was carried out during STS-46. Ambient density measurements were made with a quadrupole mass spectrometer which was calibrated for AO measurements in a unique ground-based test facility. The combination of these data with the predictions of ambient density models allows an assessment of the accuracy of measured reaction rates on a wide variety of materials, many of which had never been tested in LEO before. The mass spectrometer is also used to obtain a better definition of the local neutral and plasma environments resulting from interaction of the ambient atmosphere with various spacecraft surfaces. In addition, the EOIM-3 experiment was designed to produce information on the effects of temperature, mechanical stress, and solar exposure on the AO reactivity of a wide range of materials. An overview of the EOIM-3 methods and results are presented.

Leger, Lubert J.↗

NASA NTRS1996

Novel Composites for Wing and Fuselage Applications: Novel Wing Design Concepts - Task 1

Design trade studies were conducted to arrive at advanced wing designs that integrated new material forms with innovative structural concepts and cost-effective fabrication methods. A representative spar was selected for design, fabrication, and test to validate the predicted performance. Textile processes, such as knitting, weaving and stitching, were used to produce fiber preforms that were later fabricated into composite span through epoxy Resin Transfer Molding (RTM), Resin Film Infusion (RFI), and consolidation of commingled thermoplastic and graphite tows. The target design ultimate strain level for these innovative structural design concepts was 6000 mu in. per in. The spars were subjected to four-point beam bending to validate their structural performance. The various material form /processing combination Y-spars were rated for their structural efficiency and acquisition cost. The acquisition cost elements were material, tooling, and labor.

Suarez, J. A.↗

DOE OSTI2024

Incorporating A Risk-Informed, Performance-Based Concept into Nuclear Fuel and Materials Development for Advanced Reactors

The NRC’s regulatory concept for advanced reactors under 10 CFR Part 53 promotes the use of an RIPB concept. RIPB is usually referenced as a general, overarching concept. This paper is focused on how to, and if it would be worthy to, incorporate an RIPB concept into nuclear fuel and materials development for advanced reactors. This paper proposes three potential RIPB applications for nuclear fuel and materials development, including RIPB test matrix development, RIPB test matrix reduction, and RIPB design optimization. This paper discusses the projected benefits from incorporating RIPB in reducing development timeline, cost, and regulatory risk.

99 GENERAL AND MISCELLANEOUS↗

DOE OSTI2025

Manipulation of intramolecular hydrogen bonds in conjugated pseudoladder polymer for semiconductivity and solution-processability

The conformational coplanarity and local rigidity of π-conjugated backbones are critical for the semiconducting performance of organic electronic materials. The conformational coplanarity and local rigidity of π-conjugated backbones are critical for the semiconducting performance of organic electronic materials. While fusing the aromatic system into a ladder-type structure effectively enhances these properties, it also often results in poor solution processability and hence limits their transition to device application. To address this challenge, an intramolecularly hydrogen-bonded pseudoladder polymer (HPLP) system based on alternating hydrogen bond donating benzobisimidazole (BBI) and hydrogen bond accepting benzodifuran (BDF) units, is designed and synthesized. A Boc-protected precursor of HPLP allows for feasible solution processing of the polymer into thin films. Subsequently, in situ thermal Boc-deprotection generates the HPLP polymer, in which intramolecular hydrogen bonds form between each pair of neighboring repeating units, inducing coplanarity and rigidity throughout the entire backbone. This process is accompanied by a significant red-shift of the absorption spectrum, reduced bandgap, and enhanced rigidity, as confirmed by NMR, UV-Vis, and density functional theory analyses. HPLP films exhibit a three-order-of-magnitude enhancement in charge carrier mobility compared to the Boc-protected precursor and demonstrate excellent solvent resistance in organic thin-film transistors.

Miranda, Octavio↗

NASA NTRSDate not supplied

Developments on Reusable TPS Materials Based Upon Shuttle Tile

The insulating tiles used on the Space Shuttler Orbiter, principally AETB (Alumina Enhanced Thermal Barrier), have been seen by new vehicle developers in the aerospace industry as a fast-track approach for fielding a reusable thermal protection system (TPS) given the extensive use by both the Orbiter program and the current Orion vehicle. NASA has, and is, supporting the industry through technology transfer and commercial crew and payloads programs. However, the reusable TPS community is rapidly encountering challenges rooted in Orbiter’s and Orion’s dependence on legacy material and processes. With the aim of alleviating these issues, improving availability of reusable TPS, and strengthening the nation’s space economy, ongoing efforts at NASA Ames have focused on understanding process-property relationships in AETB as well as novel materials and technologies for reusable TPS. The first portion of this talk will address the effects of raw materials and processing conditions on the properties of AETB-8, including the raw materials used, mixing and casting parameters, and thermal history. Understanding these relationships, and how they extend to aerothermal performance, is instrumental in alleviating supply chain constraints and improving manufacturability. The implications of these finding on development of novel TPS materials and systems will be discussed. AETB will likely continue to fill a niche of relatively high performance with associated costs. There exists, therefore, a gap in developed reusable TPS for a lower cost, moderate performing material system. The later portion of this talk will touch on current development efforts at Ames focusing on reduced cost and ease of integration, which are being pursued in addition to AETB and higher performing systems. In addition to summarizing these efforts, an outlook for these projects and collaborations will be given.

Peter Edward Marshall↗

NASA NTRSDate not supplied

Developments on Reusable TPS Materials Based Upon Shuttle Tile

Thermal Protection Systems↗

DOE OSTI2021

Material Interactions in Severe Accidents – Benchmarking the MELCOR V2.2 Eutectics Model for a BWR-3 Mark-I Station Blackout: Part II – Uncertainty Analysis

Single case comparisons between severe accident simulations can provide detailed insights into severe accident model behavior, however, they cannot offer insights into model uncertainty, sensitivity to uncertain parameters, or underlying model biases.Here in this analysis, the single case benchmark comparison of the MELCOR material interaction models for a station blackout (SBO) scenario of a boiling water reactor (BWR) using representative Fukushima Daiichi Unit 1 boundary conditions is expanded to include an uncertainty analysis. As part of this uncertainty analysis, 1200 simulations are performed for each material interaction model (2400 total), with random sampling of 14 uncertain MELCOR input parameters. Input parameters are selected for their impact on models representing core degradation processes. These include candling, fuel rod failure, debris quenching and dryout. The analysis performed here is not a traditional “best-estimate” uncertainty analysis that uses best-estimate parameters or identifies best-estimate figure of merit distributions. Instead, it is an exploratory uncertainty analysis that identifies and interrogates underlying model form biases of the two material interaction models (eutectics and interactive materials models). Uniform distributions are applied to all uncertain parameters to ensure coverage of the model parameter uncertainty space. Key findings from this study include underlying model form biases exhibited by material interaction models, and notable differences in accident progression outcomes between the material interaction models. This uncertainty study extends and confirms the conclusions from the first part of this study, which compared the impact of material interaction modeling on simulation of a short-term station blackout scenario with representative Fukushima Daiichi Unit I boundary conditions. In particular, this study confirms that the eutectics model generally exhibits accelerated degradation and failure of fuel components, the core plate, and the lower head. The eutectics model also has a tendency to exhibit a greater degree of core degradation, greater debris mass formation, and larger debris mass ejection. Finally, the eutectics model exhibits higher maximum temperatures for fuel, cladding, particulate debris, oxidic molten pool, and metallic molten pool components than the interactive materials model; interactive materials model simulations exhibit a soft “limitation” on maximum temperatures that is related to the temperature at which material relocation occurs.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2021

Interfacial thermal transport in spin caloritronic material systems

Interfaces often govern the thermal performance of nanoscale devices and nanostructured materials. As a result, accurate knowledge of thermal interface conductance is necessary to model the temperature response of nanoscale devices or nanostructured materials to heating. Here, we report the thermal boundary conductance between metals and insulators that are commonly used in spin-caloritronic experiments. We use time-domain thermoreflectance to measure the interface conductance between metals such as Au, Pt, Ta, Cu, and Al with garnet and oxide substrates, e.g., NiO, yttrium iron garnet (YIG), thulium iron garnet (TmIG), Cr 2 O 3 , and sapphire. We find that, at room temperature, the interface conductance in these types of material systems range from 50 to 300 MW m –2 K –1 . Furthermore, we also measure the interface conductance between Pt and YIG at temperatures between 80 and 350 K. At room temperature, the interface conductance of Pt/YIG is 170 MW m –2 K –1 and the Kapitza length is ~40 nm. A Kapitza length of 40 nm means that, in the presence of a steady-state heat current, the temperature drop at the Pt/YIG interface is equal to the temperature drop across a 40-nm-thick layer of YIG. At 80 K, the interface conductance of Pt/YIG is 60 MW m –2 K –1 , corresponding to a Kapitza length of ~300 nm.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Ta Based Damascene Resonators

Transmon qubits have become a leading technology in quantum information science (QIS), with fabrication techniques widely accessible. Historically, devices were predominantly made from aluminum (Al) and niobium (Nb), but state-of-the-art transmons now use tantalum (Ta) achieving coherence times up to and exceeding 0.5 milliseconds [1-3]. The differentiation in performance between Ta and Nb-based devices is attributed to the surface oxidation states affecting Two-Level-System (TLS) noise. One approach to quickly evaluating material and device performance consists of fabricating only the readout resonator of a qubit and evaluating the quality factor which is the strategy employed in this project. Our research focuses on Ta coplanar waveguide (CPW) resonators fabricated using a damascene technique producing pristine metal structures within silicon substrates. This approach increases the dielectric substrate's participation ratio while keeping device edges oxide-free due to entrenchment. This collaborative effort, involving Pacific Northwest National Laboratory (PNNL), NY CREATES/SUNY Poly, and Brookhaven National Laboratory (BNL), has resulted in resonators with Q factors as high as 104 at low power. Ongoing studies aim to further understand and improve device performance by systematic analysis of oxygen trapped between device layers during processing. This research showcases the potential for significant improvements in superconducting qubit performance via the damascene process, heralding new possibilities for the advancement of scalable QIS technology.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2022

Recent Advances and Prospects in Design of Hydrogen Permeation Barrier Materials for Energy Applications—A Review

The hydrogen infrastructure involves hydrogen production, storage and delivery for utilization with clean energy applications. Hydrogen ingress into structural materials can be detrimental due to corrosion and embrittlement. To enable safe operation in applications that need protection from hydrogen isotopes, this review article summarizes most recent advances in materials design and performance characterization of barrier coatings to prevent hydrogen isotopes’ absorption ingress and permeation. Barriers are crucial to prevent hydride formation and unwanted hydrogen effects to increase safety, materials’ lifetime and reduce cost for applications within nuclear and renewable energy. The coating may be applied on a material that requires protection from hydrogen pick-up, transport and hydride formation in hydrogen storage containers, in pipelines, spent nuclear fuel storage or in nuclear reactors. While existing, commercial coatings that have been much in use may be satisfactory for various applications, it is desirable to evaluate whether alternative coating concepts can provide a greater resistance to hydrogen isotope permeation along with other improved properties, such as mechanical strength and thermal resistance. The information presented here is focusing on recent findings within the past 5–7 years of promising hydrogen barriers including oxides, nitrides, carbon, carbide, MAX-phases and metals and their mechanical strength, hydrogen pick-up, radiation resistance and coating manufacturing techniques. A brief introduction to hydrogen permeation is provided. Knowledge gaps were identified to provide guidance for material’s research prospects.

08 HYDROGEN↗

NASA NTRSDate not supplied

3D Woven Mid-Density Carbon Phenolic (3MDCP) Thermal Protection System Development

3-Dimensionally Woven, Mid-Density, Carbon Phenolic (3MDCP) Thermal Protection System (TPS) material is derived from the dual layer 3D woven Heatshield for Extreme Entry Environment Technology (HEEET) material. The baseline 3MDCP design is a single piece thermal protection system that avoids the manufacturing and certification challenges associated with a tiled configuration. 3MDCP is targeted for very aggressive entry environments such as high-speed sample return missions to Earth and missions to Saturn, Venus and the ice giants. A 3MDCP heatshield begins as a flat woven preform that is formed to a given heatshield shape and then infused with phenolic resin. NASA Ames, in collaboration with TEAM Inc. (weaving) and Fiber Materials Inc. (both Spirit AeroSystems Companies) have been developing and demonstrating the manufacturing processes to fabricate a 3MDCP heatshield at a diameter of 1.25 meters. The process of forming the flat woven preform into the final heatshield shape, a sphere-cone geometry, involves local movement of the yarns in the weave. This results in a single piece heatshield with continuous fibers, albeit with property variations between different regions on the heatshield. This presentation will provide a high-level status of 3MDCP development. This will include an overview of the manufacturing processes, with an emphasis on the impact of forming on fiber orientation, material properties and performance. The presentation will layout the plan for testing to assess the impact of forming on properties and review preliminary data comparing properties of flat to formed materials.

Thermal Protection System↗

NASA NTRS2017

Arc Jet Test and Analysis of Asbestos Free Solid Rocket Motor Nozzle Dome Ablative Materials

Asbestos free solid motor internal insulation samples were recently tested at the MSFC Hyperthermal Arc Jet Facility. Objectives of the test were to gather data for solid rocket motor analog characterization of ablative and in-depth thermal performance of rubber materials subject to high enthalpy/pressure flow conditions. Tests were conducted over a range of convective heat fluxes for both inert and chemically reactive sub-sonic free stream gas flow. Active instrumentation included use of total calorimeters, in-depth thermocouples, and a surface pyrometer for in-situ surface temperature measurement. Post-test sample forensics involved determination of eroded depth, charred depth, total sample weight loss, and documentation of the general condition of the eroded profile. A complete Charring Material Ablator (CMA) style aero thermal analysis was conducted for the test matrix and results compared to the measured data. In general, comparisons were possible for a number of the cases and the results show a limited predictive ability to model accurately both the ablative response and the in-depth temperature profiles. Lessons learned and modeling recommendations are made regarding future testing and modeling improvements that will increase understanding of the basic chemistry/physics associated with the complicated material ablation process of rubber materials.

Clayton, J. Louie↗

DOE OSTI2024

Femto-second Laser’s Enabling New Length Scale Fabrications for Rapid Post Irradiation Examination of Materials: Concluding LDRD Project Poster

Mechanical testing campaigns are required to qualify materials for advanced reactor conditions, yet economical and safety limitations restrict the number of standardized mechanical tests that can be performed. Reducing the size of the sample is one approach to addressing these challenges and to accelerating testing. Previous research has shown that smaller mechanical test samples produce higher yield and ultimate stress values compared to values measured from standard sample sizes: the “smaller is stronger” effect. Specimens used in accelerated material testing campaigns must reflect bulk material performance to enable engineering scale material property measurement. The objective of this research project was to determine if engineering scale mechanical behavior—the yield stress—could be measured with micro-tensile test samples smaller than traditional standard testing geometries. The relationship between yield stress and sample size was explored with two different nuclear-relevant structural materials: Zircaloy-4 and tungsten. Mechanical testing of both metals demonstrated decreasing yield stress values with increasing sample gauge size across three different sizes. Yield stress values from the largest gauge size, fabricated with a femto-second laser ablation system, approach bulk material yield stress values reported in published literature. Preliminary analysis of the tungsten samples indicates the yield stress value depends on the grain characteristics within the gauge section, in addition to the gauge size. Accompanying modeling efforts, including response surface generation and crystal plasticity approaches, further demonstrated that the size of the sample gauge section alone cannot explain the change in yield stress values.

36 MATERIALS SCIENCE↗

DOE OSTI2023

BISON validation to in situ cladding burst test and high-burnup LOCA experiments

The process for developing and qualifying nuclear fuels for commercial nuclear application requires fundamental material development, characterization, and design; out-of-pile testing on unirradiated materials; integral fuel rod irradiations, testing, and postirradiation examinations; and transient analyses. The historical approach depends on the generation of large empirical datasets and series of integral fuel rod irradiations, and this approach ultimately takes ~20 years—or sometimes longer—to acquire data through extensive sequential testing. Thus, the qualification and eventual deployment of new fuel systems constitute a long process. However, recent technological advancements have provided researchers the opportunity to perform out-of-cell, in situ measurements to assess material performance for the duration of the experiment. One such example of this capability is the use of digital image coordination and thermal imaging to assess Zircaloy cladding performance under a simulated loss-of-coolant accident (LOCA) transient condition. In situ measurements generally provide high-fidelity strain, strain rates, and temperature surface maps. This is critical for the US nuclear industry, which is actively developing a technical basis to support extending the peak rod average burnup from 62 to ~75 GWd/tU and the deployment of accident-tolerant fuel. However, the US Nuclear Regulatory Commission (NRC) outlined in its research information letter several technical issues that the industry must address before extending burnup. One topic of specific interest is understanding the cladding balloon and rupture geometry during the LOCA heat-up phase. By leveraging these advanced in situ capabilities, this work used in situ data generated from a simulated LOCA to better understand high-temperature creep and its effect on Zircaloy balloon and rupture performance. Here, this work used the BISON fuel performance code to assess the high-temperature creep model predictions with in situ data.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2017

Simulated Space Environmental Effects on Thin Film Solar Array Components

The Lightweight Integrated Solar Array and Transceiver (LISA-T) experiment consists of thin-film, low mass, low volume solar panels. Given the variety of thin solar cells and cover materials and the lack of environmental protection afforded by typical thick coverglasses, a series of tests were conducted in Marshall Space Flight Center's Space Environmental Effects Facility to evaluate the performance of these materials. Candidate thin polymeric films and nitinol wires used for deployment were also exposed. Simulated space environment exposures were selected based on SSP 30425 rev. B, "Space Station Program Natural Environment Definition for Design" or AIAA Standard S-111A-2014, "Qualification and Quality Requirements for Space Solar Cells." One set of candidate materials were exposed to 5 eV atomic oxygen and concurrent vacuum ultraviolet (VUV) radiation for low Earth orbit simulation. A second set of materials were exposed to 1 MeV electrons. A third set of samples were exposed to 50, 500, and 750 keV energy protons, and a fourth set were exposed to >2,000 hours of ultraviolet radiation. A final set was rapidly thermal cycled between -50 and +120 C. This test series provides data on enhanced power generation, particularly for small satellites with reduced mass and volume resources. Performance versus mass and cost per Watt is discussed.

Finckenor, Miria↗

NASA NTRS2017

Simulated Space Environmental Effects on Thin Film Solar Array Components

The Lightweight Integrated Solar Array and Transceiver (LISA-T) experiment consists of thin-film, low mass, low volume solar panels. Given the variety of thin solar cells and cover materials and the lack of environmental protection typically afforded by thick coverglasses, a series of tests were conducted in Marshall Space Flight Center's Space Environmental Effects Facility to evaluate the performance of these materials. Candidate thin polymeric films and nitinol wires used for deployment were also exposed. Simulated space environment exposures were selected based on SSP 30425 rev. B, "Space Station Program Natural Environment Definition for Design" or AIAA Standard S-111A-2014, "Qualification and Quality Requirements for Space Solar Cells." One set of candidate materials were exposed to 5 eV atomic oxygen and concurrent vacuum ultraviolet (VUV) radiation for low Earth orbit simulation. A second set of materials were exposed to 1 MeV electrons. A third set of samples were exposed to 50, 100, 500, and 700 keV energy protons, and a fourth set were exposed to >2,000 hours of near ultraviolet (NUV) radiation. A final set was rapidly thermal cycled between -55 and +125 C. This test series provides data on enhanced power generation, particularly for small satellites with reduced mass and volume resources. Performance versus mass and cost per Watt is discussed.

Finckenor, Miria↗

NASA NTRS2017

Simulated Space Environmental Effects on Thin Film Solar Array Components

The Lightweight Integrated Solar Array and Transceiver (LISA-T) experiment consists of thin-film, low mass, low volume solar panels. Given the variety of thin solar cells and cover materials and the lack of environmental protection typically afforded by thick coverglasses, a series of tests were conducted in Marshall Space Flight Center's Space Environmental Effects Facility to evaluate the performance of these materials. Candidate thin polymeric films and nitinol wires used for deployment were also exposed. Simulated space environment exposures were selected based on SSP 30425 rev. B, "Space Station Program Natural Environment Definition for Design" or AIAA Standard S-111A-2014, "Qualification and Quality Requirements for Space Solar Cells." One set of candidate materials were exposed to 5 eV atomic oxygen and concurrent vacuum ultraviolet (VUV) radiation for low Earth orbit simulation. A second set of materials were exposed to 1 MeV electrons. A third set of samples were exposed to 50, 100, 500, and 700 keV energy protons, and a fourth set were exposed to >2,000 hours of near ultraviolet (NUV) radiation. A final set was rapidly thermal cycled between -55 and +125degC. This test series provides data on enhanced power generation, particularly for small satellites with reduced mass and volume resources. Performance versus mass and cost per Watt is discussed.

Finckenor, Miria↗