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DOE OSTI2018

Localized Deformation Investigation in Irradiated Materials via Electron Microscopy, EBSD, and In-Situ Mechanical Testing

This report describes the preliminary results of an analysis of dislocation defect structures in nondeformed and deformed austenitic stainless steels – materials of light water reactor internal components. The analysis was performed using an advanced modern approach: high-resolution electron backscatter diffraction (HR-EBSD). Work was performed at Oak Ridge National Laboratory’s Low Activation Materials Development and Analysis (LAMDA) facility. The report is divided into sections describing specific aspects of the project. Section 1 describes the necessity and importance of the defect microstructure analysis and demonstrates that there are very limited data regarding dislocation and defect population at the meso-level (i.e., a grain or group of interacting grains). Section 1 also introduces the HR-EBSD approach used in this research and provides a limited background. Section 2 describes the scanning electron microscope/EBSD systems available at the LAMDA facility, materials investigated in the present work, and hardware and software requirements for the HR-EBSD analysis. Section 3 provides preliminary HR-EBSD results for nonirradiated austenitic stainless steel in contrast to and in comparison with the conventional EBSD outcome. Section 4 describes the HR-EBSD results for austenitic stainless steel irradiated in a commercial-type nuclear power plant and subjected to in-situ mechanical testing. The analysis is focused on mapping and analyzing the geometrically necessary dislocations before and after deformation at small strain levels. As expected, the results will be beneficial for performing corrosion tests, including electrochemical microscopy, which is currently being performed within the Light Water Reactor Sustainability program at the University of California–Los Angeles (Dr. G. Sant). Section 5 summarizes the work performed, presents conclusions, and discusses future activities for this research.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

NASA NTRS1990

Design Graphics

A mathematician, David R. Hedgley, Jr. developed a computer program that considers whether a line in a graphic model of a three-dimensional object should or should not be visible. Known as the Hidden Line Computer Code, the program automatically removes superfluous lines and displays an object from a specific viewpoint, just as the human eye would see it. An example of how one company uses the program is the experience of Birdair which specializes in production of fabric skylights and stadium covers. The fabric called SHEERFILL is a Teflon coated fiberglass material developed in cooperation with DuPont Company. SHEERFILL glazed structures are either tension structures or air-supported tension structures. Both are formed by patterned fabric sheets supported by a steel or aluminum frame or cable network. Birdair uses the Hidden Line Computer Code, to illustrate a prospective structure to an architect or owner. The program generates a three- dimensional perspective with the hidden lines removed. This program is still used by Birdair and continues to be commercially available to the public.

Source record↗

NASA NTRS2013

JPL Contamination Control Engineering

JPL has extensive expertise fielding contamination sensitive missions-in house and with our NASA/industry/academic partners.t Development and implementation of performance-driven cleanliness requirements for a wide range missions and payloads - UV-Vis-IR: GALEX, Dawn, Juno, WFPC-II, AIRS, TES, et al - Propulsion, thermal control, robotic sample acquisition systems. Contamination control engineering across the mission life cycle: - System and payload requirements derivation, analysis, and contamination control implementation plans - Hardware Design, Risk trades, Requirements V-V - Assembly, Integration & Test planning and implementation - Launch site operations and launch vehicle/payload integration - Flight ops center dot Personnel on staff have expertise with space materials development and flight experiments. JPL has capabilities and expertise to successfully address contamination issues presented by space and habitable environments. JPL has extensive experience fielding and managing contamination sensitive missions. Excellent working relationship with the aerospace contamination control engineering community/.

Molecular Contamination Spectral Effects (MCSE) Ch↗

DOE OSTI2024

Electrolyte and Cutoff Potential Effects on Cycle Life of Li4Ti5O12/LiNi0.9Mn0.1O2 Batteries for Behind-the-Meter Storage Applications

Behind-the-Meter Storage (BTMS) is a stationary battery energy storage system that is connected to the electrical distribution system on the customer's side of the utility's service meter. BTMS systems are used to store electrical energy from the grid as well as inconstant, renewable energy, such as local solar and wind generation. A successful BTMS system will allow the customer to pair their energy generation and storage to optimize electrical consumption from the grid, improving reliability and minimizing cost. For BTMS applications, batteries must be designed and optimized with different set of criteria from other leading segments of the Li-ion battery market, like transportation, due the system being stationary and proximal to the residential or commercial building it's benefitting. BTMS applications prioritize safety, cost (low/no-critical materials), reliability (20-year calendar life), and durability (10,000 cycle life), while having the ability to (minimally) compromise energy density and rate capability. Lithium titanate (Li4Ti5O12-, LTO) is a promising anode candidate for BTMS applications due to its high safety and capacity retention, while maintaining a reasonable 160 mAhg-1 reversable capacity and composition of relatively abundant materials. (1) Specifically, LTO has a high working voltage which helps to prevent Li dendrite formation, improving safety. Furthermore, LTO also has negligible lithiation-based volume change, leading to less mechanical pulverization, or loss of active material, upon cycling. For the cathode, materials with little or no Co are of high interest due to the high cost and low abundance of Co. LiMn2O4 (LMO) has been paired with LTO for BTMS applications in the past due to its safety, low cost (abundancy), and reasonably high operating voltage. (2-4) However, the low capacity of LMO limits energy density and specific energy. While not the highest priority for BTMS applications, increasing energy density will enable deployment in space constrained BTMS applications and decrease total cost. LiNi0.9Mn0.1O2 (LN-MO) is a recently developed material with promise due to its high operating voltage and relatively low price. (5) However, Ni-rich layered oxides, including LNMO, tend to struggle with capacity retention during high-voltage cycling due to mechanical pulverization, irreversible phase transitions, and unstable solid-electrolyte interphase. The study presented here focuses on building an understanding of how electrolyte solvent and varied cutoff potentials will impact the cycle life of LTO/LN-MO cells. Specifically, a comparison is provided between ethylene carbonate (EC), ethyl methyl carbonate (EMC), fluoroethylene carbonate (FEC), and Gen2 electrolyte solvents with 1M Lithium hexafluorophosphate (LiPF6) salt, cycling to two upper termination potentials, 2.6V and 2.7V. Electrochemical testing and diagnostics (e.g., differential capacity analysis, area specific impedance, constant voltage hold, and rate capability) and post-mortem characterization will be used to understand the aging behavior and failure mechanisms of the 8 cell combinations (four electrolytes and two voltage cutoffs). Cells with FEC electrolyte showed a lower initial capacity compared to cells with Gen2, EMC, and EC cycling at both voltages; however, the cells with FEC showed consistent trends in capacity retention with 2.6V and 2.7V termination potentials, while the cells with the other electrolytes showed much higher rates of capacity loss when cycling to the higher voltage. These results indicate that FEC may play a role in improving durability of high-voltage, Ni-rich electrode systems for use in high-cycle applications, such as BTMS.

electrolyte↗

NASA NTRS1996

P and W Cryogenic Fluid-Film Bearing and Seal Technology Development and Implementation

This presentation will summarize Pratt & Whitney's past, present, and future activities toward cryogenic fluid-film bearing and seal technology development and implementation. The three major areas of focus for this technology are analytical models and design tools, component testing, and technology implementation. The analytical models and design tools area will include a summary of current tools along with an overview of P&W's new full 3-D Navier-Stokes solution for hydrostatic bearings, HYDROB3D. P&W's comprehensive component test program, including teaming with the Air Force Phillips Laboratory, NASA's Marshall Space Flight Center, and Carrier Corporation, will be outlined. Component test programs consisting of material development and testing, surface patterns/roughness, pocket and orifice geometry variations, and static and dynamic performance of both journal and thrust bearings will be summarized. Finally, the technology implementation area will show the benefits and plans for P&W to incorporate this technology into products.

Pelfrey, Philip C.↗

NASA NTRS1992

Improved inhomogeneous finite elements for fabric reinforced composite mechanics analysis

There is a need to do routine stress/failure analysis of fabric reinforced composite microstructures to provide additional confidence in critical applications and guide materials development. Conventional methods of 3-D stress analysis are time consuming to set up, run and interpret. A need exists for simpler methods of modeling these structures and analyzing the models. The principal difficulty is the discrete element mesh generation problem. Inhomogeneous finite elements are worth investigating for application to these problems because they eliminate the mesh generation problem. However, there are penalties associated with these elements. Their convergence rates can be slow compared to homogeneous elements. Also, there is no accepted method for obtaining detailed stresses in the constituent materials of each element. This paper shows that the convergence rate can be significantly improved by a simple device which substitutes homogeneous elements for the inhomogeneous ones. The device is shown to work well in simple one and two dimensional problems. However, demonstration of the application to more complex two and three dimensional problems remains to be done. Work is also progressing toward more realistic fabric microstructural geometries.

Foye, R. L.↗

NASA NTRS1991

Heat pipe radiation cooling of advanced hypersonic propulsion system components

Heat transfer, heat pipe, and system studies were performed to assess the newly proposed heat pipe radiation cooling (HPRC) concept. With an HPRC system, heat is removed from the ramburner and nozzle of a hypersonic aircraft engine by a surrounding, high-temperature, heat pipe nacelle structure, transported to nearby external surfaces, and rejected to the environment by thermal radiation. With HPRC, the Mach number range available for using hydrocarbon fuels for aircraft operation extends into the Mach 4 to Mach 6 range, up from the current limit of about Mach 4. Heat transfer studies using a newly developed HPRC computer code determine cooling system and ramburner and nozzle temperatures, heat loads, and weights for a representative combined-cycle engine cruising at Mach 5 at 80,000 ft altitude. Heat pipe heat transport calculations, using the Los Alamos code HTPIPE, reveal that adequate heat trasport capability is available using molybdenum-lithium heat pipe technology. Results show that the HPRC system radiator area is limited in size to the ramburner-nozzle region of the engine nacelle; reasonable system weights are expected; hot section temperatures are consistent with advanced structural materials development goals; and system impact on engine performance is minimal.

Martin, R. A.↗

DOE OSTI2025

Quantum Sieving for Isotopic Separations of Gases Using Porous Materials─30 Years of Progress

Here, this paper reviews theoretical and experimental efforts to establish microporous materials that can be used to separate isotopologues of molecular gases such as H 2 and D 2 . Emphasis is placed on use of simplified models to highlight the quantum phenomena that make these separations possible. In equilibrium adsorption, differences in zero point energy in the adsorbed states of molecules favor binding of heaver isotopologues (e.g. D 2 relative to H 2 ). Experimental data showing this effect was reported as early as 1933, but the theoretical work of Beenakkers et al. in 1995 [Chem. Phys. Lett. 232 (1995) 379-382] spurred modern efforts to develop materials with strong so-called quantum sieving. In porous materials where the transition state for molecular diffusion is more strongly confined than the energy minima associated with equilibrium adsorption, differences in zero point energies between these two sites can lead to isotopic differences in molecular diffusivities. This effect favors diffusion of heavier species (e.g. D 2 ) relative to lighter species (e.g. H 2 ). This so-called kinetic quantum sieving has been observed experimentally in porous carbons and in porous organic cage materials. We show that quantum tunneling, which favors hopping of lighter species across energy barriers, diminishes the strength of kinetic quantum sieving but that it appears to make only a small contribution to the net molecular diffusivities in many porous materials of practical interest.

Sholl, David S. [Oak Ridge National Laboratory (OR↗

NASA NTRS2005

A Preliminary Investigation of the E-Beam Induced Polymerization of Maleimide and Norbornene End-capped Polyimides

A research area of high activity in connection with aerospace engineering has been the development of polymer thermosetting resins that can resist temperature as high as 300 C while maintaining adequate toughness, and providing ease of processing to enable low temperature and low cost composite fabrication methods. In order to meet such requirements, sequential interpenetrating polymer networks (IPNs) based on bismaleimide (BMI) and cyanate ester (CE) monomers were investigated. In these systems, a polycyanurate network is first formed in the presence of BMI and appropriate reactive diluent monomers and in a second step, a network based on the BMI is created in the presence of a fully formed polycyanurate network. The materials developed can be processed at relatively low temperature (less than 150 C) and with the aid of electron beam (EB) curing. Of major importance to the success of this work was the identification of a reactive diluent that improves ease of processing and has tailored reactivity to allow for the controlled synthesis of CE-BMI sequential IPNs. Based on solubility and reactivity of a number of reactive diluents, N-acryloylmorpholine (AMP) was selected as a comonomer for BMI copolymerization. A donor-acceptoreaction mechanism was suggested to explain the relative reactivity of a variety of reactive diluents towards maleimide functionality. The optimum processing parameters for the formation of the first network were determined through the study of metal catalyzed cure and hydrolysis of cyanate esters, whereas the reaction behavior for second network formation in terms of the influence of EB dose rate and temperature was elucidated through an in-situ kinetics study of maleimide and AMP copolymerization. Structure-property relationships were developed which allowed for the design of improved resin systems. In particular, appropriate network coupler possessing cyanate ester and maleimide functionality was synthesized to link the polycyanurate first network to the BMI/AMP second network and thus form linked sequential IPNs (LIPNs). Consequently, Tg as high as 370 C was achieved and a fracture toughness of 120 Joules per square meters was obtained for resin systems that possess adequately low viscosity for processing using liquid molding techniques at low temperature.

Palmese, Giuseppe R.↗

NASA NTRS1999

Higher-Order Theory for Functionally Graded Materials

This paper presents the full generalization of the Cartesian coordinate-based higher-order theory for functionally graded materials developed by the authors during the past several years. This theory circumvents the problematic use of the standard micromechanical approach, based on the concept of a representative volume element, commonly employed in the analysis of functionally graded composites by explicitly coupling the local (microstructural) and global (macrostructural) responses. The theoretical framework is based on volumetric averaging of the various field quantities, together with imposition of boundary and interfacial conditions in an average sense between the subvolumes used to characterize the composite's functionally graded microstructure. The generalization outlined herein involves extension of the theoretical framework to enable the analysis of materials characterized by spatially variable microstructures in three directions. Specialization of the generalized theoretical framework to previously published versions of the higher-order theory for materials functionally graded in one and two directions is demonstrated. In the applications part of the paper we summarize the major findings obtained with the one-directional and two-directional versions of the higher-order theory. The results illustrate both the fundamental issues related to the influence of microstructure on microscopic and macroscopic quantities governing the response of composites and the technologically important applications. A major issue addressed herein is the applicability of the classical homogenization schemes in the analysis of functionally graded materials. The technologically important applications illustrate the utility of functionally graded microstructures in tailoring the response of structural components in a variety of applications involving uniform and gradient thermomechanical loading.

Aboudi, Jacob↗

NASA NTRS1987

Transportable educational programs for scientific and technical professionals: More effective utilization of automated scientific and technical data base systems

This grant final report executive summary documents a major, long-term program addressing innovative educational issues associated with the development, administration, evaluation, and widespread distribution of transportable educational programs for scientists and engineers to increase their knowledge of, and facilitate their utilization of automated scientific and technical information storage and retrieval systems. This educational program is of very broad scope, being targeted at Colleges of Engineering and Colleges of Physical sciences at a large number of colleges and universities throughout the United States. The educational program is designed to incorporate extensive hands-on, interactive usage of the NASA RECON system and is supported by a number of microcomputer-based software systems to facilitate the delivery and usage of the educational course materials developed as part of the program.

Dominick, Wayne D.↗

DOE OSTI2018

Solid-State NMR Identification of Intermolecular Interactions in Amelogenin Bound to Hydroxyapatite

The ability to develop materials with hierarchical structure and controlled properties is highly desirable. Biomineralization processes govern the formation of hierarchical hard tissues such as bone and teeth and mimicking these processes could allow new materials with difffernet properties. The proteins present during biomineral formation are proposed to play a critical role in the unique properties of these minerals. While structure is commonly affiliated with the function of proteins, biomineralization proteins are bound to a solid surface in their physiologically relevant form, limiting the role of protein structure due to the inability to use many conventional structure characterization techniques. Here, solid state NMR spectroscopy was applied to study the intermolecular interactions of amelogenin in self-assembled oligomers bound to hydroxyapatite. Amelogenin is the most abundant protein present during the early stages of enamel formation and is essential for normal enamel development. Intermolecular dipolar couplings were identified that support amelogenin dimer formation due to interactions between residues in the C-termini. These dipolar interactions were corroborated by molecular dynamics computer simulations. We also identified b-sheet structure in multiple regions of the protein, further developing our knowledge of this protein. This is the first intermolecular protein-protein interaction reported for a biomineralization protein, representing an advancement in understanding enamel development and a new general strategy towards investigating biomineralization proteins.

amelogenin, biomineralization, intermolecular, int↗

DOE OSTI2025

Preliminary results of molten salt corrosion of high entropy alloys manufactured at INL

Materials development is needed to support the design and deployment of advanced nuclear reactors that will operate at higher temperatures and in harsher environments than the current light water reactor fleet. High entropy alloys have been identified as a class of alloy that could address the needs of advanced reactors, such as the molten salt reactors, due to their potential strength, radiation resistance, and corrosion resistance. This project summarizes the work done in the year 2024 for the Additive Manufacturing of High Entropy Alloys for Nuclear Applications Project. This part of the work has focused on molten salt corrosion of high entropy alloys which were developed and manufactured at INL.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2024

Additively Manufactured Carbon Fiber and Fused Deposition Modeling PLA Interlaminar Shear Testing Report

This test report summarizes the torsional test setup, procedure, and results for interlaminar shear (ILS) failure of additively manufactured carbon fiber (CFAM) material developed at LLNL. In addition, the report also includes testing of fused deposition modeled (FDM) polylactic acid (PLA), including ILS test standard D7078 and the same torsional test mentioned above. The test hopes to characterize ILS properties of CFAM, however substantial further testing and improvements still need to be done to induce a proper failure mode. This testing was performed by Sundi Win as part of her summer internship project in Kinetic Technologies.

36 MATERIALS SCIENCE↗

NASA NTRS2002

Airframe Research and Technology for Hypersonic Airbreathing Vehicles

The Hypersonics Investment Area (HIA) within NASA's Advanced Space Transportation Program (ASTP) has the responsibility to develop hypersonic airbreathing vehicles for access to space. The Airframe Research and Technology (AR and T) Project, as one of six projects in the HIA, will push the state-of-the-art in airframe and vehicle systems for low-cost, reliable, and safe space transportation. The individual technologies within the project are focused on advanced, breakthrough technologies in airframe and vehicle systems and cross-cutting activities that are the basis for improvements in these disciplines. Both low and medium technology readiness level (TRL) activities are being pursued. The key technical areas that will be addressed by the project include analysis and design tools, integrated vehicle health management (IVHM), composite (polymer, metal, and ceramic matrix) materials development, thermal/structural wall concepts, thermal protection systems, seals, leading edges, aerothermodynamics, and airframe/propulsion flowpath technology. Each of the technical areas or sub-projects within the Airframe R and T Project is described in this paper.

Glass, David E.↗

NASA NTRS2012

Flexible Plug Repair for Shuttle Wing Leading Edge

In response to the Columbia Accident Investigation Board report, a plug repair kit has been developed to enable astronauts to repair the space shuttle's wing leading edge (WLE) during orbit. The plug repair kit consists of several 17.78- cm-diameter carbon/silicon carbide (C/SiC) cover plates of various curvatures that can be attached to the refractory carbon-carbon WLE panels using a TZM refractory metal attach mechanism. The attach mechanism is inserted through the damage in the WLE panel and, as it is tightened, the cover plate flexes to conform to the curvature of the WLE panel within 0.050 mm. An astronaut installs the repair during an extravehicular activity (EVA). After installing the plug repair, edge gaps are checked and the perimeter of the repair is sealed using a proprietary material, developed to fill cracks and small holes in the WLE.

Camarda, Charles J.↗

DOE OSTI2023

Microstructure modeling of nuclear structural materials: Recent progress and future directions

Modeling and simulation of microstructures are essential to understand the complex responses and behaviors of nuclear materials in extreme environments. The needs to assess the extended life operation as well as the growing interest in accelerating nuclear materials development and qualification have stimulated the use of high-fidelity multiscale models aided by empirical and ab initio data. This paper reviews the role of various models across different length and time scales in investigating irradiation effects on microstructure evolution and degradation, in particular the embrittlement caused by radiation induced or enhanced formation of nanoscale chemical heterogeneities. The strength and limitations of these models, including classical rate theories, cluster dynamics, phase-field methods, and atomistic models informed by ab initio energies, are discussed with seminal examples. Challenges regarding the lack of thermo-kinetic data and theoretical treatments considering chemical complexities and magnetic excitations, as well as the stabilizing effect by excess point defects in nuclear structural materials are presented, along with potential solutions based on ab initio informed surrogate energy models and statistical sampling by Monte Carlo simulations. Further, the review then highlights the opportunities to leverage the advantages of different methods by establishing hybrid models by shared variables or coupled codes and applications. Finally, the review concludes with forward-looking remarks on how the use of physics-based models can aid the improvement of machine-learning models of property degradation and vice versa.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Infrastructure Investments in LAMDA: SEM Mill and Vault (NSUF 2019 Milestone Report)

This document summarizes the procurement, installation, and commissioning of a scanning electron microscope (SEM) mill produced by Fischione Instruments and a lead-shielded vault for specimen storage in support of Nuclear Science User Facility (NSUF) awards for use in Oak Ridge National Laboratory’s (ORNL) Low Activation Materials Development and Analysis (LAMDA) laboratory. The Model 1061 SEM mill is a tabletop ion milling system for advanced sample preparation of high-quality SEM samples. This device was chosen for its broad range of ion energies allowing for both rapid milling and final polishing of the sample surface. The purchase order with Fischione Instruments was released and awarded by ORNL procurement on September 11, 2018. The instrument was shipped in December of 2018 and was installed in the LAMDA laboratory in March of 2019. During the commissioning of this equipment, electron backscatter diffraction (EBSD) was performed on specimens before and after milling to show the enhanced surface quality. With the purchase of a lead vault dedicated to NSUF library materials co-located in the LAMDA laboratory, the NSUF program will be able to maintain a significant sample library in LAMDA. These specimens will be easily accessible for rapid turnaround experiment (RTE) awards and will reduce the overall cost of year-over-year storage and shipments to and from ORNL hot cell facilities. The contract to fabricate a fourth lead vault dedicated to NSUF specimen storage was awarded by ORNL procurement on August 10, 2018. Installation of the new vault was completed in January of 2019.

47 OTHER INSTRUMENTATION↗