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DOE OSTI2023

Self-assembled Seashell Like Coatings for Large Area Robust Debris Shields for Next Generation Pulsed Power Drivers

During this LDRD project, our team developed a technology which enables the fabrication of novel nanostructures replicating seashell – “nature’s toughest material”. The resulting coatings exhibit high thermal stability up to 1650°C, which exceeds the hardness of Spectra® by ~44%, as well as the compressive strength of aluminum by ~57%. Coatings made with this technology are stronger, environmentally friendly, more sustainable, and more versatile than other comparable materials. Beryllium wafers, the current, most favorable shielding material in terms of thermal and mechanical properties, are very toxic and cost hundreds of times more than the new material developed in this project. The coatings on silicon wafer and stainless steel, respectively, have been tested as ride-along on the Z machine and clearly outperform the bare substrate. Use of this technology will have a profound global impact for pulsed power and fusion energy development, debris mitigation for spacecraft and satellites, durability of drill bits used in deep well drilling and tunnel boring operations, thermal protection of aircraft and manned spacecraft, and various other thermal and mechanical protection applications.

36 MATERIALS SCIENCE↗

NASA NTRS2003

Hydrostatic Stress Effects Incorporated Into the Analysis of the High-Strain-Rate Deformation of Polymer Matrix Composites

Procedures for modeling the effect of high strain rate on composite materials are needed for designing reliable composite engine cases that are lighter than the metal cases in current use. The types of polymer matrix composites that are likely to be used in such an application have a deformation response that is nonlinear and that varies with strain rate. The nonlinearity and strain rate dependence of the composite response is primarily due to the matrix constituent. Therefore, in developing material models to be used in the design of impact-resistant composite engine cases, the deformation of the polymer matrix must be correctly analyzed. However, unlike in metals, the nonlinear response of polymers depends on the hydrostatic stresses, which must be accounted for within an analytical model. An experimental program has been carried out through a university grant with the Ohio State University to obtain tensile and shear deformation data for a representative polymer for strain rates ranging from quasi-static to high rates of several hundred per second. This information has been used at the NASA Glenn Research Center to develop, characterize, and correlate a material model in which the strain rate dependence and nonlinearity (including hydrostatic stress effects) of the polymer are correctly analyzed. To obtain the material data, Glenn s researchers designed and fabricated test specimens of a representative toughened epoxy resin. Quasi-static tests at low strain rates and split Hopkinson bar tests at high strain rates were then conducted at the Ohio State University. The experimental data confirmed the strong effects of strain rate on both the tensile and shear deformation of the polymer. For the analytical model, Glenn researchers modified state variable constitutive equations previously used for the viscoplastic analysis of metals to allow for the analysis of the nonlinear, strain-rate-dependent polymer deformation. Specifically, we accounted for the effects of hydrostatic stresses. An important discovery in the course of this work was that the hydrostatic stress effects varied during the loading process, which needed to be accounted for within the constitutive equations. The model is characterized primarily by shear data, with tensile data used to characterize the hydrostatic stress effects.

Goldberg, Robert K.↗

DOE OSTI2015

Development of ASTM Standard for SiC-SiC Joint Testing Final Scientific/Technical Report

As the nuclear industry moves to advanced ceramic based materials for cladding and core structural materials for a variety of advanced reactors, new standards and test methods are required for material development and licensing purposes. For example, General Atomics (GA) is actively developing silicon carbide (SiC) based composite cladding (SiC-SiC) for its Energy Multiplier Module (EM2), a high efficiency gas cooled fast reactor. Through DOE funding via the advanced reactor concept program, GA developed a new test method for the nominal joint strength of an endplug sealed to advanced ceramic tubes, Fig. 1-1, at ambient and elevated temperatures called the endplug pushout (EPPO) test. This test utilizes widely available universal mechanical testers coupled with clam shell heaters, and specimen size is relatively small, making it a viable post irradiation test method. The culmination of this effort was a draft of an ASTM test standard that will be submitted for approval to the ASTM C28 ceramic committee. Once the standard has been vetted by the ceramics test community, an industry wide standard methodology to test joined tubular ceramic components will be available for the entire nuclear materials community.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Regulating hydrogel mechanical properties with an electric field

Stimuli-responsive polymeric materials have attracted significant attention due to their ability to change properties in response to various external stimuli. Using an electric field as the stimulus is of particular interest as it possesses the potential for seamless integration of materials with electronic systems. While many materials with electric field responsive actuation have an associated mechanical property change, it is beneficial to develop materials that exhibit mechanical property changes without accompanying significant shape deformation. To address this challenge, here we designed a semi-interpenetrating polymer network (semi-IPN) hydrogel system containing both polyelectrolytes and salt ions, which enables electric field induced changes in mechanical properties while minimizing actuation. We first successfully verified the viability of our design by removing salt ions through a diffusion-only method where we witnessed the stiffness increased to 4.5 times the initial value while still being highly deformable. After this, we applied an electric field to transport the salt ions out of the hydrogel, as shown by both Raman spectroscopy and scanning electron microscopy. We were able to show a time-dependent stiffness increase, the maximum of which was 5 times the original stiffness. We quantified ion transport and water-splitting in the hydrogel by both experiments and simulations. Following this, we showed functional system reversibility by reversing the direction of the current to reinject salt ions into the semi-IPN hydrogel and reducing its stiffness to below the initial value. It's worth noting that our simulations enable us to understand the governing mechanisms behind ion generation and salt transport that leads to mechanical property changes. Finally, we were able to fabricate a spatially variable stiffness haptic interface with our hydrogel, with demonstrated reversibility and cyclability. This research can possibly find applications in soft robotics and haptics and also inspire the development of bio-compatible electronics related devices.

36 MATERIALS SCIENCE↗

DOE OSTI2016

A microstructure-guided constitutive modeling approach for random heterogeneous materials: Application to structural binders

This paper presents a microstructure-guided modeling approach to predict the effective elastic response of heterogeneous materials, and demonstrates its application toward two highly heterogeneous, uncon- ventional structural binders, i.e., iron carbonate and fly ash geopolymer. Microstructural information from synchrotron X-ray tomography (XRT) and intrinsic elastic properties of component solid phases from statistical nanoindentation are used as the primary inputs. The virtual periodic 3D microstructure reconstructed using XRT, along with periodic boundary conditions is used as a basis for strain- controlled numerical simulation scheme in the linear elastic range to predict the elastic modulus as well as the stresses in the microstructural phases. The elastic modulus of the composite material predicted from the microstructure-based constitutive modeling approach correlates very well with experimental measurements for both the materials considered. This technique efficiently links the microstructure to mechanical properties of interest and helps develop material design guidelines for novel heterogeneous composites

36 MATERIALS SCIENCE↗

DOE OSTI2023

Well-Tunable, 3D-printable, and Fast Autonomous Self-Healing Elastomers

Self-healing elastomers provide extended longevity of functional materials, due to their unique adaptability and durability. However, a major scientific challenge remains in developing materials with a rapid healing process combined with decent mechanical properties, that can be prepared by a relatively simple synthesis approach. Herein, we report a versatile design approach on self-healing elastomers by incorporating two different hydrogen bonding containing monomers, i.e., 2-[[(butylamino)carbonyl]oxy]ethyl acrylate (BCOE) and 2-ureido-4[1H]pyrimidinone (UPy) functionalized ethyl methacrylate. Poly(BCOE-r-UPy)s are synthesized by reversible addition-fragmentation chain-transfer (RAFT) polymerization, and controlling the ratio of two monomers enables well-tunable mechanical properties with tensile strength ranging from 0.04 to 6.3 MPa and tensile strain up to 3,000 %. The characteristic dissociation energy is calculated from a temperature dependence of terminal relaxation followed by subtracting the segmental relaxation. The rapid autonomous self-healing is achieved when the molar composition of Poly(BCOE-r-UPy) is tailored to BCOE/UPy = 99/1. The self-healing process is monitored in situ by a helium-ion microscope, and its macroscopic study using tensile tests indicates that Poly(BCOE-r-UPy1) with 1 % molar ratio of UPy recovers 70 % of its original toughness at ambient temperature within 10 mins. 3D printing of Poly(BCOE-r-UPy) affords a self-healable 3D structure, demonstrating the adaptability of Poly(BCOE-r-UPy) for on-demand fabrication. The simplicity of synthesis, well-tunable mechanical properties, unique self-healability, and 3D printing capability of Poly(BCOE-r-UPy)s indicate their potential for a range of applications.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Side Chain and Solvent Direction of Film Morphology in Small-Molecule Organic Solar Materials

Film morphology control is essential to materials development for efficient organic solar cells (OSCs). Unlocking methods to optimize the film morphology for materials without changing the fundamental electronic characteristics can enable previously unacceptable materials to achieve high performance. In this work, a series of acceptor-donor-acceptor (ADA) small molecule p-type OSC semiconductors having benzo[1,2-b:6,5-b0]dithiophene (bBDT) donor units and thiophene capped diketopyrrolopyrrole (TDPP) acceptor units are examined where the sole molecular design variation is in the electronically inactive side chains. Four bBDT(TDPP) 2 compounds with all possible combinations of either 2-ethelhexyl (EH), or 3,7-dimtheyloctyl (DMO) side chains on the bBDT core and TDPP units are discussed. When processed from a chloroform (CF)-only solution, blend films of the molecules with the PC 71 BM electron acceptor exhibit similar thin film properties and photovoltaic performance, regardless of the side chain composition. However, when the additive 1,8-diiodooctane (DIO) is included in the processing solution, the morphological properties and OSC performance diverge dramatically, with the side chain variations now dictating the film morphology, resulting in a >400% spread in power conversion efficiency (PCE). Donor molecules with a mixed side chain motif having the larger DMO side chain on the bBDT core unit deliver the best performance owing to greater donor:acceptor phase intermixing while maintaining contiguous and efficient charge transport pathways. Using in situ GIWAXS during spin-coating, it is shown that DIO extends crystallization times, thereby promoting more thermodynamically driven structures where the side chain compositions have greater impact. Lastly, general guidelines are presented for achieving morphological optimization via combined side chain engineering and processing additives.

36 MATERIALS SCIENCE↗

DOE OSTI2020

A practical guide for crystal growth of van der Waals layered materials

This Tutorial provides an overview of the techniques that are most commonly utilized to grow bulk van der Waals crystals. The materials discussed were selected to highlight various challenges that are often encountered during crystal growth. Additionally, in relatively equal parts, the text covers melt-based techniques, vapor transport growths, and the characterization of crystal quality with an emphasis on structural and chemical homogeneities. Furthermore, pertinent details are given regarding the growth and characterization of many specific compounds, with examples mostly drawn from our own research, and an effort is made to highlight cases where the growths offer a particular lesson or the conditions have a significant impact on the crystal’s physical properties. A primary goal is to motivate more researchers to grow crystals by providing general descriptions and considerations for different growth techniques and equipment while sharing some of our own lessons learned and best practices for the growth and characterization of layered van der Waals crystals. The Tutorial is not written solely for aspiring crystal growers, however, because any researcher who collaborates with a crystal grower can benefit from having a greater understanding and appreciation of the processes of crystal growth and materials development.

36 MATERIALS SCIENCE↗

NASA NTRS1993

Preliminary results from the CONCAP-2-01 and EIOM-3 experiments on STS-46

CONCAP-2-01 (complex autonomous payload, first flight) was the maiden flight of 'CONCAP-2,' a secondary payload, utilizing the get-away special (GAS) carrier system, sponsored by the Consortium for Materials Development in Space (CMDS) at the University of Alabama in Huntsville (UAH). A host of materials such as high-T(sub c) superconductor samples, metal films, polymers, carbons, and semiconducting materials were exposed to a low earth orbit (LEO) environment. We have also measured on orbit the changes in the electrical resistance of some of the high-T(sub c) materials plus carbon and silver dosimeters exposed to the space environment. The preliminary results of this experiment are compared with those from EOIM-3, both of which flew on STS-46.

Gregory, John C.↗

NASA NTRSDate not supplied

Thermally Conductive Insulation for High Power Density Electric Machines

In the mid 2000’s NASA challenged the aeronautics industry to identify the routes for achieving ambitious improvements in fuel burn, emission, and noise reductions. These so-called “N+3” studies were exploring broad changes three commercial aircraft generations, or nominally 30 years, in the future. Many intriguing propulsion-airframe integrated solutions were proposed and pursued, which incorporated technologies such as high-aspect-ratio wings, boundary-layer ingestion, and hybrid electric powertrains. This talk summarizes the approaches and achievements from the Hybrid Gas-Electric Propulsion Concept Technical Challenge that concluded in 2019. The balanced portfolio of concepts studies anchored with practical technology development demonstrated that electrified aircraft propulsion is an aircraft revolution whose time has come. Advanced materials will play a key role with enabling the increase in operating efficiencies and lifetime of these high power-dense electric machines. Progress made in materials development as part of NASA’s Advanced Air Transport Technology project will also be discussed.

electrical insulation↗

NASA NTRSDate not supplied

Space Charge Analysis Capabilities for the Evaluation of High Voltage Insulation Materials

Materials development is crucial for the advancement of electric aviation. Current research focusing on novel multifunctional materials is underway to solve the needs for aerospace systems; however, additional testing of these materials to understand their failure modes is equally critical. This project will utilize pulsed electroacoustic (PEA) instrumentation to investigate space charge accumulation of multifunctional composites and other insulation materials critical to robust high power transmission systems. Evaluating the space charge phenomena in dielectric materials will provide unique and fundamentally necessary data to determine the feasibility and lifetime of any high voltage insulation system. When electrical charge is injected into a solid dielectric, charge can accumulate and become trapped, leading to the failure of the insulation via breakdown or arcing events. This study will discuss the pulsed electroacoustic methodology and its use on evaluating various dielectric polymer and composite films.

pulsed electroacoustic↗

NASA NTRS2004

Automated Guided-Wave Scanning Developed to Characterize Materials and Detect Defects

The Nondestructive Evaluation (NDE) Group of the Optical Instrumentation Technology Branch at the NASA Glenn Research Center has developed a scanning system that uses guided waves to characterize materials and detect defects. The technique uses two ultrasonic transducers to interrogate the condition of a material. The sending transducer introduces an ultrasonic pulse at a point on the surface of the specimen, and the receiving transducer detects the signal after it has passed through the material. The aim of the method is to correlate certain parameters in both the time and frequency domains of the detected waveform to characteristics of the material between the two transducers. The scanning system is shown. The waveform parameters of interest include the attenuation due to internal damping, waveform shape parameters, and frequency shifts due to material changes. For the most part, guided waves are used to gauge the damage state and defect growth of materials subjected to various mechanical or environmental loads. The technique has been applied to polymer matrix composites, ceramic matrix composites, and metal matrix composites as well as metallic alloys. Historically, guided wave analysis has been a point-by-point, manual technique with waveforms collected at discrete locations and postprocessed. Data collection and analysis of this type limits the amount of detail that can be obtained. Also, the manual movement of the sensors is prone to user error and is time consuming. The development of an automated guided-wave scanning system has allowed the method to be applied to a wide variety of materials in a consistent, repeatable manner. Experimental studies have been conducted to determine the repeatability of the system as well as compare the results obtained using more traditional NDE methods. The following screen capture shows guided-wave scan results for a ceramic matrix composite plate, including images for each of nine calculated parameters. The system can display up to 18 different wave parameters. Multiple scans of the test specimen demonstrated excellent repeatability in the measurement of all the guided-wave parameters, far exceeding the traditional point-by-point technique. In addition, the scan was able to detect a subsurface defect that was confirmed using flash thermography This technology is being further refined to provide a more robust and efficient software environment. Future hardware upgrades will allow for multiple receiving transducers and the ability to scan more complex surfaces. This work supports composite materials development and testing under the Ultra-Efficient Engine Technology (UEET) Project, but it also will be applied to other material systems under development for a wide range of applications.

Martin, Richard E.↗

NASA NTRSDate not supplied

Nanomechanical Characterization of Additive Manufactured GRCop-42 Alloy Developed by Directed Energy Deposition Methods

Propulsion applications such as combustion chambers and nozzles for liquid rocket engines require the use of unique materials with superior mechanical and thermal properties. GRCop-42(Cu-4 wt.% Cr-2 wt.% Nb) is one such candidate material developed by NASA and is now being manufactured using additive manufacturing (AM) techniques. AM offers a unique processing environment different from traditional metal fabrication processes. This study characterized the mechanical and structural properties of as-deposited and heat-treated GRCop-42manufactured with Blown Powder Directed Energy Deposition (BPD)based on preliminary testing. The materials were characterized using several techniques including surface profiling by laser microscopy, mechanical stiffness by instrumented indentation, crystal structure, residual stress measurements using XRD and residual XRD, and chemical composition and microstructural evaluation using SEM with EBSD. The results of the study are compared using the BPD techniques for samples in the as-deposited and heat-treated conditions.

GRCop-42↗

NASA NTRS2008

Structural Materials and Fuels for Space Power Plants

A fission reactor combined with Stirling convertor power generation is one promising candidate in on-going Fission Surface Power (FSP) studies for future lunar and Martian bases. There are many challenges for designing and qualifying space-rated nuclear power plants. In order to have an affordable and sustainable program, NASA and DOE designers want to build upon the extensive foundation in nuclear fuels and structural materials. This talk will outline the current Fission Surface Power program and outline baseline design options for a lunar power plant with an emphasis on materials challenges. NASA first organized an Affordable Fission Surface Power System Study Team to establish a reference design that could be scrutinized for technical and fiscal feasibility. Previous papers and presentations have discussed this study process in detail. Considerations for the reference design included that no significant nuclear technology, fuels, or material development were required for near term use. The desire was to build upon terrestrial-derived reactor technology including conventional fuels and materials. Here we will present an overview of the reference design, Figure 1, and examine the materials choices. The system definition included analysis and recommendations for power level and life, plant configuration, shielding approach, reactor type, and power conversion type. It is important to note that this is just one concept undergoing refinement. The design team, however, understands that materials selection and improvement must be an integral part of the system development.

Bowman, Cheryl↗

DOE OSTI2019

Analysis of Localized Deformation Processes in Highly Irradiated Austenitic Stainless Steel through In Situ Techniques

This report describes new experimental results obtained during in situ mechanical tests with neutron-irradiated (10.7 dpa) austenitic 304L steel specimens. The in situ tensile tests inside a scanning electron microscope (SEM) were accompanied by modern high-resolution electron backscatter diffraction (HR-EBSD) analysis. The HR-EBSD approach allowed for investigating and quantifying internal stresses and dislocation structures in nondeformed and deformed steels, materials used in light water reactor internal components. The literature regarding the HR-EBSD analysis of metals and alloys is very limited, and practically no publications on the HR-EBSD analysis coupled with in situ tests are available. Experimental work, performed at Oak Ridge National Laboratory’s Low Activation Materials Development and Analysis facility, is detailed in this report. Section 1 briefly describes strain and stress localization processes and underlines their importance and role in irradiated materials, materials used in nuclear power plants. The section demonstrates that very limited quantitative data exist regarding localized stresses and strains in the irradiated materials at the meso-level (i.e., inside the grain, for a group of interacting grains, or for channel–grain boundary [GB] interaction) whereas local stresses at GBs are key contributors to the stress corrosion crack initiation.Section 2 documents the key methods used to conduct the experimental work: the SEM/EBSD system, miniature tensile frame, and irradiated material. Irradiated specimen manufacturing is described, as this option may be of special interest for other projects. Section 3 provides details of the HR-EBSD in situ tests (e.g., tensile curves, geometry, dimensions of regions of interest, load, and deformation steps). Section 4 discusses the results related to the evolution of geometrically necessary dislocations (GNDs) and their density, spatial, and statistical distributions.Section 5 focuses on the HR-EBSD analysis with respect to a channel–GB interaction. Two aspects are discussed in detail: mapping and analyzing the GND fields before and after loading, and the possibility of investigating local stresses and elastic strains at the channel–GB interaction. The present work results are beneficial for understanding strain and stress localization processes leading to crack initiation, for analyzing the material after long-term in-service life, and for developing predictive models. Section 6 summarizes the work performed and discusses future activities within this research direction.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2017

Characterization of the Tribological Behavior of Oxide-Based NanoMaterials: Final CRADA Report

Under the Argonne/Pixelligent cooperative research and development agreement (CRADA – C1200801), Argonne performed labscale tribological tests on proprietary nano-sized ZrO 2 material developed by Pixelligent. Pixelligent utilized their proprietary process to prepare variants with different surfactants at different loadings in different carrier fluids for testing and evaluation at Argonne. Argonne applied a range of benchtop tribological test rigs to evaluate friction and wear under a range of conditions (contact geometry, loads, speeds, and temperature) that simulated a broad range of conditions experienced in engines and driveline components. Post-test analysis of worn surfaces provided information on the structure and chemistry of the tribofilms produced during the tests.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Synthetic Accessibility and Sodium Ion Conductivity of the Na8–x A x P2O9 (NAP) High-Temperature Sodium Superionic Conductor Framework

Advancement of solid-state electrolytes (SSEs) for all solid-state batteries typically focuses on modification of a known structural framework to improve conductivity, e.g., cation substitution for an immobile ion or varying the concentration of the mobile ions. Novel frameworks can be disruptive by enabling fast ion conduction aided by different structure and diffusion mechanisms, thereby unlocking optimal conductors with different properties. Herein, we perform a high-throughput survey of a structural framework for sodium ion conduction, Na8–x A x P2O9 (NAP), to understand the family’s thermodynamic stability, synthesizability, and ionic conduction. We show that the parent phase Na4TiP2O9 (NTP) undergoes a structural distortion (with accompanying conductivity transition) due to unstable phonons arising from pseudo-Jahn–Teller mode in the 1D titanium chains. Screening compounds in which Ti is substituted by other metals computationally reveal a number of candidates that are predicted to be low in formation energy and have high predicted ionic conductivities. High-throughput experimental and subsequent methodology optimization trials deliver one new compound, Na4SnP2O9 (NSP). X-ray diffraction (XRD), microscopy, and spectroscopy characterization indicate that the room-temperature structure of NSP is similar to the high-temperature, orthorhombic NTP phase but with some small unresolved structural differences. These uncharacterized structural details are speculated to limit the ion conductivity. Temperature-dependent XRD and electrochemical impedance spectroscopy indicate multiple coupled conductivity–structure transitions at a high temperature. We demonstrate the challenges with synthesis development and a priori identification of promising SSE phases as a major bottleneck in new (energy) materials development.

Chemical reactions↗

DOE OSTI2024

Understanding Formation of Irradiation-Induced Defects through 4D-STEM, Electron Tomography, and WBDF-STEM

A major challenge in advancing nuclear materials for next-generation fission and proposed fusion reactors is to comprehensively understand the formation of irradiation-induced defects. Here it is essential to correlate the evolution of irradiation-induced defects and the degradation of mechanical properties, as they collectively dictate the material's lifespan and ensure nuclear safety. Scanning transmission electron microscopy (STEM) based techniques have emerged as indispensable tools for irradiation-induced defect characterization, offering high spatial resolution imaging and chemical analysis, such as electron energy loss spectroscopy (EELS) and energy dispersive X-ray spectroscopy (EDXS). These techniques have been effectively used to obtain an atomic-scale view of the defect structure. Recent advances in electron microscopy, particularly in 4D-STEM, offer detailed insight into microstructural evolution by capturing full 2D diffraction patterns at every pixel position. Using high-speed direct electron detectors, this technology generates a four-dimensional dataset, overcoming the limitations of traditional STEM imaging.

36 MATERIALS SCIENCE↗