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All sourcesNASA NTRSDOE OSTI
NASA NTRS2018

The Importance of Contamination Knowledge - Insights into Mars Sample Return

The Astromaterials Acquisition and Curation Office at NASA Johnson Space Center (JSC), in Houston, TX (henceforth Curation Office) manages the curation of all past, present, and future extraterrestrial samples returned by NASA missions and shared collections from international partners, preserving their integrity for future scientific study while providing the samples to the international community in a fair and unbiased way. The Curation Office also curates all reference and witness materials for each mission (e.g., flight and non-flight hardware coupons; lubricants; non-flight, flight-like, and flown witness plates). These reference and witness materials provide the scientific community with the fundamental ability to reconstruct the contamination/alteration history of the sample collection through the course of the mission, with the overall goal of strengthening the scientific conclusions drawn from the study of returned materials. The information gained from characterizing the physical, biological, inorganic, and organic chemical properties of reference and witness materials is defined as the Contamination Knowledge (CK) of the sample collection. Unlike the data collected for Contamination Control (CC) and Planetary Protection (PP), CK is exclusively concerned with preserving reference and witness materials for study by future scientists upon sample return. Although CC and PP data collected for sample integrity and forward contamination purposes can be complementary to CK, they are two separate data sets with distinct objectives. A robust collection of samples for CK is necessary to allow the extraterrestrial material in a returned sample to be distinguished from terrestrial contamination. Traditionally CK is utilized by sample scientists in order to accomplish the mission’s scientific objectives, however this information can also be utilized by the Office of Planetary Protection to help evaluate the presence of any back contamination. Mars 2020, the first phase of a potential multipart Mars Sample Return (MSR) campaign, is expected to contribute to NASA’s Mars Exploration Program Science Goals by filling in knowledge gaps concerning: 1) the existence of past or present life on Mars, 2) the past and present climate of Mars, 3) the geology of Mars, and 4) hazards associated with human exploration of Mars. Although there is debate concerning which samples will best answer these questions, the necessity for proper sample blanks is well-understood. The CC and PP requirements, driven by the restricted Class V mission designation, are the most stringent of any sample return mission in recent history. The extremely low levels of allowable terrestrial contamination on the spacecraft and rover can complicate these analyses given the detection limits of current analytical instrumentation, especially in the case of biological contamination. By collecting and curating unanalyzed samples specifically for CK, future sample scientists will not be relegated to: 1) relying on data collected using possibly obsolete tools and techniques for return sample blanks, or 2) using remnants of extracted and/or cultured samples from ATLO (Assembly, Test, and Launch Operations), which could be incompatible with the desired experimental endpoints or state-of-the-art techniques available at the time of sample return.The addition of biological experimental endpoints to a sample return campaign’s objectives broadens the requisite range in preservation environments (e.g. inert ultra-pure nitrogen gaseous environment at 18 degrees Centigrade versus less than or equal to minus 80 degrees Centigrade) and types of CK samples. As a result, the Curation Office will also curate the following CK samples at less than or equal to minus 80 degrees Centigrade for the Mars 2020 mission: 1) unanalyzed swabs and wipes in sterile containers, 2) all recirculation filters from the clean rooms used for sample and caching subsystem assembly and all filters from the laminar flow benches used to assemble sample intimate hardware, and 3) witness plates collecting airborne contamination within the assembly clean rooms. It has been Curation Office policy since the Apollo missions to preserve as many pristine samples as possible for future scientific research. Although CK is required to be collected for all stages of the MSR campaign, the CK for the Mars 2020 mission is the most critical for understanding contamination in the returned samples given the intimacy between the Martian samples and the Mars 2020 flight hardware. This presentation highlights the importance of CK for sample return missions as well as the traditional and novel types of CK samples required for a successful MSR campaign.

Harrington, A. D.↗
DOE OSTI2023

Laboratory-Scale Coal-Derived Graphene Process (Final Report)

The Energy & Environmental Research Center (EERC) conducted a laboratory-scale coal-derived graphene (CDG) project focused on developing a technological process for making graphene from four U.S. domestic coal or coal wastes, including lignite from North Dakota, subbituminous coal from Wyoming, bituminous coal from Utah, and anthracite from Pennsylvania. The project was divided into two performance or budget periods (BPs), with BP1 comprising the up-front laboratory experiments to make graphene materials from coal beginning on May 1, 2020, to April 30, 2022. BP2 was conducted from May 1, 2022, to April 30, 2023, and was focused on analyzing the CDG process economic feasibility and the technical gaps for technological scale-up and commercialization. During this project, a few different coal-derived high-value products have been demonstrated, including graphite, graphene oxide (GO), reduced graphene oxide (rGO), and graphene quantum dots (GQDs). A new graphite microstructure was discovered and named “croissant graphite” because of the exterior morphological and textural resemblance to croissant food items sold in commercial groceries stores. The new graphite structure and the associated preparation from coal or coal waste feedstocks has been the subject of a U.S. patent application. The systematic experimental processes involving coal cleaning, upgrading, and conversion to high-value carbon products culminated into a developed upgraded coal-to-products (UCP) technology that is being pursued for potential fast-track commercialization, if funding is available. It is envisioned that commercialization of the UCP technology would increase consumption of U.S. domestic coals or coal wastes to make environmentally sustainable high-value products for the electronics industry, high-energy-storage applications, and clean energy technologies such as electric vehicle (EV) lithium-ion batteries (LIBs), for which graphite has become a critical mineral commodity. Croissant graphite microstructures, when observed by field emission scanning electron microscopy (FESEM), display wavy surface morphology and often grow from a base that is made of graphitized particles with honeycomb-like layers, which are believed to be graphene layers. While more studies are needed to fully ascertain the mechanisms of the croissant graphite microstructure formation, it is postulated that their growth may begin from curling of the graphene sheets into ribbon-like structures, and continuous growth and densification of the ribbon-like structures forms croissant microstructures. Additional studies are ongoing to evaluate the electrochemical performance of croissant graphite for LIB applications and to determine the experimental conditions necessary to tune on/off croissant formation so that it can be either optimized or suppressed depending on performance evaluation results. In addition to the discovery of croissant graphite, the graphitization process from the four coal ranks in general was successful. X-ray diffraction (XRD) analysis showed that the degree of graphitization (DoG) ranged from 12% to 80% in an early sample set, and further optimization on lignite coal produces a DoG of about 92%, which was spectacular to see as lignite is the lowest-rank coal. Thus, it is expected that the graphitization performance for higher-rank coals will be similar or better when optimized as well. The coal-derived graphite was used to make GO and rGO. Analytical characterization, e.g., by methods such as Raman spectroscopy, XRD, Fourier transform infrared (FTIR) spectroscopy and FESEM, showed that the sequence of converting the coal to graphite, exfoliating it to GO, and then chemically reducing the GO to rGO was successful. Although coal naturally contains aromatic compounds and some relatively small-sized condensed aromatic units, it does not contain graphene sheets. In the UCP process, the aromatic domains in the coals, particularly low-rank coals, are concentrated and condensed further into graphene sheets, which are ordered into a 3D stack during graphitization. The synthesized graphite is then unpacked by methods such as exfoliation to various graphene products. GQDs were synthesized from all four coal types, and their optical properties were demonstrated to be tunable by the coal precursor preprocessing treatments. In all four coal types, enhanced optical properties were observed for the produced GDQs with incremental improvements made to the coal precursors. GQDs produced from raw coal samples displayed lower ultraviolet–visible (UV–Vis) spectroscopy absorbance intensity compared to those obtained from cleaned and upgraded coal residues. The photoluminescence (PL) intensities also varied with pretreatment conditions and with the concentration of GQDs in aqueous solutions. GQDs obtained from anthracite show longer emission wavelengths and can be excited by visible light as opposed to GQDs derived from the other coal ranks. UV fluorescence 3D maps and spectra revealed that the emission wavelength at which the GQDs solutions display the highest intensity was slightly redshifted based on the coal precursor pretreatments. In low-rank coal (lignite and subbituminous) samples, two clusters were observed in the maps for GQDs, which may suggest that there are potentially two types of fluorophores in solution or two main size populations. The ability to tune the properties of GQDs based on processing methods can be exploited to make GQDs for various optical display or optoelectronics applications. The results also highlight the importance of removing coal-borne impurities to improve the quality of the coal precursor for preparation of graphene products. Coal and/or coal wastes preprocessing methods were developed and applied to clean and upgrade the coal precursors prior to graphitization and subsequent conversion to graphene products. The preprocessing methods involve high specific-gravity separations, mineral acid cleaning (no hydrofluoric acid), and subsequent upgrading by reducing the coal-borne heteroatom (nitrogen, sulfur, and oxygen) content using proprietary chemical agents. Analytical characterization revealed that the preprocessing steps were successful, with ash reductions that range from 38% to 80% and residual ash content that was below the 5 wt% initial target. Based on proximate and ultimate analysis, the heteroatom reduction reactions produced upgraded coal residues with the oxygen content reduced by 8% to 24%, with additional reductions in the nitrogen and sulfur contents. An initial assessment of the waste streams from the UCP process shows very small to negligible environmental impact due to CO 2 , NO x , and SO x because most process steps are performed under inert atmosphere with argon. Consequently, reactive oxygen environments that tend to create these species are avoided. The inorganic and potentially hazardous species are released into aqueous waste streams that are easy to handle for proper disposal. The liquid waste streams were found to contain low-level concentrations of rare-earth elements (REEs), which could be concentrated and recovered as value-added by-products. Additionally, the volatile and gaseous fractions from carbonization and heat treatment contain useful organic compounds that can also be recovered as potential valuable by-products. Thus, the UCP technology is considered an environmentally sustainable and promising emerging technology for making high-value products from coal and coal wastes, with potential additional value-added by-products. Analysis of potential markets for the coal-derived carbon products shows a strong demand in both niche market sectors and across a wide variety of other industrial sectors. Graphite is currently considered a critical mineral commodity that has a large and growing demand in the LIB industry for EV applications. Based on data from Fortune Business Insights (2022) and Marketwatch (2023) reports, the average global graphite market is projected to reach about 33 billion by 2028, growing at a compound annual growth rate (CAGR) of about 7%, with much of this growth expected to be in the LIB industry. GO and rGO have strong market potentials in various application areas, such as coatings for anticorrosion, anti-icing, and antimicrobial protection, thermal barriers, wear resistance, sensors, additive manufacturing such as 3D inks, and others. GQDs are the emerging key player in the bioimaging, photovoltaics, and light-emitting diodes (LEDs) applications, with the potential to replace traditional semiconductor quantum dots (SQDs), which are based on metallic systems that are more toxic and more expensive. Biomedical applications of GQDs are becoming more attractive because of low to no toxicity and extremely low cost compared to SQDs. The major challenges for scale-up and commercialization of coal-derived carbon products such as graphene vary from the inherent attributes of graphene itself to reluctance to accept graphene in new manufacturing processes because of the uncertainty of the unknown. The 2D nature of graphene materials with a thickness of one atom presents significant challenges to proper handling/processing, and process scale-up becomes difficult because it requires high-end, expensive equipment, even for routine handling and analysis for quality assurance and control. Pristine graphene can also be extremely difficult to work into other matrices, thus hindering downstream processibility, especially at large scale. Currently, the cost of graphene and graphene products is still high and presents an economic risk that tends to slow down investment in scaling up emerging technologies. The lack of a standard for graphene materials for quality assurance and quality control poses a great challenge not only for the markets but also for commercialization efforts. A first-look economic feasibility analysis of the UCP technology provided valuable information that suggests the UCP process would be feasible, especially when it is scaled to a pilot scale and could be more competitive at the full scale. Graphitization was found to be the most energy-consuming and most capital-intensive step in the overall process. In small laboratory- and bench-scale experiments, labor is a significant contributor to the total process costs. Although these energy, capital, and labor constraints contribute to a higher selling price for the product, a preliminary economic model suggests that the process would be feasible at large scale when the process is fully integrated, optimized, and automated.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2025

Electronic Configurational Transformation of Network Modifiers in Aluminate Glass above Megabar Pressures

Electronic responses of glasses under extreme pressures differ from those of crystalline analogs. Their distinct electronic environments are found in network formers with well-defined, covalent-bonded coordination environments (e.g., [4] Si and [4] Al) and in network modifiers with more disordered, ionic-bonded configurations (e.g., [5,6,7] Ca). Deciphering the evolution of the bonding environment of network modifier cations upon compression provides atomic insights into the pressure-driven hardening and transport properties of glasses. Despite the importance, in contrast to extensive efforts to uncover how network formers behave under pressure, considerable structural disorder around network modifiers makes it challenging to probe their electronic bonding environments under compression. Our understanding of the evolution of network modifiers above megabars is currently absent. Here, we report a discovery of highly densified electronic configurations of network modifier Ca in aluminate glass under extreme compression via the first inelastic X-ray scattering at the Ca L-edge up to 140 GPa. As evidenced by the prominent pressure-driven increases in electronic dispersion and delocalization, densified calcium environments are characterized by a decreased average Ca–O distance, the formation of highly coordinated calcium, a broader distribution of topological variables, and a greater distortion of Ca polyhedra above megabars. The spectral features for the Ca environments reveal significant electronic and bonding modifications, including pressure-driven increases in the ligand field interaction, the covalence characteristic of the Ca–O bond, and the electron–hole Coulomb interaction. These densification paths identify the electronic adaptation of network modifiers above megabars, shedding light on the origins of enhanced electron transport and the electron-storing capacity of glasses under pressure.

amorphous materials↗
DOE OSTI2023

Development of pebble-based extruded carbon rods for extreme plasma heat flux environments

This work presents first experiments toward the development of continuously renewable (extrudable) pebble-based carbon rods for use as plasma-facing components in extreme steady-state plasma flux environments. The primary envisioned application of this work is a first wall that can survive long-term in future magnetic fusion power reactors while also improving recovery of the reactor fuel (tritium and deuterium atoms). Bench tests applying extreme steady-state front-surface heat loads of up to 50 MW/m 2 are presented. Continuous pebble rod front-surface recession and intact pebble recovery are successfully demonstrated, at a rate of order 0.2 cm/s. Numerical simulations of the pebble rod front-surface recession are able to match observations reasonably well, indicating that the recession mechanism can be understood as occurring due to pebble thermal expansion and resulting shock and cracking of the inter-pebble binder. Tests of the pebble rod extrusion demonstrate that friction between the rods and the stainless-steel extrusion channel is tolerably low (<50 N for the expected channel length) over a wide range of temperatures. Front-surface outgassing rates below 1000 Torr L/s/m 2 are achieved, believed to be sufficiently low for use in magnetic fusion reactors. In conclusion, initial parametric scans over pebble rod size and binder fraction to vary front-surface recession rates are presented.

36 MATERIALS SCIENCE↗
NASA NTRSDate not supplied

Active Volcanoes of Kamchatka as Suitable Terrestrial Analogs for Future Landing Missions and for Change Detection Analysis on Venus

The next decade will see the return to Venus due to a number of missions which have been recently selected and proposed for launch. The selected missions NASA DAVINCI and VERITAS, Roscosmos Venera-D, and ESA EnVision, along with the proposed missions ISRO Shukrayaan- 1, and CNSA VOICE, will open a new era for the exploration of the Earth’s hellish twin planet. These missions will shed new light on the science questions such as: (a) whether recent volcanic activity is locally constrained, or active volcanism occurs on a global scale; (b) the rate of the present-day volcanic activity; (c) the styles of volcanism on Venus, including possible occurrences of pyroclastic/explosive volcanism; and (d) how does the extreme environment on Venus effect volcanic activity. In preparation for these future missions to Venus, the Analogs for VENus’ GEologically Recent Surfaces (AVENGERS) initiative has the scope to select and analyze a number of active terrestrial volcanoes as suitable analogs for the identification and analysis of active volcanism on Venus. The Roscosmos Venera-D is the only mission, among the currently selected or planned mission, equipped with a lander to analyze the elemental and mineralogical composition of the surface. Therefore, it is crucial to find applicable volcanic areas on Earth to perform operational tests such as surface drilling and in-situ elemental composition analysis. To this regard, we propose the analysis of active volcanoes of the Kamchatka Peninsula, which is in a geodynamic setting (subduction) contrasting to that of the volcanic rises on Venus (hot spot). Thus, Kamchatka may represent a helpful geodynamic endmember to put the expected landing site of the Venera-D mission within the context of the entire variety of volcanic landforms and surface chemistry. The Kamchatka Peninsula is located on the eastern margin of the Eurasian plate, in proximity to the Kuril-Kamchatka subduction zone. The frequent eruptions characterizing the volcanoes of the Kamchatka Peninsula make them a suitable terrestrial analog for the possible detection of ongoing eruptions on Venus by future missions, which can be achieved by comparing a sequence of radar images of the same volcano and its surroundings taken at different times. Moreover, it is possible to collect samples of both unweathered and weathered volcanic deposits, to analyze their near infrared spectra in the laboratory for direct comparison with the spectra to be provided by the future missions to Venus. The chemical analyses of Venusian surface materials from the previous Soviet Venera and Vega missions are consistent with that of tholeiitic basalts. Since the volcanism of the Kamchatka Peninsula is characterized by both basaltic lava flows eruptions and pyroclastic activity, performing operational tests in the Kamchatka Peninsula also offers the unique opportunity to provide us the tools to potentially interpret the diverse output given by both effusive and explosive volcanic products.

Piero D'Incecco↗
DOE OSTI2022

High Velocity, Low‐Voltage Collective In‐Plane Switching in (100) BaTiO 3 Thin Films

Abstract Ferroelectrics are being increasingly called upon for electronic devices in extreme environments. Device performance and energy efficiency is highly correlated to clock frequency, operational voltage, and resistive loss. To increase performance it is common to engineer ferroelectric domain structure with highly‐correlated electrical and elastic coupling that elicit fast and efficient collective switching. Designing domain structures with advantageous properties is difficult because the mechanisms involved in collective switching are poorly understood and difficult to investigate. Collective switching is a hierarchical process where the nano‐ and mesoscale responses control the macroscopic properties. Using chemical solution synthesis, epitaxially nearly‐relaxed (100) BaTiO 3 films are synthesized. Thermal strain induces a strongly‐correlated domain structure with alternating domains of polarization along the [010] and [001] in‐plane axes and 90° domain walls along the [011] or [01] directions. Simultaneous capacitance–voltage measurements and band‐excitation piezoresponse force microscopy revealed strong collective switching behavior. Using a deep convolutional autoencoder, hierarchical switching is automatically tracked and the switching pathway is identified. The collective switching velocities are calculated to be ≈500 cm s −1 at 5 V (7 kV cm −1 ), orders‐of‐magnitude faster than expected. These combinations of properties are promising for high‐speed tunable dielectrics and low‐voltage ferroelectric memories and logic.

36 MATERIALS SCIENCE↗
NASA NTRSDate not supplied

Measuring the Wear and Abrasive Resistance of Air Plasma Sprayed Aluminum Oxide for Lunar Exploration

Lunar regolith, especially finer dust particles traveling at high velocities, can cause significant wear and abrasive damage to structural components that ensure a prolongated presence on the surface of the Moon. With the absence of an atmosphere and lower gravity than on Earth, regolith particles maintain high velocities at large distances from where they were generated, for example next to lunar landers. Wear-resistant ceramic and ceramic composite materials can improve the durability of spacecraft components during long missions on the Moon’s surface. Aluminum oxide coatings are lightweight, have multifunctional properties, and have high strength including high hardness and wear resistance. These properties can help improve the durability of structures used in space exploration. Air plasma sprayed (APS) aluminum oxide coatings have demonstrated the potential to protect critical structures. This study investigated the abrasive wear resistance of APS aluminum oxide coatings via Taber abrasion experiments. Taber abrasion offers the advantage of quantifying the abrasive wear behavior of particles with different shapes on a surface. In this work, an abrasive wheel made of silicon carbide was utilized to evaluate wear properties of specimens progressively over 5000 cycles. This experiment focused on testing two series of specimens to determine whether a bond coat composed of nickel, chromium, aluminum, and yttrium (NiCrAlY) improved the protective behavior of the APS aluminum oxide coating. The specimens varied in topcoat thickness and were made with and without an approximately 100 µm bond coat layer. The mass of the specimens was measured at 400 cycles, 800 cycles, 3800 cycles, and 5000 cycles. Increasing thickness was found to result in higher wear for samples with and without a bond coat. Increased mass loss in samples with a bond coat was observed indicating a need for further studies on the overall impact of the use of a bond coat on the protective behavior of the coatings. To continue designing wear resistant coatings for structural protection in space missions, the multifunctional properties of the APS aluminum oxide coating will be studied. Future experiments will determine whether the APS aluminum oxide coating can protect the structures from other aspects of the harsh space environment, such as extreme temperature variations and ionizing radiation.

aluminum oxide↗
DOE OSTI2023

Predicting oxidation damage of ultra high-temperature carbide ceramics in extreme environments using machine learning

Determining the oxidation resistance of UHTC carbides in extreme environments is challenging theoretically and experimentally due to the high dimensional complexity of influencing variables and intricate testing setups. Herein we demonstrate the use of machine learning (ML) models trained with experimental literature data to predict the oxide thickness of UHTC carbides exposed to air based on composition, mean grain size, relative densification, holding time, and temperature. A multi-dimensional database with 76 occurrences is created containing experimental results of Hf, Zr, and Ta carbides plus additives. In this study, the preprocessed database is then used to train ML models to predict their oxidation behavior. The trained model predicts the oxidation damage in the form of an average oxide thickness in UHTC carbides with a Mean Absolute Error (MAE) of ±65.45 μm for samples in the testing set that developed thicknesses up to 1000 μm. The model successfully predicted oxidation damage for a recession rate lower than 60 μm/min. It is noticed that the ensemble method MAE is increased to ±134.34 μm while forecasting the oxidation of samples with a recession rate higher than the threshold. The unprecedented approach is a novel way to predict the damage through the oxidation of carbide compounds before processing for a smarter design with room for improvement.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Wyandotte Integrated Renewable Energy Strategy (WIRES 2) (Final Technical Report)

Wyandotte Municipal Services (WMS), a Michigan Municipal Utility offering electric generation, transmission & distribution, water filtration & distribution and Broadband/Video sought to deploy a set of renewable energy projects for their Electric Utility that contributed to reducing the City’s environmental and energy impact, provided examples that would encourage businesses and citizens to adopt cleaner energy practices and help WMS meet the required renewable energy standards of the State of Michigan (10% in 2015, 15% in 2021). WMS generates and delivers roughly 280,000 megawatt hours (MWh) of electricity annually to more than 10,000 homes and 1,000 businesses within the City of Wyandotte. The Wyandotte Integrated Renewable Energy Strategy – WIRES 2 resulted in deployment of a set of community-scale micro-wind turbines, evaluation and installation of energy-efficient and low-maintenance light-emitting diode (LED) street lights and park lights in highly visible locations in the City and expansion of the geothermal heating and cooling district that already included residential geothermal systems, to include larger scale business/institutional systems at the Utility’s largest electric customer and at the City Library. Finally, WMS identified the need for job training in energy efficiency and renewable energy technologies to further develop a local skilled workforce in these areas. Partially funded by the grant, the wind turbine project provides a benchmark for WMS, local businesses and residents in the evaluation of utility-scale wind v. micro-wind in an urban environment as a renewable energy strategy. Also partially funded by the grant, the LED project benefited the City of Wyandotte by reducing load on the electric system for the public utility but also reduced City costs for streetlighting, parking lot lighting and park lighting without a compromise in security. The project also resulted in a visual success that has led to additional approvals for non-Grant related LED lighting installations resulting in further reduction in the electric load in the City. Commercial Geothermal installations resulted in the Utility being able to eliminate steam customers who formerly utilized the byproduct of steam from WMS electric production. Due to the reduction in natural gas prices and the overall reduction in market purchased power, it was no longer feasible for WMS to operate its Power Plant as a base load plant and to only operate on a market dispatch philosophy when market prices dictated that WMS could produce electricity cheaper than the market purchase price. This has resulted in fewer operating days for the WMS Power Plant, resulting in less environmental impact. WMS has now completely exited the steam business and the ability to offer a geothermal option to two (2) former steam customers (BASF-Wyandotte and the Bacon Memorial Library) allowed for that. In addition, peak loads have been shaved for these two (2) large customers due to the consistent temperature offered by geothermal heating and cooling, reducing the swings associated with thermostat changes caused by outside temperature changes during extreme high and low temperatures. Finally, energy efficiency and renewable energy college-level classes at Wayne County Community College allowed a group of interested students to pursue studies in those technologies through grant provided tuition, books and course materials. This effort provided a foundation of potential future employees not only for WMS but other energy efficiency/renewable energy employers such as Franklin Energy, a partner with WMS in energy optimization efforts with Wyandotte businesses.

17 WIND ENERGY↗
NASA NTRS2015

Layered Thermal Insulation Systems for Industrial and Commercial Applications

From the high performance arena of cryogenic equipment, several different layered thermal insulation systems have been developed for industrial and commercial applications. In addition to the proven areas in cold-work applications for piping and tanks, the new Layered Composite Insulation for Extreme Environments (LCX) has potential for broader industrial use as well as for commercial applications. The LCX technology provides a unique combination of thermal, mechanical, and weathering performance capability that is both cost-effective and enabling. Industry applications may include, for example, liquid nitrogen (LN2) systems for food processing, liquefied natural gas (LNG) systems for transportation or power, and chilled water cooling facilities. Example commercial applications may include commercial residential building construction, hot water piping, HVAC systems, refrigerated trucks, cold chain shipping containers, and a various consumer products. The LCX system is highly tailorable to the end-use application and can be pre-fabricated or field assembled as needed. Product forms of LCX include rigid sheets, semi-flexible sheets, cylindrical clam-shells, removable covers, or flexible strips for wrapping. With increasing system control and reliability requirements as well as demands for higher energy efficiencies, thermal insulation in harsh environments is a growing challenge. The LCX technology grew out of solving problems in the insulation of mechanically complex cryogenic systems that must operate in outdoor, humid conditions. Insulation for cold work includes equipment for everything from liquid helium to chilled water. And in the middle are systems for LNG, LN2, liquid oxygen (LO2), liquid hydrogen (LH2) that must operate in the ambient environment. Different LCX systems have been demonstrated for sub-ambient conditions but are capable of moderately high temperature applications as well.

thermal conductivity↗
DOE OSTI2025

NSUF RTE completion report for 23-4780: Microstructural Defect Induced Thermal Conductivity Reduction in Uranium Nitride and Thorium Nitride

Uranium nitride (UN) is known to have a higher thermal conductivity than traditional oxide fuels, which could lead to a more efficient energy transport and lower local temperature during its lifetime. But the thermal transport performance of UN in extreme environments has not been systematic studied. This study investigated the irradiation induced microstructural defects in UN and the impacts on thermal conductivity. The samples were produced by spark plasma sintering at University of Texas-San Antonio (UTSA), Los Alamos National Laboratory (LANL), and Idaho National Laboratory (INL). Thermal conductivity of UN before and after 2MeV proton irradiation were measured by using laser metrology at INL in a temperature range of 77-295K. Thermal conductivity measurements in this wide, cryogenic temperature range is critical to understand the phonon scattering mechanisms between the thermal energy carrier, phonons, and different types of irradiation-induced defects. In order to ensure the measurements were conducted in the same grains and minimize the impact of the local heterogeneities, the measurement locations were highlighted by fiducial marks using the focused ion beam (FIB) with grain orientation identified using the electron backscatter diffraction (EBSD) at the Center of Advanced Energy Studies (CAES). Irradiation experiment was conducted at the Ion Beam Laboratory at Texas A&M University (TAMU). A total of 6 samples were irradiated with different irradiation doses and temperatures. After irradiation, the microstructure was characterized by using Transmission Electron Microscope (TEM) at CAES (also in the FIB marks).

36 - MATERIALS SCIENCE↗
DOE OSTI2021

Enhanced oxidation resistance of (Mo 95 W 5 ) 85 Ta 10 (TiZr) 5 refractory multi-principal element alloy up to 1300°C

Refractory-metal-based alloys are a potential replacement of current nickel-based superalloys due to their excellent mechanical strength at extremely high temperatures. However, severe oxidation in a high-temperature working environment limits their application. To address this challenge, a two-step coating process (including a Mo precoat and a Si-B pack cementation) was applied to an innovative refractory multi-principal element alloy (RMPEA) (Mo 95 W 5 ) 85 Ta 10 (TiZr) 5 . The coating is composed of an aluminoborosilica glass layer on top of a RMPEA-Si-B multilayered structure. Here, the coating effectively protects the RMPEA from oxidation in high-temperature environments, as demonstrated by phase-stable operation at 10–20% higher temperatures over state-of-the-art systems without any forced-cooling system. Following an isothermal exposure at 1300 °C, the weight change of the coated sample follows a paralinear kinetics with a minor weight loss of 4.2 mg/cm 2 after 50 h. Thermal cycling tests between 1300 °C and room temperature in air resulted in the total weight gain of only 2.6 mg/cm 2 after 450 cycles. The coating shows an excellent adherence to the substrate with a boride layer acting as a barrier that maintains the coating integrity. This two-step Mo-Si-B coating method can be adapted to provide environmental resistance to a wide range of RMPEA.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Exploring the impact of multivalent substitution on high-temperature electrical conductivity in doped lanthanum chromite perovskites: An experimental and ab-initio study

Doped LaCrO 3 perovskites hold promise as robust materials for electrical interconnects and sensor applications in harsh environments. In this work, we investigated the high-temperature behavior of La 1–x Sr x CrO 3 , La 1–x Ca x CrO 3 and La 0.8 Sr 0.2 Cr 1-x Mn x O3 (0.1 ≤ x ≤ 0.4) through a combination of computational modeling and physical characterization up to 1500 °C. Crystalline structural properties were determined and compared with ab-initio calculations, which demonstrated excellent agreement with experimental findings. High-temperature electrical conductivity measurements were performed under different atmospheres. Calcium and strontium/manganese co-doped lanthanum chromites exhibited typical semiconductor exponential trends and conductivity showed proportional correlation with substitutions levels up to 30 %. The DFT modelling was completed up to 1500 °C, including low and high temperature chromite phases and oxygen vacancies insertion. Calculations were correlated with experimental electrical properties. This work expands the understanding of doped lanthanum chromites and paves the way for the development of materials suitable for demanding high-temperature applications.

20 FOSSIL-FUELED POWER PLANTS↗
DOE OSTI2019

Alloying effects on low-energy recoil events in concentrated solid-solution alloys

Alloying elements at low-concentrations into pure metals is usually adopted to improve their mechanical properties and irradiation performance. Recently developed single-phase concentrated solid-solution alloys (CSAs) comprised of two or more elements, all at high concentrations, have demonstrated good radiation resistance. CSAs are characterized by their extreme disordered states that arise from the random arrangement of different elements and accompanied random local lattice distortions. In this work, we investigate low-energy recoil events in Ni 0.5 X 0.5 (X = Fe and Co) CSAs and Ni 0.8 X 0.2 (X = Fe, Co, Cr, and Pd) CSAs using ab initio molecular dynamics simulations to understand the effects of different disorder on defect production in CSAs. The threshold displacement energies are determined along three high-symmetric directions by randomly choosing independent primary knock-on atoms in each direction. As expected, the threshold energies in Ni and its CSAs are anisotropic, with the highest values found in the [111] direction. The calculated threshold energies of Fe in NiFe are smaller than those in NiCo and Ni, especially along the [111] direction. An inspection of the atomic trajectories inside the collision cascade reveals that the effect of chemical disorder outweighs the site-to-site lattice distortions in determining the threshold energies. Especially, different interaction properties between elements due to their different electronic structures are responsible for the observed different threshold energies. Finally, the local environment dependence of threshold energies suggests that local elemental arrangement can be used to understand and predict threshold energies in disordered alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Optimizing Insulation Design for Transformers in Medium Voltage Power Conversion Systems

Medium-frequency transformers (MFTs) play a crucial role in medium-voltage (MV) solidstate transformer (SST) systems, particularly in extreme fast charging applications. Achieving partial discharge (PD)-free operation while maintaining high power density is a significant challenge due to the high electric field (E-field) stresses inherent in MV applications. This dissertation focuses on the insulation design and optimization of MFTs used in both the main power electronics circuits and auxiliary power supplies. The study begins with an overview of insulation testing methodologies, including high potential tests, basic insulation level tests, and PD tests, which are critical for evaluating MFT insulation reliability. Given the importance of PD-free operation for long-term reliability, particular emphasis is placed on understanding PD mechanisms, including void, corona, and surface discharge, and their mitigation strategies. A high voltage isolated auxiliary power supply is then introduced, utilizing a gapped transformer encapsulated in silicone gel. This design achieves PD-free insulation up to 18 kV RMS while maintaining low coupling capacitance to minimize common-mode current. The proposed solution ensures reliable operation in MV environments and offers a scalable approach for auxiliary power in cascaded SST architectures. To improve MFT insulation in main power conversion circuits, a novel structure is developed using polypropylene sheets and potting compounds to create a void-free air gap, effectively mitigating E-field intensity. A prototype transformer with this insulation structure is built and achieves PD-free operation up to 30 kV RMS. This design is experimentally validated in a resonant converter operating at 46 kW, demonstrating its feasibility for MV SST applications. Further optimization is implemented to enhance MFT performance for dual-active-bridge(DAB) converters by integrating a semiconductive shielding layer within the insulation structure. This shielding layer improves the magnetic coupling coefficient while effectively confining the E-field within high insulation materials, thereby reducing eddy current losses. The optimized MFT achieves PD-free operation at 12.6 kV RMS and is successfully tested in a DAB converter operating at 43 kW, which meets the insulation requirements for a 13.2 kV SST system. This dissertation advances MFT insulation design by introducing and experimentally validating novel approaches that improve high voltage insulation while optimizing magnetic coupling and manufacturability. The proposed insulation structures enable PD-free operation while minimizing insulation material usage and simplifying assembly, making them ideal for high power, high voltage applications.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2024

On the Mechanical Behavior of LP-DED C103 Thin-Wall Structures

Laser Powder Directed Energy Deposition (LP-DED) can produce thin-wall features on the order of 1 mm. These features are essential for large structures operating in extreme environments such as regeneratively cooled nozzles and heat exchangers, which often make use of refractory metals. In this work, the mechanical behavior of LP-DED C103 was investigated via quasi-static tensile testing and low cycle fatigue (LCF) testing. The effects of vacuum stress relief (SR) and hot isostatic pressing (HIP) heat treatments were investigated for specimens in the vertical and horizontal build orientations during tensile testing. The AB and SR properties were lower than literature values for wrought and laser powder bed fusion (L-PBF) bulk components but higher than electron beam powder bed fusion (EB-PBF). The application of a HIP cycle improved strength by 7% and ductility by 27% past the initial as-built condition. Fracture images reveal that interlayer stress concentration sites are responsible for fracture in specimens in the vertical orientation. Meanwhile, fracture in the horizontal specimens mainly propagates at a slanted angle typical of plane stress conditions. The LCF results show cycles to failure ranging from 100 cycles to 8000 cycles for max strain levels of 2% and 0.5%, respectively. Fractography on the fatigue specimens reveals an increasing propagation zone as max strain levels are increased. The impact of these findings and future work are discussed in detail.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Machine learning assisted prediction of tungsten heavy alloy plasma facing component performance for fusion energy applications

Tungsten and tungsten heavy alloys (WHAs), known for their remarkably high hardness, durability, and corrosion resistance, play a critical role in the thriving development of nuclear fusion reactors in recent years. However, the exploration in tungsten alloys for the nuclear-related applications has been limited by the difficulty of manufacturing and the complexity of experiments to reproduce the environment of nuclear reaction. Therefore, this project aims to utilize nanoscale simulation methods such as density functional theory (DFT) and molecular dynamics (MD) with the help of machine learning techniques to not only understand the mechanisms of tungsten alloys but also allow us to computationally predict their mechanical behaviors under extreme environments. One critical problem of the application of WHAs in nuclear reactors is the surface melting. In the current design of the SPARC reactor, the WHA, W97Ni2.1Fe0.9 or W97NiFe, is chosen to be the first wall components to confine the plasma where the particles are fiercely moving and colliding into each other to create nuclear fusion reaction. This process will generate extremely high heat flux onto these WHA tiles, leaving high surface temperature that could possibly melt the surface of the WHA tiles, As illustrated in Fig. 1(a). a laser experiment previously done illustrates that a rough surface damage would be made after the surface melting where the matrix area mainly composed of nickel and iron as shown in Fig. 1(b), will first melt and then leave vacancies between these tungsten grains. Unfortunately, these kinds of roughness on the first-wall components could be deadly to the plasma inside a Tokmak reactor because the heat that is supposed to dissipate at a designed ratio through the tiles may in turn be excessively absorbed and accumulated on any uneven area of the surface, which will eventually make the whole nuclear reaction fail. In this project, we will introduce a machine learning potential, Allegro, based on DFT calculation and then build a MD model for W-Ni-Fe alloys.

36 MATERIALS SCIENCE↗
NASA NTRSDate not supplied

Initial Results of the MISSE-Flight Facility Polymers and Composites Experiment 1-4 (PCE 1-4)

Spacecraft in low Earth orbit (LEO) are subjected to harsh environmental conditions, including radiation (cosmic rays, ultraviolet (UV), x-ray and charged particle radiation), micrometeoroids and orbital debris, temperature extremes, thermal cycling, and atomic oxygen (AO). These environmental exposures can result in erosion, embrittlement and optical property degradation of susceptible materials threatening spacecraft performance and durability. To increase our understanding of effects such as AO erosion and radiation induced embrittlement of spacecraft materials, NASA Glenn Research Center has developed a series of experiments that are flown as part of the Materials International Space Station Experiment (MISSE) missions on the exterior of the International Space Station (ISS). These experiments have provided critical space environmental durability data such as AO erosion data of polymers and composites, and radiation induced mechanical property degradation of spacecraft insulation materials, after long term space exposure. In continuing these studies, four Glenn experiments with 365 flight samples have been flown on ISS’s external MISSE-Flight Facility (MISSE-FF). These experiments are the Polymers and Composites Experiment-1 (PCE-1) flown as part of the inaugural MISSE-9 mission, the PCE-2 flown as part of the MISSE-10 mission, the PCE-3 flown as part of the MISSE-12 and MISSE-15 missions, and the PCE-4 flown as part of the MISSE-13 mission. The primary objective of the PCE 1-4 experiments is to determine the AO and radiation durability of spacecraft polymers and composites. In addition, each experiment has a wide variety of spacecraft materials and hence they each have numerous additional sample objectives. Each of the PCE 1-4 is designed to examine the consequences of AO interactions including AO erosion yield (Ey) and optical and thermal property characterization. Several polymers were flown in both ram and zenith flight orientations to determine the effect of varying solar to AO ratios on Ey. Common spacecraft materials including Teflon FEP, white Tedlar and Upilex-S were included on multiple MISSE missions so erosion dependence on environment exposure can be determined. The PCE-1 includes epoxy composite samples with varying ZnO levels to determine the effect of inorganic filler level on AO durability. And, a variety of samples were flown to characterize AO scattering and AO undercutting processes. All four PCE experiments include samples to provide better insight into radiation durability of polymers and composites. The MISSE-9 PCE-1 includes Teflon FEP tensile samples flown in the wake and zenith direction so variations in radiation exposure from the different flight directions can provide insight into radiation induced embrittlement of Teflon FEP. Teflon FEP tensile samples were also flown in the wake direction as part of the MISSE-13 PCE-4. In addition, shape memory alloys, shape memory composites, melanin based composites, stressed and unstressed gossamer sun shield materials, coated and uncoated docking seal samples, and new solar cell cover slides were flown for space radiation durability and/or shielding assessment. This paper provides an overview of Glenn’s PCE 1-4 MISSE-FF experiments and provides initial post-flight observations and results.

atomic oxygen↗