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DOE OSTI2022

Europium diffusion in IG-110 nuclear graphite

Europium diffusion in graphite has been recognized to be of interest in high-temperature gas reactor safety analysis, particularly as an indicator of strontium diffusion. However, no measurements of europium diffusion coefficients have been reported in the literature. In this work, the effective diffusion coefficient of europium was measured using a time-release method. Natural europium was loaded into pre-milled unirradiated IG-110 graphite spheres using a pressurized acid digestion vessel. The time-release experiments were performed in the temperature range 1823 K – 1973 K using a SiC diffusion cell connected to an inductively-coupled plasma mass spectrometer (ICP-MS) via a He gas line. Finally, the results of this work are: D Eu, IG-110 = (1.5 x 10 -3 m 2 /s) exp $(\frac{-2.87\mathrm{x}10^{5} J/mol}{RT})$ This effective diffusion coefficient can be used to aid in predictive modelling of europium transport in HTGRs.

36 MATERIALS SCIENCE↗

NASA NTRS1981

Electrochemical Energy Storage for an Orbiting Space Station

The system weight of a multi hundred kilowatt fuel cell electrolysis cell energy storage system based upon alkaline electrochemical cell technology for use in a future orbiting space station in low Earth orbit (LEO) was studied. Preliminary system conceptual design, fuel cell module performance characteristics, subsystem and system weights, and overall system efficiency are identified. The impact of fuel cell module operating temperature and efficiency upon energy storage system weight is investigated. The weight of an advanced technology system featuring high strength filament wound reactant tanks and a fuel cell module employing lightweight graphite electrolyte reservoir plates is defined.

Martin, R. E.↗

DOE OSTI2024

Synthesizing Highly Crystalline Graphite Powder from Bulk Polyethylene Waste for Lithium-Ion Battery Anodes

Upcycling plastic waste into graphite can potentially be used, in conjunction with other methods, to manage existing waste materials and diversify graphite supply chains. However, synthesizing large quantities of crystalline graphite powder from plastic waste, particularly polyethylene (PE), remains a challenge because PE decomposes into light gases during thermal processing, and simple methods do not exist at any appreciable size scale to address this challenge. In this work, a method is developed for air processing bulk forms of PE waste to create a stable carbon char that does not readily decompose during high-temperature processing. This method employs solid additives in the form of salts, which are combined with the PE melt during air processing to increase the effective surface area of the melt and improve the oxygen-driven chemistry that stabilizes the PE for high-temperature processing. After removing the solid salt additives from the PE-derived char, it is converted into a highly crystalline bulk graphite powder using a Fe-based low-temperature (<1500 °C) catalytic process. The PE-derived graphite powder showed excellent electrochemical performance as an anode material for lithium-ion batteries (LIBs) with a capacity of up to 302 mAh/g at 0.5 discharge/charge cycles per hour (0.5 C) and capacity retention of 100% after 415 cycles. This method illustrates there are opportunities for upcycling large quantities of PE waste to produce graphite powders.

Huynh, Ngoc Tien [NETL Site Support Contractor, Na↗

DOE OSTI2023

NanoMechanics: Elasticity and Friction in Nano‐Objects

A large scientific and technological effort is underway to investigate the properties of two‐dimensional (2D) materials to become building blocks in integrated nano‐electronic and photonic circuits, composites, coatings, energy harvesting nano‐ systems, nano‐sensors, and nano‐electro‐mechanical systems (NEMS).While several experiments and calculations have revealed exciting novel phenomena in these nanostructures, many scientific and technological questions remain open. In particular, understanding and controlling the structure and mechanical properties of 2D materials at the interface with a solid surface is of key importance to enable the aforementioned nanotechnologies, as well as to fulfill the potential of strain engineering to tailor their properties. The vision of this DoE research program was to investigate novel mechanical properties and phenomena in 1D and 2D materials with the overarching goal of defining a new basic understanding of mechanical behavior in nano and quantum systems. The group of the PI has developed in the last years several studies on the mechanical properties of Carbon nanotubes and oxide nanobelts, more recently the PI has focused her attention on the properties of two‐dimensional materials, such as graphene and MoS 2 , which are a few‐atomic‐layer thick films and hold a great potential for technological and energy applications. The most studied 2D material is graphene, existing as a single layer of graphite or a few‐layer thick epitaxial graphene film. Graphene possesses a large in‐plane Young’s modulus as well as high intrinsic carrier mobility, and high in‐plane thermal conductivity. Besides graphene, also 2D films of graphene oxide (GO), hexagonal Boron Nitride (h‐BN), and transition metal dichalcogenides such as MoS 2 exhibit unique and excellent properties and hold great promise for nanotechnology applications. This research program was aimed at developing a new basic understanding of the mechanical properties of 1D and 2D materials at the interface with solid substrates, with a focus on the role of defects, materials structure, and substrate interaction. Ultimately, we aimed at developing the basic knowledge and experimental tools for manipulating 1D and 2D materials’ structure, stacking, substrate interaction, defects, and number of layers to realize an entirely new class of ultra‐hard, ultra‐thin, and ultra‐light active materials with ad‐ hoc mechanical properties for a variety of applications.

2D Materials↗

NASA NTRS1983

Alkaline fuel cells for the regenerative fuel cell energy storage system

The development of the alkaline Regenerative Fuel Cell System, whose fuel cell module would be a derivative of the 12-kW fuel cell power plant currently being produced for the Space Shuttle Orbiter, is reviewed. Long-term endurance testing of full-size fuel cell modules has demonstrated: (1) the extended endurance capability of potassium titanate matrix cells, (2) the long-term performance stability of the anode catalyst, and (3) the suitability of a lightweight graphite structure for use at the anode. These approaches, developed in the NASA-sponsored fuel cell technology advancement program, would also reduce cell weight by nearly one half.

Martin, R. E.↗

NASA NTRS1992

Structural testing of the technology integration box beam

A full scale section of a transport aircraft wing box was designed, analyzed, fabricated, and tested. The wing box section, which was called the technology integration box beam, contained blade stiffened covers and T-stiffened channel spars constructed using graphite-epoxy materials. Covers, spars, and the aluminum ribs were assembled using mechanical fasteners. The box beam was statically tested for several loading conditions to verify the stiffness and strength characteristics of the composite wing design. Failure of the box beam occurred at 125 pct. of design limit load during the combined unbending and torsion ultimate design load test. It appears that the failure initiated at a stiffener runout location in the upper cover which resulted in rupture of the upper cover and portions of both spars.

Griffin, C. F.↗

NASA NTRS1997

Compressor Case Manufactured Using High-Temperature Polyimides

High-temperature polymer composites (PMC's) offer lighter weight and higher specific strengths than titanium alloys for advanced aircraft engine applications-especially in fan and compressor components, where temperatures do not exceed 550 F (288 C). VCAP, a polyimide resin developed at the NASA Lewis Research Center, was filament wound at Lincoln Composites in Lincoln, Nebraska, with graphite and glass fibers to produce a lightweight compressor case for an Integrated High Performance Turbine Engine Technology (IHPTET) engine. This engine application requires a PMC that can withstand air pressures (60 psi) and temperatures exceeding the degradation limits of other high-temperature polyimides, such as PMR-15.

Sutter, James K.↗

NASA NTRS2012

Composite with In Situ Plenums

A document describes a high-performance thermal distribution panel (TDP) concept using high-conductivity (greater than 800 W/mK) macro composite skin with in situ heat pipes. The processing technologies proposed to build such a panel result in a one-piece, inseparable assembly with high conductance in both the X and Y planes. The TDP configuration can also be used to produce panels with high structural stiffness. The one-piece construction of the TDP eliminates the thermal interface between the cooling plenums and the heat spreader base, and obviates the need for bulky mounting flanges and thick heat spreaders used on baseline designs. The conductivity of the TDP can be configured to exceed 800 W/mK with a mass density below 2.5 grams per cubic centimeter. This material can provide efficient conductive heat transfer between the in situ heat plenums, permitting the use of thinner panel thicknesses. The plenums may be used as heat pipes, loop heat pipes, or liquid cooling channels. The panel technology used in the TDP is a macro-composite comprised of aluminum-encapsulated annealed pyrolytic graphite (APG). APG is highly aligned crystalline graphite with an in-plane thermal conductivity of 1,700 W/mK. APG has low shear strength and does not constrain the encapsulating material. The proposed concept has no thermal interfaces between the heat pipes and the spreader plate, further improving the overall conductance of the system. The in situ plenums can also be used for liquid cooling applications. The process can be used to fabricate structural panels by adding a second thin sheet.

Montesano, Mark↗

NASA NTRS1982

Component technology for space power systems

Progress made by NASA toward implementation of equipment for the conversion, management, and distribution of voltage power in space applications are reviewed. Work has been carried forward on components such as bipolar transistors, deep impurity semiconductors, conductors, dielectrics, magnetic devices, and rotary power transfer. Specific programs for the high voltage systems have included research on lightweight, low-cost conductors featuring graphite fibers containing electron donor materials for wires and cables with reduced mass and the conductivity of copper. Attention has also been given p-n junction technology for high-speed, high-current, high-voltage materials and diamond-like dielectric films which are hard, have high dielectric strength, and can operate up to 300 C. A transistor has been fabricated with a voltage of 1200 V at 100 A, with a gain of 10 and a 0.5 microsec rise/fall time. A 25 kW transformer has also been built which performs at 20 kHz with an efficiency of 99.2%.

Finke, R. C.↗

NASA NTRS1998

Power Management and Distribution System Developed for Thermionic Power Converters

A spacecraft solar, bimodal system combines propulsion and power generation into a single integrated system. An Integrated Solar Upper Stage (ISUS) provides orbital transfer capabilities, power generation for payloads, and onboard propulsion to the spacecraft. A key benefit of a bimodal system is a greater payload-to-spacecraft mass ratio resulting in lower launch vehicle requirements. Scaling down to smaller launch vehicles increases space access by reducing overall mission cost. NASA has joined efforts with the Air Force Phillips Laboratory to develop enabling technologies for such a system. The NASA/Air Force bimodal concept uses solar concentrators to focus energy into an integrated power plant. This power plant consists of a graphite core that stores thermal energy within a cavity. An array of thermionic converters encircles the graphite cavity and provides electrical energy conversion functions. During the power generation phase of the bimodal system, the thermionic converters are exposed to the heated cavity and convert the thermal energy to electricity. Near-term efforts of the ISUS bimodal program are focused on a ground demonstration of key technologies in order to proceed to a full space flight test. Thermionic power generation is one key technology of the bimodal concept. Thermionic power converters impose unique operating requirements upon a power management and distribution (PMAD) system design. Single thermionic converters supply large currents at very low voltages. Operating voltages can vary over a range of up to 3 to 1 as a function of operating temperature. Most spacecraft loads require regulated 28-volts direct-current (Vdc) power. A combination of series-connected converters and powerprocessing boosters is required to deliver power to the spacecraft's payloads at this level.

Baez, Anastacio N.↗

NASA NTRS1998

Next Generation Space Telescope Ultra-Lightweight Mirror Program

The Next Generation Space Telescope is currently envisioned as a eight meter diameter cryogenic deployable telescope that will operate at the earth sun libration point L2. A number of different designs are being examined within NASA and under industry studies by Ball Aerospace, Lockheed-Martin and TRW. Although these designs differ in many respects, they all require significant advancements in the state-of-the-art with respect to large diameter, ultra-lightweight, mirrors. The purpose of this paper is to provide insight into the current status of the mirror development program NGST is a tremendously ambitious undertaking that sets the mark for new NASA missions. In order to achieve the weight, cost and performance requirements of NGST, the primary mirror must be made lighter, cheaper and better than anything that has ever been done. In order to accomplish this an aggressive technology program has been put in place. The scope of the program was determined by examining historically what has been accomplished; assessing recent technological advances in fabrication and testing; and evaluating the effect of these advances relative to enabling the manufacture of lightweight mirrors that meet NGST requirements. As it is currently envisioned, the primary mirror for NGST is on the order of eight meters in diameter, it is to be diffraction limited at a wave length of 2 microns and has an overall weight requirement of 15 kilograms per square meter. Two large scale demonstration projects are under way along with a number of smaller scale demonstrations on a variety of mirror materials and concepts. The University of Arizona (UA) mirror concept is based around a 2mm thick Borosilicate glass face sheet mounted to a composite backplane structure via actuators for mirror figure correction. The Composite Optics Inc.(COI) concept consists of a 3.2mm thick Zerodur face sheet bonded to a composite support structure which in turn is mounted to a composite backplane structure via actuators for mirror phasing. These mirrors are due to be performance tested in ambient conditions in the fall of '98, and cryogenically tested in the spring of '99. The smaller scale efforts include the following: Beryllium is being investigated at Ball Aerospace, Electroform nickel is being investigated in-house at MSFC, Chemical Vapor Deposition (CVD) Silicon Carbide (SiC) is being investigated at Morton International Silicon mirrors are being investigated at Schafer, Carbon Fiber Reinforced Silicon Carbide (CSIC) is being investigated at IABG. SiC at SSG, Composite mirrors at COI, pyrolyzed graphite mirrors at Ultramet, reaction bonded SiC mirrors at Xinetics, along with techniques for lightweighting using waterjets at Waterjet Technology Inc. are all being investigated under the Small Business innovative Research Program SBIR program. A procurement for a third large scale demonstration (nominally 1.5m in diameter) is being planned for release this fall.

Bilbro, James W.↗

DOE OSTI2025

Upcycling Polyethylene Waste into Hybrid Graphitic Porous Carbon Materials Used in High‐Performance Zinc‐Ion Hybrid Capacitors

Polyethylene (PE) waste is a challenge to upcycle into useful materials because this plastic tends to decompose into volatile compounds when heated at relatively low temperatures. In this work, mixtures of PE wastes into a hybrid graphitic porous carbon (HGPC) by a thermal oxidation pretreatment step, with assistance of an inert solid additive (KCl), to functionalize, crosslink, and stabilize the PE waste followed by carbonization and catalytic graphitization steps with a potassium carbonate catalyst, are upcycled. The PE waste‐derived HGPC (PW‐HGPC) has a hybrid structure composed of graphene‐like carbon nanosheets grown on the surface of carbon particles, high porosity with specific surface area, up to 1,763 m 2 g −1 , and good graphitic degree with average Raman I 2D / I G ratios of 0.53. When used as cathode material for zinc‐ion hybrid capacitors, this PW‐HGPC exhibits an excellent specific capacity, up to 126.7 mAh g −1 , at high mass loading of 10 mg cm −2 . Moreover, PW‐HGPC exhibits remarkable cycling stability with capacity retention of >94% after 10 000 cycles. Additionally, the KCl is recycled and reused over five times. This method provides a new solution for upcycling PE wastes into high value‐added carbon materials, not only for zinc‐ion hybrid capacitors but also for other electrochemical energy storage device applications.

hybrid graphitic porous carbon↗

DOE OSTI2024

Production of Carbon Nanomaterials and Sorbents from Domestic U.S. Coal (Final Report)

The main goal of this project was to produce high-value carbon nanomaterials and carbon sorbents from domestic coal resources in a cost-effective manner. Four types of domestic coal samples were processed through a combination of deashing, devolatilization, oxidation, reduction, and activation treatments to produce graphene oxide (GO), reduced graphene oxide (RGO), and activated carbon (AC). The precursors and developed materials were extensively characterized by various methods to investigate the impact of the coal feedstock type on the yield and quality of each product. A commercial graphite-based GO sample was included in the experimental work as the baseline material for comparison with the coal-based materials developed in this work. The performed work also included a technoeconomic analysis and cost estimation for a plant processing 20 tons/day coal, a market evaluation for the graphene materials, and a technology gap analysis. A simple process by concentrated nitric acid oxidation is used to oxidize coal precursors for the production of GO. Fine oxidized coal particles that were separated from larger oxidized coal particles had significantly higher oxygen contents and were identified as coal-based GO samples. Coarse oxidized coal particles were used as precursors for production of AC. Based on the Raman spectroscopy results, coal-based GO samples exhibited G and D bands similar to those of graphite-based GO samples. X-ray photoelectron spectroscopy revealed that coal-based GO samples had surface oxygen contents of ~26-35% that were higher than the oxygen contents of graphite-based GO samples. Larger particles of oxidized coal samples were activated under different conditions to produce high surface area functionalized AC. Prepared materials had surface areas exceeding 1,500 m 2 /g and pore volumes more than 1 cm 3 /g with different pore size distributions. Reduced graphene oxide samples were prepared by thermal reduction of both coal-based and graphite-based GO samples at 170-2800 ºC. Coal-based and graphite-based RGO samples exhibited similar carbon contents, Raman spectra, and XRD profiles. Heat treatment above 1500 ºC shifted RGO to synthetic graphite. Among anthracite, bituminous, subbituminous, and lignite coals tested, anthracite was the best precursor to produce carbon nanomaterials exhibiting properties similar to those of graphite-based materials. Anthracite-based carbon nanomaterials also had the highest production yields. Technoeconomic analysis estimated the production cost of GO and RGO for anthracite-based samples at about 2,600 and 4,200 $/ton, respectively, which is about two orders of magnitude lower than the current estimated price of graphite-based materials. Several gaps to further develop the proposed technology were identified and discussed that include process and equipment optimization, process integration, need for additional bench- and pilot-scale experiments, and other items to reduce the scale up risk. Market analysis reports suggested a compound annual growth rate of 40% for graphene and related materials. Short-term applications include composites, inks, and coatings. However, energy storage applications appear to be the dominant potential long-term applications. Different applications of coal-based GO and RGO need to be explored and clear metrics and standards for each application need to be developed.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2025

A cradle-to-grave life-cycle-assessment of dry-processed Li-ion batteries for electric vehicles

Maxwell-type dry processing has emerged as a promising manufacturing technology for high-areal-loading Li-ion battery electrodes, offering a significant advantage by eliminating the use of the toxic and costly NMP solvent. This study developed a cradle-to-grave life-cycle-assessment model to evaluate the environmental impacts of this innovative technology, benchmarking the results against the conventional NMP-based technique for a configured 42 kWh NMC622-graphite battery pack. Furthermore, the findings reveal that the dry-processing method merits a 4.8% lower energy consumption and achieves environmental impacts up to 47.5% lower in 12 out of 13 categories, highlighting its environmental benefits compared with the NMP-based manufacturing processes.

Electrode↗

DOE OSTI2020

Tin asymmetric membranes for high capacity sodium ion battery anodes

Sodium-ion batteries have attracted tremendous research attention as promising candidates for next generation energy storage systems due to low-cost and high abundancy. Furthermore, comparing to current Li-ion battery technology, limitations on the anode side seriously hinder the cell performance since sodium does not easily intercalate into graphite materials. Here, tin nanoparticles embedded in various asymmetric membrane structures were developed to leverage the high capacity of tin (847 mA h g -1 based on Na 15 Sn 4 ) and accommodate the significant volume expansion for long cycle life. It was demonstrated 762 mA h g -1 reversible capacity at 50 mA g -1 and stable cycling performance over 100 cycles with 92.1% capacity retention at 100 mA g -1 can be achieved for the tin asymmetric membrane electrode synthesized using polysulfone and tin tert-butoxide precursor.

25 ENERGY STORAGE↗

DOE OSTI2025

Enabling hydrogen chemisorption on charged graphene

Two-dimensional (2D) materials, including graphitic derivatives, have long been of interest for hydrogen storage applications, due to their high theoretical storage capacity, low weight, and other useful properties. However, poor kinetics for hydrogen adsorption and surface diffusion as part of the proposed spillover process for hydrogenation have limited their technological potential. Here, we use first-principles calculations to study electronic doping as a means to improve hydrogen chemisorption on graphene, which we use here as a proxy for graphitic derivatives more broadly. We find that positively charged graphene sheets have vastly improved kinetics for hydrogen diffusion and adsorption, while they limit unwanted hydrogen desorption. This combination of effects should favor hydrogen chemisorption via spillover. We connect these trends to the C–H bond, which introduces states near the Fermi level. These states are depopulated as electrons are removed, thereby lowering the bond energy and permitting more facile movement of hydrogen. Our results suggest that spillover mechanisms for hydrogen chemisorption should be revisited if strategies to apply a large charge to graphitic systems can be realized. Moreover, switchable application of the charge may lead to the reversible chemisorption of hydrogen. While the large magnitude of charging required suggests that graphene itself may not be suitable for reversible hydrogen chemisorption, the factors we identify and discuss could significantly boost the prospects of graphitic derivatives and other 2D or layered materials for hydrogen storage applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1993

Characterization and development of materials for advanced textile composites

Work ongoing under the NASA Langley - Advanced Composite Technology (ACT) program is discussed. The primary emphasis of the work centers around the development and characterization of graphite fiber that has been impregnated with an epoxy powder. Four epoxies have been characterized in towpreg form as to their weaveability and braidability. Initial mechanical properties have been generated on each resin system. These include unidirectional as well as 8-harness satin cloth. Initial 2D and 3D weaving and braiding trials will be reported on as well as initial efforts to develop towpreg suitable for advanced tow placement.

Hartness, J. Timothy↗

NASA NTRSDate not supplied

Highly Thermally Conductive Hybrid Carbon Fiber Polymer Composite for Radiator Application

Carbon fiber (CF) reinforced polymer composites have been used for aerospace structures because they have low mass, high specific strength, high specific stiffness, and low life-cycle maintenance compared to aluminum alloys. However, due to their relatively low thermal conductivity, pristine CF polymer composites fail to provide effective heat flow for certain applications such as heat exchange systems and radiators. The technology described in this paper provides novel CF polymer composites that possess high thermal conductivity by incorporating pyrolytic graphite sheets (PGS). The thermal conductivities of novel hybrid PGS/CF polymer composites were measured to be about 10 to 30 times higher than that of pristine CF polymer composite, and about two times higher than that of aluminum alloy 6061. This new material with sufficient thermal conductivity is applicable to composite radiators of heat exchange systems.

Thermal Conductivity↗