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DOE OSTI2015

A near infra-red video system as a protective diagnostic for electron cyclotron resonance heating operation in the Wendelstein 7-X stellarator

The Wendelstein 7-X stellarator is a large nuclear fusion device based at Max-Planck-Institut für Plasmaphysik in Greifswald in Germany. The main plasma heating system for steady state operation in W7-X is electron cyclotron resonance heating (ECRH). During operation, part of plama facing components will be directly heated by the non-absorbed power of 1 MW rf beams of ECRH. In order to avoid damages of such components made of graphite tiles during the first operational phase, a near infra-red video system has been developed as a protective diagnostic for safe and secure ECRH operation. Both the mechanical design housing the camera and the optical system are very flexible and respect the requirements of steady state operation. The full system including data acquisition and control system has been successfully tested in the vacuum vessel, including on-line visualization and data storage of the four cameras equipping the ECRH equatorial launchers of W7-X.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

NASA NTRS1986

Structure-to-property Relationships in Addition Cured Polymers 2: Resin Tg Composite Initial Mechanical Properties of Norbornenyl Cured Polyimide Resins

PRM (polymerization of monomeric reactants) methodology was used to prepare thirty different polyimide oligomeric resins. Monomeric composition as well as chain length between sites of crosslinks were varied to examine their effects on glass transition temperature (Tg) of the cured/postcured resins. An almost linear correlation of Tg versus molecular distance between the crosslinks was observed. An attempt was made to correlate Tg with initial mechanical properties (flexural strength and interlaminar shear strength) of unidirectional graphite fiber composites prepared with these resins. However, the scatter in mechanical strength data prevented obtaining as clear a correlation as was observed for the structural modification/crosslink distance versus Tg. Instead, only a range of composite mechanical properties was obtained at the test temperatures studied (room temperature, 288 and 316 C). Perhaps more importantly, what did become apparent during the attempted correlation study was: (1) that PMR methodology could be used to prepare composites from resins that contain a wide variety of monomer modifications, and (2) that these composites almost invariably provided satisfactory initial mechanical properties as long as the resins selected were melt processable.

Alston, W. B.↗

NASA NTRS1986

Structure-to-property relationships in addition cured polymers. II - Resin Tg and composite initial mechanical properties of norbornenyl cured polyimide resins

Alston, William B.↗

NASA NTRS1993

Thermal-mechanical behavior of high precision composite mirrors

Composite mirror panels were designed, constructed, analyzed, and tested in the framework of a NASA precision segmented reflector task. The deformations of the reflector surface during the exposure to space enviroments were predicted using a finite element model. The composite mirror panels have graphite-epoxy or graphite-cyanate facesheets, separated by an aluminum or a composite honeycomb core. It is pointed out that in order to carry out detailed modeling of composite mirrors with high accuracy, it is necessary to have temperature dependent properties of the materials involved and the type and magnitude of manufacturing errors and material nonuniformities. The structural modeling and analysis efforts addressed the impact of key design and materials parameters on the performance of mirrors.

Kuo, C. P.↗

NASA NTRS2022

Building and Breaking Carbon Composites with REACTER

Carbon-based composites have become indispensable materials in aerospace and other high-performance applications, yet obtaining a detailed, nanoscale understanding of their morphology and failure mechanisms using only experimental methods remains a difficult challenge. REACTER is a versatile computational modeling tool for atomistic molecular dynamics simulations designed to model chemical reactions at the speed and length scales of classical force fields. In this work, several recent features of REACTER were applied to the creation and subsequent mechanical testing of two classes of carbon composites: carbon nanotube (CNT) composites and carbon fiber reinforced polymers (CFRP). A network of CNTs was grown dynamically using the new ‘create atoms’ feature of REACTER. The CNT filler was embedded into a polyarylacetylene (PAA) matrix by simulated in situ polymerization to obtain the final composite model. To generate the second class of carbon composite, fully carbonized (graphitic) carbon fiber morphologies were created by the method of Desai et al. [1], but using the advanced reaction constraints framework of REACTER. Two fiber models were created, representing a circular carbon fiber core and a flat surface, and similarly infiltrated with resin to obtain the final CFRP structure. Failure mechanisms were elucidated by simulating mechanically induced bond breaking, as characterized by third order DFT-based tight-binding simulations, via a reaction constraint on the total potential energy of the involved atoms.

Polymer↗

NASA NTRS1977

Ultra high tip speed (670.6 m/sec) fan stage with composite rotor: Aerodynamic and mechanical design

A highly loaded, single-stage compressor having a tip speed of 670.6 m/sec was designed for the purpose of investigating very high tip speeds and high aerodynamic loadings to obtain high stage pressure ratios at acceptable levels of efficiency. The design pressure ratio is 2.8 at an adiabatic efficiency of 84.4%. Corrected design flow is 83.4 kg/sec; corrected design speed is 15,200 rpm; and rotor inlet tip diameter is 0.853 m. The rotor uses multiple-circular-arc airfoils from 0 to 15% span, precompression airfoils assuming single, strong oblique shocks from 21 to 43% span, and precompression airfoils assuming multiple oblique shocks from 52% span to the tip. Because of the high tip speeds, the rotor blades are designed to be fabricated of composite materials. Two composite materials were investigated: Courtaulds HTS graphite fiber in a Kerimid 601 polyimide matrix and the same fibers in a PMR polyimide matrix. In addition to providing a description of the aerodynamic and mechanical design of the 670.0 m/sec fan, discussion is presented of the results of structural tests of blades fabricated with both types of matrices.

Halle, J. E.↗

NASA NTRS1984

Space Radiation Effects on Graphite-Epoxy Composite Materials

Radiation effects on engineering properties, dimensional stability, and chemistry on state of the art composite systems were characterized. T300/934 graphite-epoxy composite was subjected to 1.0 MeV electron radiation for a total dose of 1.0 x 10(10) rads at a rate of 5.0 x 10(7) rads/hour. This simulates a worst case exposure equivalent to 30 years in space. Mechanical testing was performed on he 4-ply unidirectional laminates over the temperature range of -250 F (116K) to +250 F (394K). A complete set of in-plane tensile elastic and strength properties were obtained (E sub 1, E sub 2, nu sub 12, G sub 12, X sub T, Y sub T, and S). In addition electron microscopy was used to study and analyze the fracture surfaces of all specimens tested. Results indicate that little difference in properties is noted at room temperature, but significant differences are observed at both low and elevated temperatures.

Milkovich, S. M.↗

NASA NTRS1999

Intercalation of Lithium in Pitch-Based Graphitized Carbon Fibers Chemically Modified by Fluorine: Soft Carbon With or Without an Oxide Surface

The effects of carbon structure and surface oxygen on the carbon's performance as the anode in lithium-ion battery were studied. Two carbon materials were used for the electrochemical tests: soft carbon made from defluorination of graphite fluoride, and the carbon precursor from which the graphite fluoride was made. In this research the precursor was graphitized carbon fiber P-100. It was first fluorinated to form CF(0.68), then defluorinated slowly at 350 to 450 C in bromoform, and finally heated in 1000 C nitrogen before exposed to room temperature air, producing disordered soft carbon having basic surface oxides. This process caused very little carbon loss. The electrochemical test involved cycles of lithium intercalation and deintercalation using C/saturated LiI-50/50 (vol %) EC and DMC/Li half cell. The cycling test had four major results. (1) The presence of a basic oxide surface may prevent solvent from entering the carbon structure and therefore prolong the carbon's cycle life for lithium intercalation-deintercalation. (2) The disordered soft carbon can store lithium through two different mechanisms. One of them is lithium intercalation. which gives the disordered carbon an electrochemical behavior similar to its more ordered graphitic precursor. The other is unknown in its chemistry, but is responsible for the high-N,oltage portion (less than 0.3V) of the charge-discharge curve. (3) Under certain conditions, the disordered carbon can store more lithium than its precursor. (4) These sample and its precursor can intercalate at 200 mA/g. and deintercalate at a rate of 2000 mA/g without significant capacity loss.

Hung, Ching-Chen↗

DOE OSTI2024

Dynamic Deformation in Nuclear Graphite and Underlying Mechanisms

Time-dependent deformation in nuclear graphite is influenced by the creation and migration of radiation-induced defects in the reactor environment. This study investigates the role of pre-existing defects such as point defect clusters and Mrozowski cracks in nuclear graphite IG-110. Separate specimens were irradiated with a 2.8 MeV Au 2+ beam with a fluence of 4.38 × 10 14 cm −2 and an 8 MeV C 2+ beam with a fluence of 1.24 × 10 16 cm −2 . Microscopic specimens were either mechanically loaded inside a transmission electron microscope (TEM) or subjected to ex situ indentation-based creep loading. In situ TEM tests showed significant plasticity in regions highly localized around the Mrozowski cracks, resembling slip or ripplocation bands. Slip bands were also seen near regions without pre-existing defects but at very high stresses. Ex situ self-ion irradiation embrittled the specimens and decreased the creep displacement and rate, while heavy ion irradiation resulted in the opposite behavior. We hypothesize that the large-sized gold ions (compared to the carbon atoms) induced interplanar swelling as well as cross-plane channels for increased defect mobility. These findings illustrate the role of pre-existing defects in the dynamic relaxation of stresses during irradiation and the need for more studies into the radiation environment’s impact on the mechanical response of nuclear graphite.

creep deformation↗

NASA NTRS1986

Damage-induced property changes in composites subjected to cyclic thermal loading

Damage in the form of transverse cracks resulting from thermal loading is studied as it relates to the dimensional stability of flat laminates and stiffness changes in cylindrical tubes. Graphite-epoxy specimens were subjected to cyclic thermal loading in the temperature range -250 to + 250 F. It is shown that transverse cracking is the dominant damage mechanism in both types of structural elements. Fiber splitting is also quite common at the low test temperatures. Experimental results indicate that damage significantly reduces the inplane coefficients of thermal expansion of flat laminates and the torsional stiffness of the tubes. Theoretical predictions for coefficients of thermal expansion as a function of crack spacing in flat laminates followed the same trend as experimental results.

Herakovich, Carl T.↗

DOE OSTI2021

ECAR-1930 BASELINE CHARACTERIZATION DATABASE VERIFICATION REPORT - NBG-18 BILLET 635-14

The purpose of this Engineering Calculations and Analysis Report is to present the data being collected in the Baseline Graphite Characterization program, which is directly tasked with supporting the Idaho National Laboratory’s (INL’s) research and development efforts on the Next Generation Nuclear Plant (NGNP)/Very High Temperature Reactor (VHTR). This program is populating a comprehensive database that will reflect the baseline properties of nuclear-grade graphite with regard to individual grade, billet, and position within individual billets. The physical and mechanical property information being collected will be transferred to the NGNP Data Management and Analysis System (NDMAS), and from that database will help populate handbook of property data available to member nations of the Generation IV International Forum (GIF). The transfer of this data from the applicable technical lead to the dissemination databases available to other end users requires a full review of the test procedures and data collection efforts through an analysis of the multiple summary spreadsheets and values being collected. This report represents that analysis for a single billet of nuclear grade graphite (NBG-18 billet 635-14) and facilitates the release of the associated data to the NDMAS custodians.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

NASA NTRS1991

Atomic oxygen testing with thermal atom systems - A critical evaluation

The use of thermal atom (kinetic energy near 0.04 eV) test methods as a materials selection and screening technique for LEO spacecraft is critically evaluated in this paper. The physics and chemistry of the thermal atom environments are shown to produce specific mass loss rates (mg/sq cm per min) and reaction efficiencies (Re) radically different from those produced in the LEO environment. A response surface study shows that specific mass loss rates change rapidly with plasma-asher parameters and seldom agree with flight data. FEP Teflon is shown to react by a different mechanism than Kapton, polyethylene, or graphite. The Re (Re = volume of material removed/oxygen atom) of Kapton, polyethylene, Mylar, Tedlar, FEP Teflon, and graphite measured in a flowing afterglow apparatus are 0.001 to 0.0001 those measured with high-energy atoms (kinetic energy 1.5 eV or greater) in beam systems or in LEO. The effect of sample temperature and atom impact energy on Re is discussed. A simple kinetic model describing the reaction of atomic oxygen with polymer surfaces is developed. Guidelines and recommendations for thermal atom testing and interpretation of test results are presented.

Koontz, Steven L.↗

DOE OSTI2026

Linking spout fluidization hydrodynamics to pyrolytic carbon deposition characteristics in a fluidized bed chemical vapor deposition reactor

Spout fluidized bed chemical vapor deposition (SFB-CVD) is the dominant method for producing pyrolytic carbon (PyC) coatings on tristructural-isotropic (TRISO) fuel particles, yet the relationship between gas injector design, fluidization hydrodynamics, and resulting coating quality remains poorly quantified. Here, in this work, three spout fluidized bed (SFB) nozzle geometries were designed and fabricated to empirically investigate how injector-driven changes in particle circulation influence PyC deposition. The geometries were first evaluated in a room temperature fluidization apparatus using time-resolved particle image velocimetry, which highlighted distinct differences in particle velocity fields, circulation pathways, and overall fluidization quality. Graphite versions of each injector geometry were subsequently implemented in a laboratory-scale SFB-CVD reactor to deposit PyC onto surrogate fuel kernels under similar conditions. Post-deposition characterization included particle morphology, coating thickness, porosity distribution, optical anisotropy, and microindentation mechanical testing. Overall, the results show clear differences in coating microstructure as a function of changing injector geometry, despite mechanical testing indicating comparable elastic modulus values across all coatings. This study provides one of the first fully experimental, quantitative mappings between SFB nozzle geometry, fluidization hydrodynamics, and resulting PyC coating structure. The framework established here supports rational injector design and offers a pathway toward improved coating control in future pilot- and production-scale TRISO fuel fabrication systems.

Coated particle fuel↗

NASA NTRS2007

High Thermal Conductivity Polymer Matrix Composites (PMC) for Advanced Space Radiators

High temperature polymer matrix composites (PMC) reinforced with high thermal conductivity (approx. 1000 W/mK) pitch-based carbon fibers are evaluated for a facesheet/fin structure of large space radiator systems. Significant weight reductions along with improved thermal performance, structural integrity and space durability toward its metallic counterparts were envisioned. Candidate commercial resin systems including Cyanate Esters, BMIs, and polyimide were selected based on thermal capabilities and processability. PMC laminates were designed to match the thermal expansion coefficient of various metal heat pipes or tubes. Large, but thin composite panels were successfully fabricated after optimizing cure conditions. Space durability of PMC with potential degradation mechanisms was assessed by simulated thermal aging tests in high vacuum, 1-3 x 10(exp -6) torr, at three temperatures, 227 C, 277 C, and 316 C for up to one year. Nanocomposites with vapor-grown carbon nano-fibers and exfoliated graphite flakes were attempted to improve thermal conductivity (TC) and microcracking resistance. Good quality nanocomposites were fabricated and evaluated for TC and durability including radiation resistance. TC was measured in both in-plan and thru-the-thickness directions, and the effects of microcracks on TC are also being evaluated. This paper will discuss the systematic experimental approaches, various performance-durability evaluations, and current subcomponent design and fabrication/manufacturing efforts.

Shin, E. Eugene↗

DOE OSTI2020

Mechanical Properties of Permanent Foaming Fixatives for Deactivation and Decommissioning Activities

DOE-EM have identified an operational requirement for a fixative that can immobilize and/or encapsulate residual contamination in 3D void volumes (pipes, gloveboxes, waste containers, etc.) during D and D activities. Failure to safely and effectively immobilize residual contamination can: Put workers at risk, Contaminate the public and environment, Drive up operational costs. Commercial-off-the-shelf (COTS) polyurethane (PU) foams is one possible solution and is currently being investigated in collaboration with Savannah River National Lab (SRNL). Mechanical property testing will dictate how well PU foams can withstand physical stressors outlined in safety documents while immobilizing residual contamination. Results can provide a performance criteria for Section 5 of ASTM E3191: Standard Specification for Permanent Foaming Fixatives Used to Mitigate Spread of Radioactive Contamination. Polyurethanes consists of repeating units of urethanes which are produced from an exothermic reaction between a polyol (an alcohol with two or more hydroxyl groups in a molecule) and an isocyanate [2]. PUs consists of 3D cells that are formed by a blowing agent which is normally water. Water interacting with the isocyanate creates carbon dioxide and urea which contributes to cells' growth and expansion. The cross-linking between the polyol and isocyanate solidify the cell faces and walls. Micro scale properties that can influence mechanical properties include: Relative density (ratio between density of cellular material and density of the solid of which the cell walls are made of). Cells connectivity between edges and faces, and number of cells contact neighbors [3]. Whether a foam is open-celled or closed-celled. Closed-celled foams have a thin membrane that encloses each cell which can contribute to the stiffness of the foam. Incorporating fillers in the PU matrix like carbon-based nanoparticles in the form of expandable graphite (EG) can increase the thermal and mechanical performance [4]. When exposed to heat, EG produces a char layer that prevents heat and oxygen transfer which is known as intumescing. Mechanical performance is dependent on amount of EG loading since the cell sizes are linearly dependent on it. Overall, the rigid foams (I-R2) proved superior. SEM Analysis: I-R2 had the most consistent spherical sizes (average cell diameter: 489 μm), which enhance the relative density the most [5]. Tensile Testing Results: I-R2 experienced the largest breaking load (103.65 lbf) and stress (289.42 psi). I-R2 also had a higher Young's Modulus compared to R1 (2.99 ksi to 2.09 ksi). Compression Testing Results: I-R2 had the highest stress at 80% deflection (360.67 psi), load (1387.48 lbf) and modulus (3.92 ksi)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS2008

Mechanical Properties and Durability of "Waterless Concrete"

Waterless concrete consists of molten elementary sulfur and aggregate. The aggregates in lunar environment will be lunar rocks and soil. Sulfur is present on the Moon in Troilite soil (FeS) and by oxidation soil iron and sulfur can be produced. Iron can be used to reinforce the sulfur concrete. Sulfur concrete specimens were cycled between liquid nitrogen (approximately 191 C) and room temperature (approximately 21 C) to simulate exposure to a lunar environment. Cycled and control specimens were subsequently tested in compression at room temperatures (approximately 21 C) and approximately 101 C. Test results showed that due to temperature cycling, compressive strength of cycled specimens was 20% of those non-cycled. Microscopic examination of the fracture surfaces from the cycled samples showed clear de-bonding of the sulfur from the aggregate material whereas it was seen well bonded in those non-cycled. This reduction in strength can be attributed to the large differences in thermal coefficients of expansion of the materials constituting the concrete which promoted cracking. Similar sulfur concrete mixtures were strengthened with short and long glass fibers. The glass fibers from lunar regolith simulant was melted in a 25 cc Pt-Rh crucible in a Sybron Thermoline high temperature MoSi2 furnace at melting temperatures of 1450 to 1600 C for times of 30 min to 1 hour. Glass fibers were cast from the melt into graphite crucibles and were annealed for a couple of hours at 600 C. Glass fibers and small rods were pulled from the melt. The glass melt wets the ceramic rod and long continuous glass fibers were easily hand drawn. The glass fibers were immediately coated with a protective polymer to maintain the mechanical strength. The glass fibers were used to reinforce sulfur concrete plated to improve the flexural strength of the sulfur concrete. Prisms beams strengthened with glass fibers were tested in 4-point bending test. Beams strengthened with glass fiber showed to exhibit an increase in the flexura strength by as much as 45%.

Toutanji, Houssam↗

DOE OSTI2022

Li-Ion Battery Electrode Contact Resistance Estimation by Mechanical Peel Test

Li-ion battery electrode electronic properties, including bulk conductivity and contact resistance, are critical parameters affecting cell performance and fast-charge capability. Contact resistance between the coating and current collector is often the largest electronic resistance in an electrode and is affected by chemical, microstructural, and interfacial variations. Direct measurements of contact resistance and bulk conductivity have proven to be challenging. In their absence, a mechanical electrode peel test is often used to compare adhesion and electrical contact resistance. However, using a micro-flexible-surface probe, contact resistance can be directly determined. Here, this work compares contact resistance and mechanical peel strength of multiple commercial-grade HE5050 and NCM523 cathodes and graphite and silicon anodes. It was found that peel strength correlates well with contact resistance in a carefully curated data set (p < 0.05) and in some situations may be a good metric to estimate electrical properties. However, there were distinct outliers in the data set, indicating that peel strength may not accurately reflect electrical properties when there is significant variation in electrode composition. These results illustrate the value of the micro-flexible-surface probe in quantifying contact resistance and bulk conductivity to better understand how battery composition and processing steps affect microstructure and resulting cell performance.

25 ENERGY STORAGE↗

NASA NTRS1982

Develop, demonstrate, and verify large area composite structural bonding with polyimide adhesives

The technology required to produce graphite-polyimide structural components with operational capability at 598 K (600 F) is considered. A series of polyimide adhesives was screened for mechanical and physical properties and processibility in fabricating large midplane bonded panels and honeycomb sandwich panels in an effort to fabricate a structural test component of the space shuttle aft body flap. From 41 formulations, LaRC-13, FM34B-18, and a modified LaRC-13 adhesive were selected for further evaluation. The LaRC-13 adhesive was rated as the best of the three adhesives in terms of availability, cost, processibility, properties, and ability to produce void fee large area (12" x 12") midplane bonds. Surface treatments and primers for the adhesives were evaluated and processes were developed for the fabrication of honeycomb sandwich panels of very good quality which was evidenced by rupture in the honeycomb core rather than in the facesheet bands on flatwise tensile strength testing. The fabrication of the adhesively bonded honeycomb sandwich cover panels, ribs, and leading edge covers of Celion graphite/LARC-160 polyimide laminates is described.

Bhombal, B. D.↗