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NASA NTRS1974

Effect of chlorine purification on oxidation resistance of some mechanical carbons

Oxidation experiments were conducted with some experimental and commercial mechanical carbons at 650 C in dry air flowing at 28 cc/sec (STP). In general, purification of these carbon-graphites with chlorine at 2800 C improved oxidation resistance. Additional improvements in oxidation resistance were obtained from purification followed by an antioxidant (zinc phosphate) treatment. For the commercial materials, purification alone gave greater oxidation resistance than the antioxidant treatment alone. The reverse, however, was the case for the experimental materials.

Wisander, D. W.↗

DOE OSTI2025

Computational Modeling of Molten Salt Infiltration and Oxidation in Nuclear Graphite

Graphite is utilized as a moderator and reflector in advanced nuclear reactor designs due to its high thermal conductivity, neutron moderation properties, and resistance to radiation damage. However, its longterm performance and reliability are challenged by degradation mechanisms such as molten salt infiltration in molten salt reactors (MSRs) and oxidation in gas-cooled reactors (GCRs). These mechanisms can compromise the structural integrity and operational lifetime of graphite components, necessitating a more detailed assessment of their physical behavior. This report focuses on the development of computational models for molten salt infiltration and oxidation of graphite to aid the design and performance analysis of graphite components. For molten salt infiltration, a computational framework is developed that couples incompressible Navier-Stokes and phase-field model to simulate the penetration of molten salt into graphite?s interconnected pore structure. Initial model verification is performed using two-phase flows in two dimensions, demonstrating the models ability to capture fundamental physical behavior and agree with analytical solution. This framework is then applied to a realistic IG110 nuclear graphite , where a computed tomography extracted pore geometry is used to analyse the infiltration behavior of FLiNaK molten salt. This model provides insights into how the microstructure and other relevant parameters influence the transport pathways of molten salt into graphite, potentially offering a means to rapidly evaluate a graphite grade?s resistance to infiltration. For oxidation, the report details pore-scale mass and heat transport models, describing the diffusion of gases, reaction kinetics, and thermal effects. Additionally, this report highlights inconsistencies in the existing volume-averaged macroscopic model, particularly in upscaling of reaction kinetics and flux terms, and surface to volume transformations. These inconsistencies suggest that current formulations may not accurately capture the experimentally observed graphite oxidation process, highlighting the need for improved model development. This work advances the development of physics-based computational models for graphite degradation, contributing to improved predictive models for next-generation nuclear reactor designs. Future efforts will focus on refining the infiltration model to address non-physical behaviors and enhance its robustness. Additionally, for oxidation, further studies will employ the principles of volume averaging to rigorously derive the upscaled equations, potentially in collaboration with subject matter experts.

Computational Modeling of Molten Salt Infiltration↗

NASA NTRS1980

Fiber release characteristics of graphite hybrid composites

The paper considers different material concepts that can be fabricated of hybridized composites which demonstrate improved graphite fiber retention capability in a severe fire without significant reduction to the composite properties. More than 30 panels were fabricated for mechanical and fire tests, the details and results of which are presented. Methods of composite hybridization investigated included the addition of oxidation resistant fillers to the resin, mechanically interlocking the graphite fibers by the use of woven fabrics, and the addition of glass fibers and glass additives designed to melt and fuse the graphite fibers together. It is concluded that a woven fabric with a serving of glass around each graphite tow is by far the superior of those evaluated: not only is there a coalescing effect in each graphite layer, but there is also a definite adhesion of each layer to its neighbor.

Henshaw, J.↗

NASA NTRS1974

Structural studies on carbon materials for advanced space technology. Part 1: Structure and oxidation behavior of some carbon/carbon composite materials

The microstructure and some microstructural effects of oxidation have been investigated for laminar carbon fiber cloth/cloth binder matrix composite materials. It was found that cloth wave is important in determining the macrostructure of the composites X-ray diffraction analysis showed that the composites were more graphitic than the constituent fiber phases, indicating a graphitic binder matrix phase. Various tests which were conducted to investigate specific properties of the material are described. It was learned that under the moderate temperature and oxidant flow conditions studied, C-700, 730 materials exhibit superior oxidation resistance primarily because of the inhibiting influence of the graphitized binder matrix.

Fischbach, D. B.↗

NASA NTRS1986

An evaluation of candidate oxidation resistant materials for space applications in LEO

Ground based testing of materials considered for polyimide (Kapton) solar array blanket protection and graphite-epoxy stroctural member protection was performed in an RF plasma asher. Protective coatings on Kapton from various commercial sources and from NASA Lewis Research Center were exposed to the air plasma; and mass loss per unit area was measured for each sample. All samples evaluated provided some protection to the underlying surface, but metal-oxide-fluoropolymer coatings provided the best protection by exhibiting very little degradation after 47 hr of asher exposure. Mica paint was evaluated as a protective coating for graphite-epoxy structural members. Mica appeared to be resistant to attack by atomic oxygen, but only offered limited protection as a paint. this is believed to be due to the paint vehicle ashing underneath the mica leaving unattached mica flakes lying on the surface. The protective coatings on Kapton evaluated so far are promising but further research on protection of graphite-epoxy support structures is needed.

Rutledge, Sharon↗

NASA NTRS1987

An evaluation of candidate oxidation resistant materials

Ground based testing of materials considered for Kapton solar array blanket protection, graphite epoxy structural member protection, and high temperature radiators was performed in an RF plasma asher. Ashing rates for Kapton were correlated with rates measured on STS-8 to determine the exposure time equivalent to one year in low Earth orbit (LEO) at a constant density space station orbital flux. Protective coatings on Kapton from Tekmat, Andus Corporation, and LeRC were evaluated in the plasma asher and mass loss rates per unit area were measured for each sample. All samples evaluated provided some protection to the underlying surface but ion beam sputter deposited samples of SiO2 and SiO2 with 8% polytetrafluoroethylene (PTFE) showed no evidence of degradation after 47 hours of exposure. Mica paint was evaluated as a protective coating for graphite epoxy structural members. Mica appears to be resistant to attack by atomic oxygen but only offers some limited protection as a paint because the paint vehicles evaluated to date were not resistant to atomic oxygen. Four materials were selected for evaluation as candidate radiator materials: stainless steel, copper, niobium-1% zirconium, and titanium-6% aluminum-4% vanadium. These materials were surface textured by various means to improve their emittance. Emittances as high as 0.93 at 2.5 microns for stainless steel and 0.89 at 2.5 microns for Nb-1 Zr were obtained from surface texturing. There were no significant changes in emittance after asher exposure.

Rutledge, Sharon↗

NASA NTRS1990

High-temperature polymer matrix composites

Polymers research at the NASA Lewis Research Center has produced high-temperature, easily processable resin systems, such as PMR-15. In addition, the Polymers Branch has investigated ways to improve the mechanical properties of polymers and the microcracking resistance of polymer matrix composites in response to industry need for new and improved aeropropulsion materials. Current and future research in the Polymers Branch is aimed at advancing the upper use temperature of polymer matrix composites to 700 F and beyond by developing new resins, by examining the use of fiber reinforcements other than graphite, and by developing coatings for polymer matrix composites to increase their oxidation resistance.

Meador, Michael A.↗

NASA NTRS1979

Study of high resistance inorganic coatings on graphite fibers

Coatings made of boron, silicon carbide, silica, and silica-like materials were studied to determine their ability to increase resistance of graphite fibers. The most promising results were attained by chemical vapor depositing silicon carbide on graphite fiber followed by oxidation, and drawing graphite fiber through ethyl silicate followed by appropriate heat treatments. In the silicon carbide coating studies, no degradation of the graphite fibers was observed and resistance values as high as three orders of magnitude higher than that of the uncoated fiber was attained. The strength of a composite fabricated from the coated fiber had a strength which compared favorably with those of composites prepared from uncoated fiber. For the silica-like coated fiber prepared by drawing the graphite fiber through an ethyl silicate solution followed by heating, coated fiber resistances about an order of magnitude greater than that of the uncoated fiber were attained. Composites prepared using these fibers had flexural strengths comparable with those prepared using uncoated fibers, but the shear strengths were lower.

Galasso, F. S.↗

NASA NTRS1982

Processing of fused silicide coatings for carbon-based materials

The processing and oxidation resistance of fused Al-Si and Ni-Si slurry coatings on ATJ graphite was studied. Ni-Si coatings in the 70 to 90 percent Si range were successfully processed to melt, wet, and bond to the graphite. The molten coatings also infiltrated the porosity in graphite and reacted with it to form SiC in the coating. Cyclic oxidation at 1200 C showed that these coatings were not totally protective because of local attack of the substrate, due to the extreme thinness of the coatings in combination with coating cracks.

Smialek, J. L.↗

NASA NTRS1983

Processing of fused silicide coatings for carbon-based materials

Smialek, J. L.↗

NASA NTRS1979

Graphite fiber reinforced glass matrix composites for aerospace applications

The graphite fiber reinforced glass matrix composite system is described. Although this composite is not yet a mature material, it possesses low density, attractive mechanical properties at elevated temperatures, and good environmental stability. Properties are reported for a borosilicate glass matrix unidirectionally reinforced with 60 volume percent HMS graphite fiber. The flexural strength and fatigue characteristics at room and elevated temperature, resistance to thermal cycling and continuous high temperature oxidation, and thermal expansion characteristics of the composite are reported. The properties of this new composite are compared to those of advanced resin and metal matrix composites showing that graphite fiber reinforced glass matrix composites are attractive for aerospace applications.

Prewo, K. M.↗

NASA NTRS1980

Coatings for Graphite Fibers

Several approaches for applying high resistance coatings continuously to graphite yarn were investigated. Two of the most promising approaches involved (1) chemically vapor depositing (CVD) SiC coatings on the surface of the fiber followed by oxidation, and (2) drawing the graphite yarn through an organo-silicone solution followed by heat treatments. In both methods, coated fibers were obtained which exhibited increased electrical resistances over untreated fibers and which were not degraded. This work was conducted in a previous program. In this program, the continuous CVD SiC coating process used on HTS fiber was extended to the coating of HMS, Celion 6000, Celion 12000 and T-300 graphite fiber. Electrical resistances three order of magnitude greater than the uncoated fiber were measured with no significant degradation of the fiber strength. Graphite fibers coated with CVD Si3N4 and BN had resistances greater than 10(exp 6) ohm/cm. Lower pyrolysis temperatures were used in preparing the silica-like coatings also resulting in resistances as high as three orders of magnitude higher than the uncoated fiber. The epoxy matrix composites prepared using these coated fibers had low shear strengths indicating that the coatings were weak.

Galasso, F. S.↗

DOE OSTI2025

Electrically Conductive Amine Functionalized Reduced Graphite Oxide Foam for CO 2 Removal from the Air

Rapid regeneration of CO 2 adsorbents is critical to improving the productivity of direct air capture (DAC) systems. In this study, we codesigned a material to have appropriate electrical conductivity and CO 2 adsorption properties to enable efficient CO 2 capture from air. Specifically, we present a poly(ethylenimine) (PEI)-impregnated thermally annealed graphite oxide (TAGO900) foam adsorbent tailored for vacuum-assisted electrically driven thermal swing adsorption (V-ETSA). This structured adsorbent leverages the high electrical conductivity of the reduced graphite oxide framework to enable fast and direct heating of the adsorbent material by electrical resistance heating (Joule heating). An optimal sample, 40 wt % PEI (molecular weight 25k) impregnated TAGO900, shows the best balance between adsorption capacity (1.54 mmol g –1 ) and adsorption rates (0.016 mmol g –1 min –1 ) using fixed bed breakthrough experiments at 25 °C and 70% RH using 50 sccm 400 ppm of CO 2 /N 2 flow. Compared to conventional temperature vacuum swing adsorption (TVSA), the V-ETSA approach achieves substantially faster CO 2 desorption, achieving average desorption rates (including cooling time) of 0.09 mmol g –1 min –1 ─approximately 2.5 times faster than TVSA under similar operating conditions. The maximum desorption rate reaches 0.23 mmol/g/min during the desorption stage. These results underscore the importance of the direct heating strategy, such as Joule heating, for fast and highly productive vacuum swing adsorption in DAC systems.

amines↗

DOE OSTI2017

Oxidation Behavior of Matrix Graphite and Its Effect on Compressive Strength

Matrix graphite (MG) with incompletely graphitized binder used in high-temperature gas-cooled reactors (HTGRs) is commonly suspected to exhibit lower oxidation resistance in air. In order to reveal the oxidation performance, the oxidation behavior of newly developed A3-3 MG at the temperature range from 500 to 950°C in air was studied and the effect of oxidation on the compressive strength of oxidized MG specimens was characterized. Results show that temperature has a significant influence on the oxidation behavior of MG. The transition temperature between Regimes I and II is ~700°C and the activation energy ( E a ) in Regime I is around 185 kJ/mol, a little lower than that of nuclear graphite, which indicates MG is more vulnerable to oxidation. Oxidation at 550°C causes more damage to compressive strength of MG than oxidation at 900°C. Comparing with the strength of pristine MG specimens, the rate of compressive strength loss is 77.3% after oxidation at 550°C and only 12.5% for oxidation at 900°C. Microstructure images of SEM and porosity measurement by Mercury Porosimetry indicate that the significant compressive strength loss of MG oxidized at 550°C may be attributed to both the uniform pore formation throughout the bulk and the preferential oxidation of the binder.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2023

Synthesis and Thermal Oxidation Resistance of Boron-Rich Boron–Carbide Material

A boron-rich boron–carbide material (B4+δC) was synthesized by spark plasma sintering of a ball-milled mixture of high-purity boron powder and graphitic carbon at a pressure of 7 MPa and a temperature of 1930 °C. This high-pressure, high-temperature synthesized material was recovered and characterized by X-ray diffraction, X-ray photoelectron spectroscopy, Raman spectroscopy, Vickers hardness measurements, and thermal oxidation studies. The X-ray diffraction studies revealed a single-phase rhombohedral structure (space group R-3m) with lattice parameters in hexagonal representation as a = 5.609 ± 0.007 Å and c = 12.082 ± 0.02 Å. The experimental lattice parameters result in a value of δ = 0.55, or the composition of the synthesized compound as B4.55C. The high-resolution scans of boron binding energy reveal the existence of a B-C bond at 188.5 eV. Raman spectroscopy reveals the existence of a 386 cm−1 vibrational mode representative of C-B-B linear chain formation due to excess boron in the lattice. The measured Vickers microhardness at a load of 200 gf shows a high hardness value of 33.8 ± 2.3 GPa. Thermal gravimetric studies on B4.55C were conducted at a temperature of 1300 °C in a compressed dry air environment, and its behavior is compared to other high-temperature ceramic materials such as high-entropy transition metal boride. The high neutron absorption cross section, high melting point, high mechanical strength, and thermal oxidation resistance make this material ideal for applications in extreme environments.

36 MATERIALS SCIENCE↗

NASA NTRS2003

Analysis of the Effect of Surface Modification on Polyimide Composites Coated with Erosion Resistant Materials

The aim of this research is to enhance performance of composite coatings through modification of graphite-reinforced polyimide composite surfaces prior to metal bond coat/ hard topcoat application for use in the erosive and/or oxidative environments of advanced engines. Graphite reinforced polyimide composites, PMR-15 and PMR-II-50, formed by sheet molding and pre-pregging will be surface treated, overlaid with a bond coat and then coated with WC-Co. The surface treatment will include cleaning, RF plasma or ultraviolet light- ozone etching, and deposition of SiO(x) groups. These surface treatments will be studied in order to investigate and improve adhesion and oxidation resistance. The following panels were provided by NASA-Glenn Research Center(NASA-GRC): Eight compression molded PMR-II-50; 6 x 6 x 0.125 in. Two vacuum-bagged PMR-II-50; 12 x 12 x 0.125 in. Eight compression molded PMR-15; 6 x 6 x 0.125 in. One vacuum-bagged PMR-15; 12 x 12 x 0.125 in. All panels were made using a 12 x 12 in. T650-35 8HS (3K-tow) graphite fabric. A diamond-wafering blade, with deionized water as a cutting fluid, was used to cut PMR-II-50 and PMR-15 panels into 1 x 1 in. pieces for surface tests. The panel edges exhibiting delamination were used for the preliminary surface preparation tests as these would be unsuitable for strength and erosion testing. PMR-15 neat resin samples were also provided by NASA GRC. Surface profiles of the as-received samples were determined using a Dektak III Surface profile measuring system. Two samples of compression molded PMR-II-50 and PMR-15, vacuum-bagged PMR-II-50 and PMR-15 were randomly chosen for surface profile measurement according to ANSI/ASME B46.1. Prior to each measurement, the samples were blasted with compressed air to remove any artifacts. Five 10 mm-long scans were made on each sample. The short and long wavelength cutoff filter values were set at 100 and 1000 m, diamond stylus radius was 12.5 microns. Table 1 is a summary of the arithmetic average roughness (Ra) and waviness (Wa) for the composite surfaces.

Ndalama, Tchinga↗

DOE OSTI2019

Preparation of Nano-SiO{sub 2}-Coated Graphite Films by a Laser-Assisted Sol–Gel Process

Here, we prepared nano-SiO{sub 2}-coated graphite films using a novel laser-assisted sol–gel method. The SiO{sub 2} sol–gel prepositioned on the graphite substrate was irradiated by the fiber laser at different energy densities. The growth mechanism of the coatings under laser irradiation was studied and the effects of processing parameters on the coating structure were systematically investigated. In addition, the high-temperature oxidation resistance of these samples was examined. Surface morphology and elemental composition were examined using scanning electron microscopy and energy-dispersive spectrometer. Phase constituents and microstructure were identified by x-ray diffraction and transmission electron microscopy. The oxidation resistance was analyzed by thermal gravimetric analysis. The results found that laser irradiation significantly modifies the sol–gel-deposited nano-SiO{sub 2} layer. A uniform and compact nano-SiO{sub 2} coating was obtained when irradiated by laser energy density of 14.4 kJ/cm{sup 2}. Optimum high-temperature oxidation resistance was achieved for the two-layer SiO{sub 2}-coated films.

36 MATERIALS SCIENCE↗

NASA NTRS1984

Phosphorus-containing imide resins - Modification by elastomers

The syntheses and general features of addition-type maleimide resins based on bis(m-aminophenyl)phosphine oxide and tris(m-aminophenyl)phosphine oxide have been reported previously. These resins have been used to fabricate graphite cloth laminates having excellent flame resistance. These composites did not burn even in pure oxygen. However, these resins were somewhat brittle. This paper reports the modification of these phosphorus-containing resins by an amine-terminated butadiene-acrylonitrile copolymer (ATBN) and a perfluoroalkylene diaromatic amine elastomer (3F). An approximately two-fold increase in short beam shear strength and flexural strength was observed at 7 percent ATBN concentration. The tensile, flexural, and shear strengths were reduced when 18 percent ATBN was used. Anaerobic char yields of the resins at 800 C and the limiting oxygen indexes of the laminates decreased with increasing ATBN concentration. The perfluorodiamine (3F) was used with both imide resins at 6.4 percent concentration. The shear strength was doubled in the case of the bisimide with no loss of flammability characteristics. The modified trisimide laminate also had improved properties over the unmodified one. The dynamic mechanical analysis of a four-ply laminate indicated a glass transition temperature above 300 C. Scanning electron micrographs of the ATBN modified imide resins were also recorded.

Varma, I. K.↗