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At least 91 records · Page 5

Primary igneous carbon in ureilites - Petrological implications

The ureilite meteorites are carbonaceous olivine-pyroxene achondrites. They typically contain up to 4 wt.% carbon (carbonaceous matrix) as graphite, diamond, and lonsdaleite. Shock degradation has effectively obliterated primary textures in the carbonaceous matrix of previously described ureilites, a factor that has hampered efforts to explain the origin of this material. In contrast, the Antarctic ureilite ALHA78019 displays perfectly preserved primary textures in the carbonaceous matrix characterized by euhedral graphite blades intergrown with Fe-Ni metal and sulfide (diamonds are absent). This petrographic feature suggests that most graphite in ureilites originated by crystallization from a C-rich metallic phase. Assuming that fO2 is controlled by C-CO-CO2 reactions, the compositions of silicates and metals in ureilites imply a two-stage redox history. The noble gases and rare earths of ureilites are discussed in light of this model.

Berkely, J. L.↗

Characterization of selected LDEF polymer matrix resin composite materials

The characterization of selected graphite fiber reinforced epoxy (934 and 5208) and polysulfone (P1700) matrix resin composite materials which received 5 years and 10 months of exposure to the LEO environment on the Long Duration Exposure Facility is reported. Resin loss and a decrease in mechanical performance as well as dramatic visual effects were observed. However, chemical characterization including infrared, thermal, and selected solution property measurements showed that the molecular structure of the polymeric matrix had not changed significantly in response to this exposure. The potential effect of a silicon-containing molecular contamination of these specimens is addressed.

Young, Philip R.↗

Effects of LDEF flight exposure on selected polymer matrix resin composite materials

The characterization of selected graphite fiber reinforced epoxy and polysulfone matrix resin composites which received exposure to the LEO environment on the LDEF is reported. The changes in mechanical properties of ultimate tensile strength and tensile modulus for exposed flight specimens are compared to the three sets of control specimens. Marked changes in surface appearance are discussed, and resin loss is reported. The chemical characterization including IR, thermal, and selected solution property measurements showed that the molecular structure of the polymeric matrix had not changed significantly in response to this exposure.

Slemp, Wayne S.↗

Effects of LDEF flight exposure on selected polymer matrix resin composite materials

The characterization of selected graphite fiber reinforced epoxy (934 and 5208) and polysulfone (P1700) matrix resin composites materials which received over five years and nine months of exposure to the low earth orbit (LEO) environment in experiment AO134 on the Long Duration Exposure Facility is reported. The changes in mechanical properties of ultimate tensile strength and tensile modulus for exposed flight specimens are compared to the three sets of control specimens. Marked changes in surface appearance are discussed, and resin loss is reported. The chemical characterization including infrared, thermal, and selected solution property measurements showed that the molecular structure of the polymetric matrix had not changed significantly in response to this exposure.

Slemp, Wayne S.↗

An investigation of fracture behaviors of NBG-18 nuclear graphite using in situ mechanical testing coupled with micro-CT

Nuclear graphite contains defects spanning from nanoscale basal cracks to sub-mm scale voids. This study aims to establish an experimental method to investigate pre-existing defects and 3-D crack growth inside nuclear graphite, NBG-18. Three-point bending tests were performed on single-edge notched beam specimens with and without coupling with micro-CT. The fracture toughness was measured to be 1.17 ± 0.06 MPa $\sqrt{{m}}$. Cracks were observed to initiate from the pores and thermal cracks on the edge of the notch and then defect or twist to grow along the pre-existing defects. Crack bridging, defection, and twisting were the primary toughening mechanisms. The crack resistance curve exhibited a trend of rising-plateau-rising that can be related to the interaction of crack front and the pre-existing defects. In conclusion, the results highlight the capability of laboratory micro-CT-based experimental method for the visualization of multi-scale defect interactions, which remains to be a challenge in the characterization of nuclear graphite.

36 MATERIALS SCIENCE↗

Influence of electron radiation and temperature on the cyclic, matrix dominated response of graphite-epoxy

The effects of electron radiation and elevated temperature on the matrix-dominated cyclic response of standard T300/934 and a chemically modified T300/934 graphite-epoxy are characterized. Both materials were subjected to 1.0 x 10 to the 10th rads of 1.0 MeV electron irradiation, under vacuum, to simulate 30 years in geosynchronous orbit. Cyclic tests were performed at room temperature and elevated temperature (121 C) on 4-ply unidirectional laminates to characterize the effects associated with irradiation and elevated temperature. Both materials exhibited energy dissipation in their response at elevated temperature. The irradiated modified material also exhibited energy dissipation at room temperature. The combination of elevated temperature and irradiation resulted in the most severe effects in the form of lower proportional limits, and greater energy dissipation. Dynamic-mechanical analysis demonstrated that the glass transition temperature, T(g), of the standard material was lowered 39 C by irradiation, wereas the T(g) of the modified material was lowered 28 C by irradiation. Thermomechanical analysis showed the occurrence of volatile products generated upon heating of the irradiated materials.

Reed, Susan M.↗

Micromechanical Modeling of the Thermal Expansion of Graphite/copper Composites with Nonuniform Microstructure

Two micromechanical models were developed to investigate the thermal expansion of graphite/copper (Gr/Cu) composites. The models incorporate the effects of temperature-dependent material properties, matrix inelasticity, initial residual stresses due to processing history, and nonuniform fiber distribution. The first model is based on the multiple concentric cylinder geometry, with each cylinder treated as a two-phase composite with a characteristic fiber volume fractions. By altering the fiber volume fraction of the individual cylinders, unidirectional composites with radially nonuniform fiber distributions can be investigated using this model. The second model is based on the inelastic lamination theory. By varying the fiber content in the individual laminae, composites with nonuniform fiber distribution in the thickness direction can be investigated. In both models, the properties of the individual regions (cylinders or laminae) are calculated using the method of cells micromechanical model. Classical incremental plasticity theory is used to model the inelastic response of the copper matrix at the microlevel. The models were used to characterize the effects of nonuniform fiber distribution on the thermal expansion of Gr/Cu. These effects were compared to the effects of matrix plasticity, choice of stress-free temperature, and slight fiber misalignment. It was found that the radially nonuniform fiber distribution has little effect on the thermal expansion of Gr/Cu but could become significant for composites with large fiber-matrix transverse CTE and Young's modulus mismatch. The effect of nonuniform fiber distribution in the through-thickness direction of a laminate was more significant, but only approached that of the stress-free temperature for the most extreme cases that include large amounts of bending. Subsequent comparison with experimental thermal expansion data indicated the need for more accurate characterization of the graphite fiber thermomechanical properties. Correlation with cyclic data revealed the presence of a mechanism not considered in the developed models. The predicted response did, however, exhibit ratcheting behavior that has been observed experimentally in Gr/Cu. Finally, simulation of the actual fiber distribution of particular specimens had little effect on the predicted thermal expansion.

Bednarcyk, Brett A.↗

Development of design data for graphite reinforced epoxy and polyimide composites

Processing techniques and design data were characterized for a graphite/epoxy composite system that is useful from 75 K to 450 K, and a graphite/polyimide composite system that is useful from 75 K to 589 K. The Monsanto 710 polyimide resin was selected as the resin to be characterized and used with the graphite fiber reinforcement. Material was purchased using the prepreg specification for the design data generation for both the HT-S/710 and HM-S/710 graphite/polyimide composite system. Lamina and laminate properties were determined at 75 K, 297 K, and 589 K. The test results obtained on the skin-stringer components proved that graphite/polyimide composites can be reliably designed and analyzed much like graphite/epoxy composites. The design data generated in the program includes the standard static mechanical properties, biaxial strain data, creep, fatigue, aging, and thick laminate data.

Scheck, W. G.↗

Graphite fluoride fibers and their applications in the space industry

Characterization and potential space applications of graphite fluoride fibers from commercially available graphitized carbon fibers are presented. Graphite fluoride fibers with fluorine to carbon ratios of 0.65 and 0.68 were found to have electrical resistivity values of 10(exp 4) and 10(exp 11) Ohms-cm, respectively, and thermal conductivity values of 24 and 5 W/m-K, respectively. At this fluorine content range, the fibers have tensile strength of 0.25 + or - 0.10 GPa (36 + or - 14 ksi), Young's modulus of 170 + or - 30 GPa (25 + or - 5 Msi). The coefficient of thermal expansion value of a sample with fluorine to carbon ratio of 0.61 was found to be 7 ppm/C. These properties change and approach the graphite value as the fluorine content approach 0. Electrically insulative graphite fluoride fiber is at least five times more thermally conductive than fiberglass. Therefore, it can be used as a heat sinking printed circuit board material for low temperature, long life power electronics in spacecraft. Also, partially fluorinated fiber with tailor-made physical properties to meet the requirements of certain engineering design can be produced. For example, a partially fluorinated fiber could have a predetermined CTE value in -1.5 to 7 ppm/C range and would be suitable for use in solar concentrators in solar dynamic power systems. It could also have a predetermined electrical resistivity value suitable for use as a low observable material. Experimental data indicate that slightly fluorinated graphite fibers are more durable in the atomic oxygen environment than pristine graphite. Therefore, fluorination of graphite used in the construction of spacecraft that would be exposed to the low Earth orbit atomic oxygen may protect defect sites in atomic oxygen protective coatings and therefore decrease the rate of degradation of graphite.

Hung, Ching-Chen↗

Thermal oxidation of nuclear graphite and pyrolytic carbon coatings

The oxidation of pyrolytic carbon (PyC) deposited via fluidized bed chemical vapor deposition was characterized and compared with that of standard nuclear-grade graphite. The materials were heated at 700 to 1000 °C in a thermogravimetric analysis system under 20% v/v O 2 flow, allowing for direct comparison of dynamic oxidative mass change in each material. Further, three different PyC samples fabricated under different conditions exhibited variation in total mass loss and mass loss rate, varying by as much as 709 mg/cm 2 in total mass loss and 14.2 (mg/cm 2 )/min in mass loss rate at a single temperature. These variations highlight the correlation between PyC microstructure/defect density and oxidation susceptibility. Additionally, changes in the microstructure and composition between PyC and graphite were characterized via scanning electron microscopy and correlated to the mass loss results. The results of this work have implications toward the safety of tristructural isotropic (TRISO) and other coated particle fuels, especially under off-normal conditions, given the limited information that exists about the oxidation behavior of PyC.

36 MATERIALS SCIENCE↗

Progress Report on Graphite-Salt Interaction Studies (FY21)

This report summarizes the activities performed in FY21 to investigate the interactions between nuclear graphite and molten salts, such as FLiNaK. First, building on last year’s achievements, the team improved the procedure for measurements on pressurized salt intrusion in nuclear graphite and performed new experiments at variable pressures with specimens of different sizes and shapes. Additionally, the team actively provided suggestions and comments for ASTM D8091, Standard Guide for Impregnation of Graphite with Molten Salts , which came up for periodic revision in 2021. Second, the team expanded its capabilities to further characterize salt-impregnated graphite by procuring and installing a laser-induced breakdown spectroscopy (LIBS) instrument capable of producing a 3D chemical composition of a surface and subsurface region of specimens. A methodology for accurately analyzing information was developed, and a manuscript was submitted for publication. The LIBS instrument sample cell is sealed in controlled inert atmosphere, which is an advantage for using humidity-sensitive samples and Be-contaminated samples. This aligns with the team’s effort to expand the capabilities of handling FLiBe and Becontaining materials in two newly installed glovebox units. Third, the team performed preliminary tribology tests for pebble graphite wear in contact with stainless steel in dry state and in molten salt at high temperature. These tests are needed to establish the baseline for the wear of pebble graphite by friction against metallic walls. The friction and wear of pebbles in the fluoride salt-cooled hightemperature reactor are expected to generate dust, which is a concern for other components’ properties and safe reactor operation.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

A review of dynamic mechanical characterization of high temperature PMR polyimides and composites

This paper reviews the applications of dynamic mechanical characterization for high-temperature PMR polyimides and their graphite-fiber-reinforced composites. This characterization technique provides insights into the processability, performance, and structure property relationships of the polyimides and composites. The dynamic mechanical properties of various molding powders, commercially obtained prepregs, neat resins, and as-fabricated as well as aged composites are presented. Some applied aspects of the dynamic mechanical data are discussed.

Pater, Ruth H.↗

Development of polyphenylquinoxaline graphite composites

Six polyphenylquinoxalines (PPQ) containing pendant cyano (CN) groups were synthesized. The polymers were characterized in terms of inherent viscosity, glass transition temperature, softening temperature and weight loss due to aging in air at 316 C (600 F). The potential for crosslinking PPQs by trimerization of pendant CN groups was investigated. A polymer derived from 1 mole 3,3,4,4 -tetraaminobenzophenone, .2 mole p-bis(p -cyanophenoxyphenylglyoxalyl)benzene and .8 mole p-bis(phenylglyoxalyl)benzene was selected for more extensive characterization in HM-S graphite fiber-reinforced composites. Mechanical properties were determined using composites made from HM-S fiber and polymer and composites made from HM-S fiber, polymer and a potential CN group trimerization catalyst. Composite mechanical properties, inter-laminar shear strength and flexure properties, were determined over the temperature range of +21 C to 316 C.

Shdo, J. D.↗

Historic and modern nuclear graphite impurities: Pathways to improved waste strategies

Graphite has been used in large volumes as a structural material and neutron moderator since the earliest days of nuclear fission. However, no international consensus exists on the disposal of irradiated graphite, leaving much of the historic radioactive graphite inventory in interim vault or silo storage. With several new graphite-moderated reactors planned or under construction, the issue of graphite waste management is becoming increasingly urgent. This paper reviews and quantifies impurities in both historic and modern nuclear graphite, with emphasis on nitrogen—responsible for much of the 14 C inventory—and chlorine, which plays a critical role in repository performance and design. Modern graphites, benefitting from stringent quality-control measures developed for non-nuclear industries, meet or exceed the ASTM Ultra-High Purity nuclear standards, even without halide purification. Both chlorine and nitrogen concentrations have declined over time. For chlorine, identified as a key impurity influencing U.S. waste repository design, we propose a target of 0.1 appm in as-fabricated billets as a reasonable benchmark. Nitrogen sources are traced throughout the graphite production process, with surface and bulk concentrations characterized for all materials studied. Modern graphites commonly exhibit nitrogen levels below 5 appm, with values approaching 1 appm achievable. Using such reduced-nitrogen grades is critical to keeping graphite-induced radioactivity below the greater-than-Class-C waste threshold, thereby avoiding disposal cost penalties of nearly an order of magnitude.

Chlorine↗

Slides for MS&T2022: Carbon-Carbon Composites from 3D Printed Preforms Graphitized by Electric Field Assisted Sintering

Formation of Carbon-Carbon (C-C) composite materials requires putting a carbon fiber preform through a cycle of densification, carbonization, and graphitization. This cycle is then repeated until the desired properties are achieved. The graphitization phase is particularly energy demanding as it involves heating the components to in excess of 2000°C. In traditional furnaces this is also quite time consuming as typical heating rates are low, and the actual heat treatment may be limited by component dimensions, as heat is conducted throughout the part primarily by thermal diffusion. Joule heating by means of Electric Field Assisted Sintering (EFAS) systems enables high heating rates and causes the part to be heated from the inside, which eliminates the thermal diffusion time constraint. In our process, C-C composites are formed by pyrolyzation of 3D-printed carbon fiber preforms, vacuum infiltration of naphthalene based mesophase pitch, and carbonization. The part is then graphitized in the EFAS system. By this method graphitization of the composite matrix was achieved in less than an hour. A part density of greater than 1.6g/cc (up to 1.9g/cc demonstrated) was achieved after only two rounds of infiltration and a single graphitization. Overall the process took less than a week which is significantly faster than traditional methods. Optical microscopy and XRD results are discussed to elucidate the internal porosity and characterize the degree of graphitization. Testing was performed showing the impact on fiber direction to electrical and thermal properties of the final part.

36 MATERIALS SCIENCE↗

The effects of space radiation on a chemically modified graphite-epoxy composite material

The effects of the space environment on the engineering properties and chemistry of a chemically modified T300/934 graphite-epoxy composite system are characterized. The material was subjected to 1.0 x 10 to the 10th power rads of 1.0 MeV electron irradiation under vacuum to simulate 30 years in geosynchronous earth orbit. Monotonic tension tests were performed at room temperature (75 F/24 C) and elevated temperature (250 F/121 C) on 4-ply unidirectional laminates. From these tests, inplane engineering and strength properties (E sub 1, E sub 2, Nu sub 12, G sub 12, X sub T, Y sub T) were determined. Cyclic tests were also performed to characterize energy dissipation changes due to irradiation and elevated temperature. Large diameter graphite fibers were tested to determine the effects of radiation on their stiffness and strength. No significant changes were observed. Dynamic-mechanical analysis demonstrated that the glass transition temperature was reduced by 50 F(28 C) after irradiation. Thermomechanical analysis showed the occurrence of volatile products generated upon heating of the irradiated material. The chemical modification of the epoxy did not aid in producing a material which was more radiation resistant than the standard T300/934 graphite-epoxy system. Irradiation was found to cause crosslinking and chain scission in the polymer. The latter produced low molecular weight products which plasticize the material at elevated temperatures and cause apparent material stiffening at low stresses at room temperature.

Reed, S. M.↗

Multi-modal characterization methods of solid-electrolyte interphase in silicon-graphite composite electrodes

Composite silicon-graphite (Si-Gr) anodes can improve battery energy density, due to Si's high gravimetric capacity, while mitigating mechanical degradation of the anode and solid-electrolyte interphase (SEI) caused by Si volumetric expansion. Optimizing these anodes is challenging, in part due to difficulty characterizing the SEI structure and composition. In this work, we present multi-modal characterization of the SEI on composite Si-Gr anodes to relate SEI chemical composition and structure to functional properties. Discrepancies in elemental concentrations from X-ray photoelectron spectroscopy, Auger electron spectroscopy, and energy-dispersive X-ray spectroscopy (EDS) are attributed to varying information depth and lateral resolution of the individual probes. However, by combining quantitative composition information with spatially resolved element mapping from scanning transmission electron microscopy, EDS, and electron energy loss spectroscopy, a holistic picture of the SEI emerges. We observe the bilayer SEI structure and a direct correlation between elemental Li and F, suggesting that most Li in the SEI exists as lithium fluoride (LiF). Further, LiF concentration is directly proportional to the maximum SEI resistivity, as determined by scanning spreading resistance microscopy. Lastly, there is an inverse relationship between lithium carbonate and LiF concentration in the SEI, providing insight into the detailed chemistry of SEI formation and evolution.

25 ENERGY STORAGE↗