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At least 181 records · Page 10

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.↗

Fabrication and physicochemical characterization of graphene oxide derived from thermally expanded graphite

Graphene oxide was obtained from expanded graphite according to the modified Hummers method. The reaction time was significantly reduced (from 24 to 8 h) by applying the expanded graphite in the oxidation process. The interlayer distance in obtained samples was equal to 0.70–0.74 nm. Structural features of the material were studied by the powder X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, transmission electron microscopy, XPS spectroscopy, and NMR spectroscopy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterization of Vacancy Defects in Carbon Ion Irradiated Graphite Using Positrons

Highly Oriented Pyrolytic Graphite samples are irradiated with 200 keV Carbon ions to fluences of 10{sup 14} and 10{sup 15} C{sup +} ions/cm{sup 2}. Depth resolved Doppler lineshape S-parameter exhibited large increase in peak damage regions of the sample, indicating the existence of irradiation induced vacancy defects. The depth profile of the defect region has been deduced from the analysis of the experimental data. It is found that divacancies are the dominant defects in the irradiated samples.

36 MATERIALS SCIENCE↗

Three-dimensional EBSD characterization of thermo-mechanical fatigue crack morphology in compacted graphite iron

In cylinder heads made of compacted graphitic iron (CGI), heating and cooling cycles can lead to localized cracking due to thermo-mechanical fatigue (TMF). To meticulously characterize the complex crack path morphology of CGI under TMF condition, in relation to microstructural features and to find out how and by which mechanisms the cracks predominantly develop, three-dimensional electron back scattering diffraction (EBSD) was employed. Based on the precise quantitative microstructural analysis, it is found that graphite particles not only play a crucial role in the crack initiation, but also are of primary significance for crack propagation, i.e. crack growth is enhanced by the presence of graphite particles. Furthermore, the density of graphite particles on the fracture plane is more than double as high as in any other arbitrary plane of the structure. The obtained results did not indicate a particular crystallographic preference of fracture plane, i.e. the crystal plane parallel to the fracture plane was nearly of random orientation. - Highlights: • Crystallographic features of a thermo-mechanical fatigue (TMF) crack were studied. • Wide-field 3D EBSD is used to characterize the TMF crack morphology. • Data processing was applied on a large length scale of the order of millimeters. • Graphite density in the fracture plane is much higher than any other random plane. • It is revealed that crack growth is enhanced by the presence of graphite particles.

36 MATERIALS SCIENCE↗

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↗

Time-resolved spectroscopy of CI and CII line emissions from an ultrafast laser induced solid graphite plasma

We present an experimental characterization of the evolution dynamics of CI and CII lines in an ultrafast laser produced graphite plasma under various ambient conditions. Fast and slow components are observed in the temporal evolution of CI transition at 658.7 nm (3p{sup 1}P - 4d{sup 1}P{sup 0}) and CII transition at 426.7 nm (3d {sup 2}D - 4f {sup 2}F{sup 0}). Fast peak is due to the recombination of fast ions species with electrons, found to have an increase in velocity upon increasing the ambient pressure. Whereas the slow peaks in both cases can be the results of slow ions or slow neutrals in the plume.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

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.↗

AGC-4 Graphite Preirradiation Data Analysis Report

The Advanced Reactor Technology (ART) Graphite R&D program is conducting an extensive graphite irradiation program to provide data for licensing of a high temperature reactor (HTR) design. In past applications, graphite has been used effectively as a structural and moderator material in both research and commercial high temperature gas cooled reactor (HTGR) designs. Nuclear graphite H 451, used previously in the United States for nuclear reactor graphite components, is no longer available. New nuclear graphite grades have been developed and are considered suitable candidates for new HTR reactor designs. To support the design and licensing of new HTR core components within a commercial reactor, a complete properties database must be developed for these current grades of graphite. Quantitative data on in service material performance is required for the physical, mechanical, and thermal properties of each major graphite grade with a specific emphasis on data accounting for the life limiting effects of irradiation creep on key physical properties of the HTR candidate graphite grades. Further details on the research and development activities and associated rationale required to qualify nuclear grade graphite for use within the HTR are documented in the graphite technology research and development plan. Based on experience with previous graphite core components, the phenomenon of irradiation induced creep within the graphite has been shown to be critical to the total useful lifetime of graphite components. Irradiation induced creep occurs under the simultaneous application of high temperatures, neutron irradiation, and applied stresses within the graphite components. Significant internal stresses within the graphite components can result from a second phenomenon—irradiation induced dimensional change—where the graphite physically changes (i.e., first shrinking and then expanding with increasing neutron dose). This disparity in material volume change can produce significant internal stresses within graphite components. Irradiation induced creep relaxes these large internal stresses, thus reducing the risk of crack formation and component failure. Obviously, higher irradiation creep levels tend to relieve more internal stress, thus allowing the components longer useful lifetimes within the core. Determining the irradiation creep rates of nuclear grade graphite is critical for determining the useful lifetime of graphite components and is a major component of the Advanced Graphite Creep (AGC) experiment. The AGC experiment is currently underway to determine the in service behavior of these new graphite grades for HTR and molten salt reactor designs. This experiment will examine properties and behavior of nuclear grade graphite over a large spectrum of temperatures, irradiation fluencies and applied stress levels that are expected to cause irradiation creep strains within a HTR graphite component. Irradiation data are provided through the AGC test series, which is comprised of six planned capsules irradiated in the Advanced Test Reactor (ATR) in a large flux trap located at Idaho National Laboratory (INL). Each irradiation capsule consists of over 400 graphite specimens that are characterized before and after irradiation to determine the irradiation induced material properties changes and life-limiting irradiation creep rate for each graphite grade.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

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.↗

Laser-induced dehydration of graphite oxide coatings on polymer substrates

Nanosized graphite has been oxidized by the Hummers method to give high quality graphite oxide. This reaction is characterized by a very fast kinetic behavior and a high yield. The produced graphite oxide has been conveniently used to pattern graphene by using a standard photolithographic method, and the resulting systems have been characterized by optical microscopy (OM), scanning electron microscopy (SEM) and by Fourier transform infrared spectroscopy (FT-IR) and Visible-Near Infrared spectroscopy (Vis-NIR)

77 NANOSCIENCE AND NANOTECHNOLOGY↗

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↗

Carbon nanomaterial produced by microwave exfoliation of graphite oxide: new insights.

We present detailed characterization of graphene-like material obtained through microwave stimulated exfoliation of graphite oxide (GO). Properties of this material were studied by multiple techniques including, among others, X-ray photoelectron spectroscopy, mass-spectroscopy, infrared and Raman spectroscopy, scanning electron microscopy and broadband dielectric spectroscopy. Specific surface area and volume of microwave exfoliated graphite oxide reached 600 m2 g1 and 6 cm3 g1, respectively. It is shown that during such an explosive reduction process the sample emits CO2, CO and H2O and, in some cases, SO2 gases. The resulting reduced material exhibits IR spectra similar to that of graphite and a dc-conductivity of 0.12 S cm1.

Shulga, Y. M.↗

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.↗