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At least 235 records · Page 13
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Highly Crystalline Graphite Synthesis from Coal with a Sustainable Process

Synthetic graphite is made predominantly from a petroleum-derived needle coke using the Acheson method. This involves heating the needle coke at elevated temperatures of ~ 3000 °C for more than 7 days. High-temperature heating is the most technically challenging, expensive, and energy-intensive aspect of graphite manufacturing. We will present a strategy for synthesizing high-quality graphite powder from coal using a low-temperature catalytic graphitization process. The use of a catalyst drops the processing temperatures to 1500 °C and processing times to a few hours. The graphite produced with this process has been characterized and has been shown to have comparable physical/chemical properties with commercially sourced graphite materials. We will also present a sustainable method to recover and reuse the catalyst and acid used to retrieve the catalyst. This overcomes a long-standing technical hurdle associated with using catalysts for manufacturing graphite.

crystalline graphite powder↗
NASA NTRS2011

Improved Flaw Detection and Characterization with Difference Thermography

Flaw detection and characterization with thermographic techniques in graphite polymer composites is often limited by localized variations in the thermographic response. Variations in properties such as acceptable porosity, variations in fiber volume content and surface polymer thickness result in variations in the thermal response that in general cause significant variations in the initial thermal response. These variations result in a noise floor that increases the difficulty of detecting and characterizing deeper flaws. The paper investigates comparing thermographic responses taken before and after a change in state in a composite to improve the detection of subsurface flaws. A method is presented for registration of the responses before finding the difference. A significant improvement in the detectability is achieved by comparing the differences in response. Examples of changes in state due to application of a load and impact are presented.

Winfree, William P.↗
DOE OSTI2015

PCEA Baseline Characterization: Billet XCP01S8 11 Compressive, Tensile, and Flexure Strengths

Grade PCEA graphite is one of several grades being considered for the core structures of the Next Generation Nuclear Plant (NGNP). An experimental program is underway to describe the statistical nature of the mechanical properties of PCEA graphite, information needed to support the design of graphite components and licensing of the NGNP. It will be necessary to characterize several billets from various lots or batches. The exact number of billets will depend on the observed variability in properties.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2016

EBSD characterization of the growth mechanism of SiC synthesized via direct microwave heating

Well-crystallized 3C-silicon carbide (SiC) grains/nanowires have been synthesized rapidly and conveniently via direct microwave heating, simply using silicon dioxide powders and artificial graphite as raw materials. The comprehensive characterizations have been employed to investigate the micro-structure of the obtained 3C-SiC products. Results indicated that, different from the classic screw dislocation growth mechanism, the 3C-SiC grains/nanowires synthesized via high-energy vacuum microwave irradiation were achieved through the two-dimension nucleation and laminar growth mechanism. Especially, the electron backscattered diffraction (EBSD) was employed to characterize the crystal planes of the as-grown SiC products. The calculated Euler angles suggested that the fastest-growing crystal planes (211) were overlapped gradually. Through the formation of the (421) transformation plane, (211) finally evolved to (220) which existed as the side face of SiC grains. The most stable crystal planes (111) became the regular hexagonal planes in the end, which could be explained by the Bravais rule. The characterization results of EBSD provided important experimental information for the evolution of crystal planes. - Graphical abstract: The formation of 3C-SiC prepared via direct microwave heating follows the mechanism of two-dimension nucleation and laminar growth. - Highlights: • 3C−SiC grains/nanowires were obtained via direct microwave heating. • 3C−SiC followed the mechanism of two-dimension nucleation and laminar growth. • In-situ EBSD analysis provided the experimental evidences of the growth.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Experimental study on a simplified facility of HTGR reactor building response to depressurization accidental scenarios - 18516

The analysis and understanding of air ingress events is an important aspect in the design of The High Temperature Gas Cooled Reactor (HTGR) accident scenarios including Depressurized Loss of Forced Cooling (D-LOFC) events that allow for the possibility of air ingress into the Reactor Pressure Vessel (RPV) as the result of a break in the helium pressure boundary which can ultimately result in oxidation of the fuel elements and other nuclear-grade graphite components. In order to characterize the air ingress into the vented low pressure compartments (VLPC) of NGNP HTGR during hypothetical small break D-LOFC accidents experimentally, a 1/28 down scaled simplified reactor building model was developed. A non-dimensional similarity approach was employed for the scaling analysis of the experimental facility. Two experiments were conducted under similar experimental conditions, with 1.1 kg/h helium injection through the top of the reactor cavity, resulting in oxygen concentrations reaching to steady state within 4 minutes. Differences between the steady state oxygen concentrations results in the steam generator cavity of the two tests with the same experimental conditions were 0.51{+-}0.086% at the top of the steam generator cavity and 0.29{+-}0.11% at the bottom of the steam generator cavity. Difference in the pressure in the reactor between the two experiments were 0.09{+-}0.026 psig. (authors)

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2022

Using porous random fields to predict the elastic modulus of unoxidized and oxidized superfine graphite

Nuclear graphite is a candidate material for Generation IV nuclear power plants. Porous materials such as graphite can contain complex networks of pores that influence the material's mechanical and irradiation response. A methodology known as the random finite element method (RFEM) was adapted to create synthetic microstructures and predict the influence of porosity on the elastic properties of graphite during oxidation. RFEM combines random field theory and the finite element method in a Monte Carlo framework to estimate the mechanical response of a given grade of graphite. In this research, the random fields were verified through experimental characterization to predict the elastic response of three nuclear graphite grades, ETU-10, IG-110, and 2114. Finite element models (FEM) were generated using segmentations of x-ray computed tomography (XCT) data known as image-based models (IBMs) to validate and compare with the RFEM results and better understand the effects of uniform oxidation in these graphite grades. The RFEM predictions appear to correlate well with the experimental values of the measured Young’s modulus of the three graphite grades and display the same trends as IBMs.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Local measurement of bulk thermal diffusivity using photothermal radiometry

Here, an experimental methodology using photothermal radiometry is developed for the accurate measurement of bulk thermal diffusivity of nuclear fuels and materials irradiated to high doses. Under these conditions, nuclear fuels, such as uranium oxide, and moderator materials, such as graphite, become friable, which requires characterization techniques that can accommodate irregularly shaped fragments. Photothermal radiometry, a good candidate for this application, involves locally heating a sample by using a laser and measuring the temperature field by monitoring blackbody radiation. The interaction volume for this study, less than a millimeter, is carefully chosen to sample a statistically significant number of large-scale structural features, such as pores and gas filled bubbles, and is small enough that the sample fragments can be treated as a thermal half-space. The thermal diffusivity standards considered in this study cover a range of thermal diffusivities representative of both fresh and spent nuclear fuels. We also consider a sample having a porous microstructure representative of large-scale structures found in materials irradiated to high doses. Our measurement methodology circumvents complex thermal wave models that address optical diffraction, nonlinear transfer function associated with blackbody radiation, and finite sample size effects. Consequently, the large measurement uncertainty associated with modeling these effects can be avoided. While the emphasis here is on nuclear fuels and materials, this measurement approach is well suited to measure thermal transport in a variety of technologically important materials associated with advanced synthesis techniques. Examples range from small, exotic single crystals grown using hydrothermal growth techniques to additively manufactured components having complex geometries.

36 MATERIALS SCIENCE↗
NASA NTRS1974

Polyimide resin composites via in situ polymerization of monomeric reactants

Thermo-oxidatively stable polyimide/graphite-fiber composites were prepared using a unique in situ polymerization of monomeric reactants directly on reinforcing fibers. This was accomplished by using an aromatic diamine and two ester-acids in a methyl alcohol solvent, rather than a previously synthesized prepolymer varnish, as with other A-type polyimides. A die molding procedure was developed and a composite property characterization conducted with high modulus graphite fiber tow. Flexure, tensile, compressive, and shear tests were conducted at temperatures from 72 to 650 F on laminates before and after exposures at the given temperatures in an air environment for times up to 1000 hours. The composite material was determined to be oxidatively, thermally, and hydrolytically stable.

Cavano, P. J.↗
NASA NTRS1989

A (13)C NMR analysis of the effects of electron radiation on graphite/polyetherimide composites

Initial investigations have been made into the use of high resolution nuclear magnetic resonance (NMR) for the characterization of radiation effects in graphite and Kevlar fibers, polymers, and the fiber/matrix interface in graphite/polyetherimide composites. Sample preparation techniques were refined. Essential equipment has been procured. A new NMR probe was constructed to increase the proton signal-to-noise ratio. Problem areas have been identified and plans developed to resolve them.

Ferguson, Milton W.↗
NASA NTRS1988

An investigation of the temperature dependence of the ultrasonic properties of AS4/lexan and XAS/lexan composites

An investigation of the temperature dependence of the ultrasonic properties of AS4/lexan and XAS/lexan composites is summarized. In particular, a technique for determination of velocity and attenuation as a function of temperature, for both the matrix and composite materials is determined. The separation of contributions of the matrix and fiber to ultrasonic propagation and scattering is discussed. Work begun on the characterization of wave propagation in graphite fiber/polymer matrix composites is described.

Smith, B. T.↗
NASA NTRS1990

Effects of heat treatment on carbon fibers

Commercially produced carbon fibers were heat treated to graphitization temperatures. The fibers were characterized for mechanical and physical properties, including density, D0002 spacing, strength, and modulus in both the 'as received' and heat treated conditions. Mechanical property changes were correlated with the physical property changes in the fibers.

Brown, D. Kyle↗
NASA NTRS1991

Temperature effects on high strain rate properties of graphite/epoxy composites

A unidirectional graphite epoxy material (AS4/3501-6) was characterized at strain rates ranging from 5 x 10(exp 6) s(exp -1) to 5(exp -1), at room temperature and at 128 C. Results are presented in the form of stress-strain curves to failure. The longitudinal properties remain nearly unchanged with strain rate and temperature. The transverse modulus increases with strain rate but decreases with temperature. The transverse strength and transverse ultimate tensile strain have a positive rate sensitivity at low rates, which changes to negative at intermediate rates and returns to positive rate sensitivity at the highest rates tested. A temperature-time equivalence principle was applied and master curves were obtained for the transverse mechanical properties. The in-plane shear modulus and in-plane shear strength have a positive rate sensitivity. The ultimate intralaminar shear strain has a positive rate sensitivity at low rates, which changes to negative at high rates. At the elevated temperature of 128 C, the ultimate shear strain is 25 to 30 percent higher than the room temperature value, but its strain rate dependence is moderate.

Yaniv, G.↗
DOE OSTI2025

Friction and wear of nuclear graphite exposed to molten FLiNaK salt environment

This report formally documents the completion of the Advanced Reactor Technologies Level 3 Milestone (M3TG-25OR0501104), “Initiate graphite wear studies of graphite samples exposed to molten salt environment,” due August 1, 2025. The report summarizes the ongoing activities aimed at characterizing the friction and wear behavior of graphite in molten LiF–NaF–KF (FLiNaK) salt environment. The wear and friction behavior of self-mated ET-10 nuclear graphite were tested at varying temperatures (550°C and 650°C), contact loads (40 and 80 N) and sliding speeds (1 and 10 mm/s) in a controlled argon environment. The results were compared to the wear and friction behavior of the same graphite material in a dry argon environment. This report presents initial studies on the friction and wear behavior of graphite in sliding contact mode, with future work focused on investigating the graphite matrix materials, as well as rolling and impact contact modes. The outcomes of this report could provide insights into assessing the integrity of the graphitic components of pebble-bed fluoride salt–cooled high-temperature reactors (PB-FHRs) to enhance their safe operation.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2016

Topological Defects in Graphite under Irradiation using Molecular Dynamics

Graphite is the preferred material for moderating elements and structural components in a Very High Temperature Reactor (VHTR). It has a layered structure with basal planes constituted by carbon atoms arranged in a hexagonal lattice. Graphite accommodates a wide variety of defects such as vacancies, interstitials, and dislocation loops; a detailed description can be found in a review paper by Telling and Heggie. The layered configuration in graphite engenders energetic conditions that favor the formation of topological defects. Unlike the interlayer defects, which often are sp{sup 3} hybridized, topological defects maintain their sp{sup 2} bond connectivity. Several types of topological defects are known to arise in graphite; one of the most recognizable defects corresponds to a 5-7 Stone-Wales (SW) configuration that arises by a simple rotation of bonds. While the bond rotations result in a defected configuration, each carbon atom is still bonded to three other carbon atoms in the SW configuration, albeit with different bond lengths. Topological defects are expected to arise in irradiated graphite. A recent investigation with Raman and XPS spectroscopy have concluded that a large number of such defects are generated under neutron irradiation; an earlier ab-initio investigation has also arrived at the same conclusion. While several molecular dynamics (MD) simulations have been reported on irradiated graphite in the past, none have characterized the evolution of defects that are topological in nature. Using MD simulations, the current investigation quantifies the evolution and the distribution of topological defects under irradiation. Using MD simulations, we establish the presence of 5 and 7 membered topological defects in graphite following radiation. There is a greater probability for the formation of a 7 member ring relative to that of a 5 member ring. Since a heptagon causes a lower distortion to the 120 deg. bond angle of the sp{sup 2} hybridized orbital than a pentagon it is plausible to expect a larger number of 7 member rings following a radiation perturbation. Using a spatial distribution analysis, we have verified that 7 member rings tend to stay adjacent to 5 member rings as in Stone-Wales (SW) configuration. Since there are unequal number of 5 and 7 member rings, it follows that there are several isolated 7 member topological defects in graphite following radiation, possibly connected to dangling bonds or non-planar (sp{sup 3}) defects.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Irradiation-Induced Defect Evolution in Nuclear Graphite

Graphite has historically been used as a moderator material in nuclear reactor designs dating back to the first man-made nuclear reactor to achieve criticality (Chicago Pile 1) in 1942. Additionally, graphite is a candidate material for use in the future envisioned next-generation nuclear reactors (Gen IV); specifically, the molten-salt-cooled (MSR) and very-high-temperature reactor (VHTR) concepts. Gen IV reactor concepts will introduce material challenges as temperature regimes and reactor lifetimes are anticipated to far exceed those of earlier reactors. Irradiation-induced defect evolution is a fundamental response in nuclear graphite subjected to irradiation. These defects directly influence the many property changes of nuclear graphite subjected to displacing radiation; however, a comprehensive explanation for irradiation-induced dimensional change remains elusive. The objectives of this project were focused on the characterization of irradiation-induced defect evolution in nuclear graphite via transmission electron microscopy (TEM). With the use of novel TEM specimen preparation techniques, high-temperature electron-irradiation and characterization of high-temperature neutron-irradiated nuclear graphite, novel fullerene-like defects are shown to be a dominant defect type, especially at higher temperatures. These results contradict the historical models of defect evolution and provide valuable insight into the macroscopically observed property changes in irradiated nuclear graphite.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
NASA NTRS2020

Impact Shock Origin of Diamonds in Ureilite Meteorites

The origin of diamonds in ureilite meteorites is a timely topic in planetary geology as recent studies have proposed their formation at static pressures >20 GPain a large planetary body, like diamonds formed deep within the Earth ́s mantle. We investigated fragments of three diamond-bearing ureilites (two from the Almahata Sitta polymict ureilite and one from the NWA 7983 main group ureilite). In NWA7983 we found an intimate association of large monocrystalline diamonds (up to atleast 100 μm), nanodiamonds, nanographite, and nanometric grains of metallic iron,cohenite, troilite and likely schreibersite. The diamonds show a striking texture pseudo morphing inferred original graphite laths.The silicates in NWA 7983 recorda high degree of shock metamorphism. The presence of both large mono crystalline diamonds and nano diamonds in a highly shocked ureilite can be explained by catalyzed transformation from graphite during an impact shock event characterized by peak pressures possibly as low as 15 GPa for relatively long duration (on the scale of few seconds). The formation of “large” (as opposed to nano-) diamond crystals could have been enhanced by the catalytic effect of metallic Fe-Ni-C liquid coexisting with graphite. We found no evidence that formation of micrometer(s)sized diamonds or associated Fe-S-P phases in ureilites require high static pressures and long formation times. It is unlikely that any of the diamonds in ureilites formed in bodies as large as Mars or Mercury.

Fabrizio Nestola↗
DOE OSTI2011

Amorphous Interface Layer in Thin Graphite Films Grown on the Carbon Face of SiC

Cross-sectional transmission electron microscopy (TEM) is used to characterize an amorphous layer observed at the interface in graphite and graphene films grown via thermal decomposition of C-face 4H-SiC. The amorphous layer does not cover the entire interface, but uniform contiguous regions span microns of cross-sectional interface. Scanning transmission electron microscopy (STEM) images and electron energy loss spectroscopy (EELS) demonstrate that the amorphous layer is a carbon-rich composition of Si/C. The amorphous layer is clearly observed in samples grown at 1600 C for a range of growth pressures in argon, but not at 1500 C, suggesting a temperature-dependent formation mechanism.

77 NANOSCIENCE AND NANOTECHNOLOGY↗