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At least 127 records · Page 7

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↗

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.↗

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↗

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↗

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.↗

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.↗

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.↗

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↗

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.↗

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↗

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↗

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↗

3D printed carbon fiber reinforced carbon as an energy efficient alternative to graphite for EFAS tooling

As Electric Field Assisted Sintering (EFAS) gains more industrial acceptance and use, it becomes more important to develop more efficient means to implement this technology. To this aim, 3D printed continuous carbon fiber reinforced carbon (CCC) was manufactured and fabricated into tooling for EFAS systems as an alternative to traditional graphite tooling. The impact of fiber orientation on the thermal and electrical properties of the CCC was characterized. Sample material was sintered in Tokai G535 graphite tooling, under common processing conditions and compared with CCC tooling. There was nearly 50 % energy savings compared to graphite while maintaining equivalent sample density and microstructure plus keeping ram temperatures 39 % cooler. This is due to spatial control of generated heat and thermal diffusivity within the molds, by means of fiber orientation anisotropy. Finite element modeling of the tooling design supported the experimental results as well as displays the effect of optimization of this 3D printed CCC material.

36 MATERIALS SCIENCE↗

Characteristics of graphene oxide-like materials prepared from different deashed-devolatilized coal chars and comparison with graphite-based graphene oxide, with or without the ultrasonication treatment

Deashed-devolatilized coal chars were prepared from anthracite, bituminous, subbituminous, and lignite coals, then oxidized to prepare graphene oxide (GO)-like materials that were extensively characterized and compared with a pristine graphite-based GO sample (CGO). Coal-based GO-like materials and CGO were then subjected to ultrasonication treatment for delamination, which also impacted their physicochemical properties. The surface oxygen contents of CGO and coal-based samples were ~32 % and ~26–35 %, respectively, that were reduced to ~27 % and ~21–24 %, respectively, after ultrasonication. The Fourier transform infrared and X-ray photoelectron spectroscopy spectra of all samples showed different profiles before and after the ultrasonication, suggesting a change in chemical functionalities. The Raman spectra of CGO and coal-based samples exhibited similar D and G bands with D/G intensity ratios (I D /I G ) of 0.93 and 0.88–0.92, respectively. The I D /I G ratio of CGO and most of the coal-based samples increased after the ultrasonication due to creation of more defects. The main X-ray diffraction (XRD) peak for CGO and coal-based samples were observed at ~11° and ~22–24°, respectively. Ultrasonication of the samples resulted in a reduction of crystallite size and number of layers for all CGO and coal-based samples, confirming both splitting and delamination of carbon layers. Additionally, different coal-based samples exhibited almost overlapping XRD profiles after the ultrasonication.

36 MATERIALS SCIENCE↗

Probing the Influence of Multiscale Heterogeneity on Effective Properties of Graphite Electrodes

Graphite electrodes in the lithium-ion battery exhibit various particle shapes, including spherical and platelet morphologies, which influence structural and electrochemical characteristics. It is well established that porous structures exhibit spatial heterogeneity, and the particle morphology can influence transport properties. The impact of the particle morphology on the heterogeneity and anisotropy of geometric and transport properties has not been previously studied. Herein, this study characterizes the spatial heterogeneities of 18 graphite electrodes at multiple length scales by calculating and comparing the structural anisotropy, geometric quantities, and transport properties (pore-scale tortuosity and electrical conductivity). We found that the particle morphology and structural anisotropy play an integral role in determining the spatial heterogeneity of directional tortuosity and its dependency on pore-scale heterogeneity. Our analysis reveals that the magnitude of in-plane and through-plane tortuosity difference influences the multiscale heterogeneity in graphite electrodes.

25 ENERGY STORAGE↗

High-temperature thermal conductivity measurements of macro-porous graphite

Graphite is a unique material for high temperature applications and will likely become increasingly important as we attempt to electrify industrial applications. Here, we investigate the thermal properties of low-quality, macro-porous graphite to determine the tradeoff between quality and thermal performance. We use laser flash analysis (LFA) to measure the thermal diffusivity of graphite at high temperatures. Due to the large pores in the graphite samples preventing uniform laser flash heating, we first apply a thick coating to achieve the required flat, parallel surfaces for LFA measurements. We then develop a methodology to extract properties of the sample from the diffusivity measurements, based on finite element modeling of a variety of sample/coating interface profiles. Validating the methodology against a reference sample demonstrates a mean absolute percentage error of 8.5%, with potential improvement with better sample characterization. We show low-quality graphite has a thermal conductivity of ~10 W/m/K up to 1000 °C, which is an order of magnitude lower than high-quality graphite, but contributions from photon conductivity may result in higher conductivities at higher temperatures. Overall, we demonstrate an approach for measuring thermal properties of macro-porous materials at high temperatures, and apply the approach to measuring thermal conductivity of porous graphite, which will aid in the design of hightemperature systems for cost-competitive decarbonization.

Verma, Shomik↗

Effect of microstructure and temperature on nuclear graphite oxidation using the 3D Random Pore Model

This work compared the 3D Random Pore Model (3D-RPM) with experimental and characterization data to systematically study the effect of nuclear graphite microstructure and air oxidation temperature. It is well known that oxidation-induced weight loss at elevated temperatures degrades graphite structure and properties; however, a fundamental understanding of the role of graphite microstructure is still unclear. In this work, three diverse grades of nuclear graphite—IG-110, NBG-18, and PCEA—were examined and tested at air oxidation temperatures of 600, 650, 700, and 750 °C following ASTM D7542. Here, the 3D-RPM reproduced the microstructure and temperature dependence of mass loss curves for these grades. For the first time, measurements and modeling were combined to show how bulk density and the amount and spatial distribution of open and closed porosity affects oxidation. IG-110 was less dense and had an open pore network that is finer and more uniformly spread, and showed fastest oxidation. PCEA porosity was less uniform and showed less oxidation, while NBG-18 was more dense, had the least fine and uniform porosity, and showed the slowest oxidation. In general, oxidation proceeds faster if open porosity is more uniformly distributed and can incrementally access closed pore surface area with more ease.

36 MATERIALS SCIENCE↗