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DOE OSTI2016

Characterization of LiFePO{sub 4} cathode by addition of graphene for lithium ion batteries

The improvement of LiFePO{sub 4} (LFP) cathode performance has been performed by addition of Graphene (LFP+Graphene). The cathode was prepared from the active material with 5 wt % graphene and 10 wt % polyvinylidene fluoride in an n-methyl pyrrolidone solvent. Another cathode material used only 5% artificial graphite for comparison (LFP+Graphite). The crystal structure, microstructure, electronic conductivity, electrochemical impedance spectroscopy (EIS) of the cathodes were characterized by X-ray diffraction, SEM, and Impedance spectroscopy, respectively. Two half cell coin batteries were assembled using a lithium metal as an anode and LiPf{sub 6} as an electrolyte, and two cathodes (LFP+Graphene) and (LFP+Graphite). Charge discharge performance of battery was characterized by Battery analyser (BTS 8). The electronic conductivity of cathode with grapheme increased of about one order magnitude compared with the only cathode with graphite, namely from 1.97E-7S/cm (LFP+Graphite) to 1.92E-6S/cm (LFP+Graphene). The charge-discharge capacity after 10{sup th} cycles of LiFePO{sub 4} with graphene decreased of about 0.68% from 114.3 mAh/g to113.1 mAh/g, while LFP with graphite decreased of about 2.84% from 110.2 mAh/g to 107.1 mAh, at 0.1C-rates. It could be concluded that the addition of graphene has increased the ionic conductivity, and improved performance of the LFP lithium ion battery, such as higher capacity and better efficiency.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Effects of High-Temperature Irradiation on the Microstructure of Nuclear Graphite

This report summarizes the nondestructive microstructure characterization undertaken at Oak Ridge National Laboratory (ORNL) to understand the effects of high-temperature neutron irradiation on the structure of nuclear graphite. Nuclear graphite specimens were irradiated in the ORNL High Flux Isotope Reactor (HFIR) in the High Temperature Vehicle (HTV) with target irradiation temperatures of 900ºC, 1200ºC, and 1500ºC [1, 2]. The experiment was irradiated in the HFIR flux trap for two irradiation cycles, providing the specimens in the highest-fluence positions a total exposure of 4.5×10 21 n/cm 2 [E>0.1 MeV], equivalent to radiation damage of ~3.3 dpa (displacements per atom) according to the conversion factor in Burchell [3].

36 MATERIALS SCIENCE↗

DOE OSTI2016

Graphitized hollow carbon spheres and yolk-structured carbon spheres fabricated by metal-catalyst-free chemical vapor deposition

Hard-sphere-templating method has been widely used to synthesize hollow carbon spheres (HCSs), in which the spheres were firstly coated with a carbon precursor, followed by carbonization and core removal. The obtained HCSs are generally amorphous or weakly graphitized (with the help of graphitization catalysts). In this work, we report on the fabrication of graphitized HCSs and yolk–shell Au@HCS nanostructures using a modified templating method, in which smooth, uniform graphene layers were grown on SiO 2 spheres or Au@SiO 2 nanoparticles via metal-catalyst-free chemical vapor deposition (CVD) of methane. Furthermore, our work not only provides a new method to fabricate high-quality, graphitized HCSs but also demonstrates a reliable approach to grow quality graphene on oxide surfaces using CVD without the presence of metal catalysts.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Multiscale characterization and comparison of historical and modern nuclear graphite grades

Beginning with Chicago Pile I, graphite has been used as a moderator material in nuclear power stations and is considered a potential material for use in future Generation IV advanced reactors. The microstructure of graphite is responsible for much of its mechanical and thermo-physical properties, and how it responds to irradiation. To understand graphite microstructure, it is necessary to understand its porosity at the macro- and micro-scales; and to understand its porosity, it is necessary to characterize the morphological connectivity of the void content and the two main phases of graphite: filler and binder. Here, using several microscopy and analytical techniques, a detailed examination of the heterogeneity, microstructure and pore structure of different graphite grades and their binder and filler phases is presented. Significant differences were found between coarser and finer nuclear grades. Coarse grades have a more diverse range of filler particles, pores and thermal cracks. Finer grades have a more well-defined pore size distribution, fewer variations of filler particles sizes and do not contain as many large thermal cracks. Fine grades tend to have a well-connected network of pores whereas coarser grades contain a larger content of closed porosity. The framework developed within this work can be applied and used to assess the various graphite grades that would down-select materials for specific use in graphite moderated reactor designs.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2025

Comprehensive defect evaluation of advanced nuclear fuels using high-resolution acoustic signals and optimized sensor separation

Graphite pebble composite structures based on TRistructural-ISOtropic (TRISO) particles are being developed as core nuclear fuels in advanced power reactors, promising safe operation at increased temperatures. Ensuring the structural integrity of these nuclear fuels requires comprehensive and accurate non-destructive evaluation (NDE) techniques to characterize defects and damage in the pebbles. However, traditional acoustic evaluation methods face limitations in defect characterization due to the highly attenuative, and geometrically and compositionally complex nature of these structures. This study proposes an improved acoustic NDE technique for accurate detection and classification of anticipated relevant defects and damage in graphite pebbles using high-resolution acoustic signals and optimized transmit-receive sensor networks. The proposed approach utilizes a triangular three-sensor network as the base unit, comprising three transmit-receive sensors. The sensor separation distance, as well as acoustic excitation center frequency, pulse-width, and bandwidth are optimized to enhance spatial resolution and improve signal-to-noise ratio, enabling effective characterization of the smallest size and widest range of defects in pebbles. Furthermore, the use of the triangular sensor configuration instead of a more conventional transmit-receive sensor pair expands the inspection region from a one-dimensional linear path to a two-dimensional area, increasing spatial coverage. To mitigate challenges associated with processing of complex acoustic signals arising from high-frequency, high-bandwidth excitation in these structures, a machine-learning-based signal processing algorithm is integrated with the sensor network. In the machine-learning-based algorithm, multi-domain features are extracted from the acoustic signals to capture intricate signal characteristics, significantly improving defect identification and classification compared to traditional approaches. The proposed acoustic NDE technique offers considerable promise for practical and reliable defect/damage diagnostics of advanced nuclear pebble fuels.

42 ENGINEERING↗

DOE OSTI2024

Influence of gadolinium doping on structural, optical, and electronic properties of polymeric graphitic carbon nitride

Polymeric graphitic carbon nitride (gCN) materials have received great attention in the fields of photo and electrocatalysis due to their distinct properties in metal-free systems with high physicochemical stability. Nevertheless, the activity of undoped gCN is limited due to its relatively low specific surface area, low conductivity, and poor dispersibility. Doping Gd atoms in a gCN matrix is an efficient strategy to fine-tune its catalytic activity and its electronic structure. Herein, the influence of various wt% of gadolinium (Gd) doped in melon-type carbon nitride was systematically investigated. Gadolinium-doped graphitic carbon nitride (GdgCN) was synthesized by adding gadolinium nitrate to dicyandiamide during polymerization. The X-ray diffraction (XRD) and transmission electron microscopy (TEM) results revealed that the crystallinity and the morphological properties are influenced by the % of Gd doping. Furthermore, X-ray photoelectron spectroscopy (XPS) studies revealed that the gadolinium ions bonded with nitrogen atoms. Complementary density functional theory (DFT) calculations illustrate possible bonding configurations of Gd ions both in bulk material and on ultrathin melon layers and provide evidence for the corresponding bandgap modifications induced by gadolinium doping.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Production of an impermeable composite of irradiated graphite and glass by hot isostatic pressing as a long term leach resistant waste form

Around 250,000 tons of irradiated graphite (i-graphite) exists worldwide and can be considered as a current waste or future waste stream. The largest national i-graphite inventory is located in UK (∼ 100,000 tons) with significant quantities also in Russia and France [5]. Most of the i-graphite remains in the cores of shutdown nuclear reactors including the MAGNOX type in UK and the UNGG in France. Whilst there are still operational power reactors with graphite cores, such as the Russian RBMKs and the AGRs in UK, all of them will reach their end of life during the next two decades. The most common reference waste management option of i-graphite is a wet or dry retrieval of the graphite blocks from the reactor core and the grouting of these blocks in a container without further conditioning. This produces large waste package volumes because the encapsulation capacity of the grout is limited and large cavities in the graphite blocks could reduce the packing densities. Packing densities from 0.5 to 1 tons per cubic meter have been assumed for grouting solutions. Furthermore the grout is permeable. This could over time allow the penetration of aqueous phases into the waste block and a potential dissolution and release of radionuclides. As a result particularly highly soluble radionuclides may not be retained by the grout. Vitrification could present an alternative, however a similar waste package volume increase may be expected since the encapsulation capacity of glass is potentially similar to or worse than that of grout. FNAG has developed a process for the production of a graphite-glass composite material called Impermeable Graphite Matrix (IGM) [3]. This process is also applicable to irradiated graphite which allows the manufacturing of an impermeable material without volume increase. Crushed i-graphite is mixed with 20 vol.% of glass and then pressed under vacuum at an elevated temperature in an axial hot vacuum press (HVP). The obtained product has zero or negligible porosity and a water impermeable structure. Structural analysis shows that the glass in the composite has replaced the pores in the graphite structure. The typical pore volume of a graphite material is in the range of 20 vol.%. Therefore no volume increase will occur in comparison with the former graphite material. This IGM material will allow the encapsulation of graphite with package densities larger than 1.5 ton per cubic meter. Therefore a huge volume saving can be achieved by such an alternative encapsulation method. Disposal performance is also enhanced since little or no leaching of radionuclides is observed due to the impermeability of the material NNL and FNAG have proved that IGM can be produced by hot isostatic pressing (HIP) which has several advantages for radioactive materials over the HVP process. - The sealed HIP container avoids the release of any radionuclides. - The outside of the waste package is not contaminated. - The HIP process time is shorter than the HVP process time. The isostatic press avoids anisotropic density distributions. - Simple filling of the HIP container has advantages over the filling of an axial die. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS1986

Surface control system for the 15 meter hoop-column antenna

The 15-meter hoop-column antenna fabricated by the Harris Corporation under contract to the NASA Langley Research Center is described. The antenna is a deployable and restowable structure consisting of a central telescoping column, a 15-meter-diameter folding hoop, and a mesh reflector surface. The hoop is supported and positioned by 48 quartz cords attached to the column above the hoop, and by 24 graphite cords from the base of the antenna column. The RF reflective surface is a gold plated molybdenum wire mesh supported on a graphite cord truss structure which is attached between the hoop and the column. The surface contour is controlled by 96 graphite cords from the antenna base to the rear of the truss assembly. The antenna is actually a quadaperture reflector with each quadrant of the surface mesh shaped to produce an offset parabolic reflector. Results of near-field and structural tests are given. Controls structures and electromagnetics interaction, surface control system requirements, mesh control adjustment, surface control system actuator assembly, surface control system electronics, the system interface unit, and control stations are discussed.

Miller, James B.↗

DOE OSTI2020

Radiation Effects in Graphite

Graphite has been a core structural material and neutron moderator since the first man-made chain reaction experiment in Chicago. This article will discuss the requirements of what makes graphite a good solid moderator. The manufacture and properties of some currently available near-isotropic and isotropic grades are described. The major features of a graphite moderated reactors are briefly outlined. Displacement damage and the induced structural and dimensional changes in graphite are described. Recent characterization work on nano-carbons and oriented pyrolytic graphites that have shed new light on graphite defect structures are reviewed, and the effect of irradiation temperature on the defect structures is highlighted. Changes in the physical properties of nuclear graphite caused by neutron irradiation are reported. Finally, the importance of irradiation induced creep is presented, along with current models and their deficiencies.

Campbell, Anne↗

DOE OSTI2020

The transformation of diamond to graphite: Experiments reveal the presence of an intermediate linear carbon phase

Natural diamonds that have been partially replaced by graphite have been observed to occur in natural rocks. While the graphite-to-diamond phase transition has been extensively studied the opposite of this (diamond to graphite) remains poorly understood. We performed high-pressure and temperature hydrous and anhydrous experiments up to 1.0 GPa and 1300 °C using Amplex premium virgin synthetic diamonds (20–40 μm size) as the starting material mixed with Mg(OH) 2 as a source of H 2 O for the hydrous experiments. The experiments revealed that the diamond-to-graphite transformation at P = 1.0 GPa and T = 1300 °C was triggered by the presence of H 2 O and was accomplished through a three-stage process. Stage 1: diamond reacts with a supercritical H 2 O producing an intermediate 200–500 nm size “globular carbon” phase. This phase is a linear carbon chain; i.e. a polyyne or carbyne. Stage 2: the linear carbon chains are unstable and highly reactive, and they decompose by zigzagging and cross-linking to form sp 2 -hybridized structures. Stage 3: normal, disordered, and onion-like graphite is produced by the decomposition of the sp-hybridized carbon chains which are re-organized into sp 2 bonds. Our experiments show that there is no direct transformation from sp 3 C-bonds into sp 2 C-bonds. Our hydrous high-pressure and high-temperature experiments show that the diamond-to-graphite transformation requires an intermediate metastable phase of a linear hydrocarbon. This process also provides a simple mechanism for the substitution of other elements into the graphite structure (e.g. H, S, O).

36 MATERIALS SCIENCE↗

NASA NTRS1982

Graphite-Fiber-Reinforced Glass-Matrix Composite

G/GI structural composite material made of graphite fibers embedded in borosilicate glass exhibit excellent strength, fracture toughness, and dimensional stability at elevated temperatures. It is made by passing graphite-fiber yarn through slurry containing suspension of fine glass particles in carrier liquid and winding on drum to produce prepegged uniaxial tape. After drying, tapes are cut into appropriate lengths and laid up in graphite die in desired stacking scheme. Stack is consolidated by hot pressing in furnace.

Prewo, K. M.↗

NASA NTRS1990

Method of fabricating composite structures

A method of fabricating structures formed from composite materials by positioning the structure about a high coefficient of thermal expansion material, wrapping a graphite fiber overwrap about the structure, and thereafter heating the assembly to expand the high coefficient of thermal expansion material to forcibly compress the composite structure against the restraint provided by the graphite overwrap. The high coefficient of thermal expansion material is disposed about a mandrel with a release system therebetween, and with a release system between the material having the high coefficient of thermal expansion and the composite material, and between the graphite fibers and the composite structure. The heating may occur by inducing heat into the assembly by a magnetic field created by coils disposed about the assembly through which alternating current flows. The method permits structures to be formed without the use of an autoclave.

Sigur, W. A.↗

NASA NTRS1992

Method of fabricating composite structures

Sigur, Wanda A.↗

DOE OSTI2021

Comparison of water nanodroplet properties on different graphite-based substrates

The molecular structure and dynamics of water differ considerably at various interfaces. We compare the interfacial water structure–property relationship on three different carbon substrates, namely, amorphous carbon, compressed expanded natural graphite, and pure graphite by utilizing atomistic molecular dynamics simulations. The effect of different substrates on the structural and dynamical properties of water can readily be observed. Here, the density distributions parallel and normal to the substrates show oblate droplet structures. The normal to the substrate water distribution shows a strong hydration layer at the interface that does not vary with substrates. However, the disparity in the structure and dynamics on three different substrates shows that the surface morphologies of the substrates are critical for determining nanoscale water properties. Furthermore, it is observed that the formation of an interfacial water layer or the hydration layer is a direct consequence of both water “confinement” at the nanoscale and “attraction” between water molecules and the carbon substrates.

42 ENGINEERING↗

NASA NTRS1980

Damage tolerance research on composite compression panels

The damage tolerance of composites was investigated. Results show that severe degradation in material strength may occur due to impact damage and that reduced strain allowables should be considered to compensate for possible impact damage. The mechanisms of failure involved in impact so that local damage will be reduced and arrest of propagating fracture initiated at impact locations are examined. Compression strength reductions for damage due to impact by a 1.27 cm diameter spherical projectile in thick laminates representative of wing skin panels are presented. Also discussed are the results of concepts recently evaluated to improve damage tolerance. These concepts range from improvements at the materials level to advanced structural configurations designed to arrest or limit the growth of propagating fractures. The results indicate that substantial improvements in the damage tolerance of graphite-epoxy composite structures can be achieved through the proper combination of materials and structural design.

Rhodes, M. D.↗

NASA NTRS1992

Application of fiber-reinforced bismaleimide materials to aircraft nacelle structures

Existing aircraft engine nacelle structures employ advanced composite materials to reduce weight and thereby increase overall performance. Use of advanced composite materials on existing aircraft nacelle structures includes fiber-reinforced epoxy structures and has typically been limited to regions furthest away from the hot engine core. Portions of the nacelle structure that are closer to the engine require materials with a higher temperature capability. In these portions, existing nacelle structures employ aluminum sandwich construction and skin/stringer construction. The aluminum structure is composed of many detail parts and assemblies and is usually protected by some form of ablative, insulator, or metallic thermal shield. A one-piece composite inner cowl for a new-generation engine nacelle structure has been designed using fiber-reinforced bismaleimide (BMI) materials and honeycomb core in a sandwich construction. The new composite design has many advantages over the existing aluminum structure. Multiple details were integrated into the one-piece composite design, thereby significantly reducing the number of detail parts and fasteners. The use of lightweight materials and the reduction of the number of joints result in a significant weight reduction over the aluminum design; manufacturing labor and the overall number of tools required have also been reduced. Several significant technical issues were addressed in the development of a BMI composite design. Technical evaluation of the available BMI systems led to the selection of a toughened BMI material which was resistant to microcracking under thermal cyclic loading and enhanced the damage tolerance of the structure. Technical evaluation of the degradation of BMI materials in contact with aluminum and other metals validated methods for isolation of the various materials. Graphite-reinforced BMI in contact with aluminum and some steels was found to degrade in salt spray testing. Isolation techniques such as those used for graphite-reinforced epoxy structures were shown to provide adequate protection. The springback and producibility of large BMI structures were evaluated by manufacturing prototype hardware which had the full-scale cross section of the one-piece composite structure.

Peros, Vasilios↗

DOE OSTI2024

Update on Activities Related to the Library of Graphite Microstructures

This report provides an overview and update of the ongoing efforts to create a comprehensive library of microstructures for nuclear graphite and carbon-based materials under consideration for nuclear applications. The library includes data on microstructural characterization of unirradiated graphite materials, a guide to the techniques used to analyze graphite (which complements the ASME guidelines and ASTM standards), a summary of characterization data for neutron-irradiated or oxidized material, and a compendium of microstructural information for carbon-based materials. These efforts are being conducted at various length scales for the filler and binder phases in graphite to better understand graphite’s local structure and property relationships. This report is a follow-up to the previous milestone report titled Report on initial development of a database of nuclear graphite characteristics based on microstructural characterization, ORNL/TM/-2023/2992, published in July 2023.The effort to develop the library of microstructures supports the US Department of Energy Office of Advanced Reactor Technologies program objectives of aiding the material selection, licensing, management, and core assessments of a graphite core by documenting the unirradiated microstructure of relevant grades or characterizing the microstructure’s evolution under the reactor environment. Additionally, this project aims to provide (1) information and guidelines for the characterizing of graphite and (2) a protocol to assess a nuclear graphite grade.

36 MATERIALS SCIENCE↗

NASA NTRS1991

Cost-efficient manufacturing of composite structures

The Advanced Composites Technology (ACT) program is seeking research breakthroughs that will allow structures made of graphite epoxy materials to replace metals in the wings and fuselages of future aircrafts. NASA's goals are to reduce acquisition cost by 20 to 25 percent, structural weight for a resized aircraft by 40 to 50 percent, and the number of parts by half compared to current production aluminum aircraft. The innovative structural concepts, materials, and fabrication techniques emerging from the ACT program are described, and the relationship between aerospace developments and industrial, commercial, and sporting goods applications are discussed.

Freeman, W. Tom↗