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At least 19 records

Dielectric relaxation and hopping conduction in reduced graphite oxide

Graphite oxide reduced by sodium borohydride was characterised and its electrical conduction investigated with impedance spectroscopy. Thermal dependence of electrical modulus (instead of permittivity, its inverse) was calculated from complex impedance spectra, an approach that prevents any peak in dielectric loss (imaginary component) from being swarmed by large dc conductivity. Two loss peaks appeared at each tested frequency, in a sample of either degree of reduction. The set of weaker peak should arise from the relaxation of some polar bonds, as proposed earlier by us. The stronger loss peaks may correspond to the hopping of conduction electrons; variable range hopping is also consistent with the observed thermal dependence of conductivity. However, nearer ambient temperature there is a change in mechanism, to band transport, with an activation energy of fairly similar values as derived from both loss peaks and conductivity.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Graphene prepared by thermal reduction–exfoliation of graphite oxide: Effect of raw graphite particle size on the properties of graphite oxide and graphene

Highlights: • Effect of raw graphite particle size on properties of GO and graphene is reported. • Size of raw graphite affects oxidation degree and chemical structure of GO. • Highly oxidized GO results in small-sized but well-exfoliated graphene. • GO properties affect reduction degree, structure, and conductivity of graphene. - Abstract: We report the effect of raw graphite size on the properties of graphite oxide and graphene prepared by thermal reduction–exfoliation of graphite oxide. Transmission electron microscope analysis shows that the lateral size of graphene becomes smaller when smaller size graphite is used. X-ray diffraction analysis confirms that graphite with smaller size is more effectively oxidized, resulting in a more effective subsequent exfoliation of the obtained graphite oxide toward graphene. X-ray photoelectron spectroscopy demonstrates that reduction of the graphite oxide derived from smaller size graphite into graphene is more efficient. However, Raman analysis suggests that the average size of the in-plane sp{sup 2}-carbon domains on graphene is smaller when smaller size graphite is used. The enhanced reduction degree and the reduced size of sp{sup 2}-carbon domains contribute contradictively to the electrical conductivity of graphene when the particle size of raw graphite reduces.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Graphite Oxidation Studies Irradiated Graphite, GIF Summary, ASME Task Force, ASTM Activities

Introduction Comparison of Graphite Oxidation Rates for Irradiated and Unirradiated NBG-25 (Rebecca Smith and Austin Matthews, INL) Annealing effect over range of oxidation temperatures Irradiation effect (~6.5 dpa) over range of oxidation temperatures Dose dependency of irradiation effect Generation IV International Forum High Level Deliverable Summary of DOE ART Historic Oxidation Research (Cristian Contescu, ORNL) Publications issued over the last ~10 years Acute and chronic oxidation ASME Graphite Oxidation Task Force (C. Contescu, Paul Ryan, ORNL, Joe Bass, A. Matthews, R. Smith, INL) Collaborative effort headed by ORNL and engaging INL and others Initial review of relevant oxidation discussion in ASME code ASTM Activities (C. Contescu) Virtual Meetings New and Revised Standards

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Purification and preparation of graphite oxide from natural graphite

Graphite oxide has attracted much interest as a possible route for preparation of natural graphite in the large-scale production and manipulation of graphene as a material with extraordinary electronic properties. Graphite oxide was prepared by modified Hummers method from purified natural graphite sample from West Kalimantan. We demonstrated that natural graphite is well-purified by acid leaching method. The purified graphite was proceed for intercalating process by modifying Hummers method. The modification is on the reaction time and temperature of the intercalation process. The materials used in the intercalating process are H{sub 2}SO{sub 4} and KMNO{sub 4}. The purified natural graphite is analyzed by carbon content based on Loss on Ignition test. The thermo gravimetricanalysis and the Fouriertransform infrared spectroscopy are performed to investigate the oxidation results of the obtained GO which is indicated by the existence of functional groups. In addition, the X-ray diffraction and energy dispersive X-ray spectroscopy are also applied to characterize respectively for the crystal structure and elemental analysis. The results confirmed that natural graphite samples with 68% carbon content was purified into 97.68 % carbon content. While the intercalation process formed a formation of functional groups in the obtained GO. The results show that the temperature and reaction times have improved the efficiency of the oxidation process. It is concluded that these method could be considered as an important route for large-scale production of graphene.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Graphite Oxidation Behavior: NRC Graphite Behavior Model

Graphite microstructure and oxidation Graphite crystal structure and basal planes Reactive surface area sites Zig-zag and Arm-chair Pore microstructure effects Interconnectivity Reactivity and oxygen transport Oxygen-graphitereaction Not C-O reaction! Temperature effects Oxygen diffusion to graphite Diffusion into the microstructure High temperature vs low temperature diffusion Oxidation: It’s a gradient of factors

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Graphite Oxidation Activities

Graphite Oxidation Activities to include introduction, rate determination, strength after oxidation, penetration depth analysis, strategic partnership projects, and summary and continuing work.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Thermally exfoliated graphite oxide

A modified graphite oxide material contains a thermally exfoliated graphite oxide with a surface area of from about 300 sq m/g to 2600 sq m/g, wherein the thermally exfoliated graphite oxide displays no signature of the original graphite and/or graphite oxide, as determined by X-ray diffraction.

Prud'Homme, Robert K.↗

Bridged graphite oxide materials

Bridged graphite oxide material comprising graphite sheets bridged by at least one diamine bridging group. The bridged graphite oxide material may be incorporated in polymer composites or used in adsorption media.

Herrera-Alonso, Margarita↗

Graphite Oxidation Rate Study on ET-10 and ETU-10 Grades - Task 4: QA Support and Testing for Structural Graphite Oxidation

INL performed targeted oxidation tests to measure oxidation rates for samples of ET-10 and ETU-10 graphite under CRADA No. 21CRA22 Mod. 3, Annex A, “Tritium Testing to Support Kairos Power Advanced Reactor Demonstration” (04/02/2024). All testing was conducted within INL’s Carbon Characterization Laboratory (CCL) using test standard ASTM D7542-21 "Standard Test Method for Air Oxidation of Carbon and Graphite in the Kinetic Regime" [ASTM International, 2021]. Kairos Power provided all test specimens through its graphite vendor Ibiden, Inc. to INL and ASTM specimen specified dimensions. Information within this report only provides the Arrhenius oxidation rate plots as a function of temperature for each graphite grade tested. The raw mass loss per time data will be provided on the Nuclear Data Management and Analysis System (NDMAS) portal located on the INL information system.

36 MATERIALS SCIENCE↗

Anomalous dielectric relaxation of water confined in graphite oxide

Nonmonotonic thermal dependence of dielectric relaxation of water has been observed in hydrated graphite oxide (GO). Graphite oxide prepared via Hummers method then imbued with specific water contents were characterized, with {sup 13}C and {sup 1}H nuclear magnetic resonance spectroscopies, X-ray photoelectron spectroscopy, ambient- and variable-temperature X-ray diffractometries, as well as thermogravimetric analysis. Pressed pellets provided with either conducting or blocking electrodes yielded dielectric loss, which was shown to originate from dielectric relaxation of the confined water. Three relaxation processes were observed in impedance spectroscopy. Our previous work has identified two different types of water in GO, namely, intercalated water and water in inter-grain voids. P{sub 1} expresses the reorientation of water confined inside inter-grain voids, and P{sub 2}, the rotation of intercalated water molecules confined in interlayers. The present work reveals a new process P{sub 3}, which also relates to intercalated water. It slows down with temperature, and this apparent anomaly is explained by the decrease in water content and consequent narrowing of interlayer spacing in graphite oxide, as confirmed by characterization techniques. The present study should contribute to our understanding of surface water dynamics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Elemental Metals or Oxides Distributed on a Carbon Substrate or Self-Supported and the Manufacturing Process Using Graphite Oxide as Template

A process for providing elemental metals or metal oxides distributed on a carbon substrate or self-supported utilizing graphite oxide as a precursor. The graphite oxide is exposed to one or more metal chlorides to form an intermediary product comprising carbon, metal, chloride, and oxygen. This intermediary product can be further processed by direct exposure to carbonate-solutions to form a second intermediary product comprising carbon, metal carbonate, and oxygen. Either intermediary product may be further processed: a) in air to produce metal oxide; b) in an inert environment to produce metal oxide on carbon substrate; c) in a reducing environment to produce elemental metal distributed on carbon substrate. The product generally takes the shape of the carbon precursor.

Hung, Ching-Cheh↗

Elemental Metals or Oxides Distributed on a Carbon Substrate or Self-Supported and the Manufacturing Process Using Graphite Oxide as Template

A process for providing elemental metals or metal oxides distributed on a carbon substrate or self-supported utilizing graphite oxide as a percursor. The graphite oxide is exposed to one or more metal chlorides to form an intermediary product comprising carbon, metal, chloride, and oxygen. This intermediary product can be further processed by direct exposure to carbonate solutions to form a second intermediary product comprising carbon, metal carbonate, and oxygen. Either intermediary product may be further processed: a) in air to produce metal oxide; b) in an inert environment to produce metal oxide on carbon substrate; c) in a reducing environment to produce elemental metal distributed on carbon substrate. The product generally takes the shape of the carbon precursor.

Hung, Ching-Chen↗

Separation medium containing thermally exfoliated graphite oxide

A separation medium, such as a chromatography filling or packing, containing a modified graphite oxide material, which is a thermally exfoliated graphite oxide with a surface area of from about 300 m.sup.2/g to 2600 m.sup.2/g, wherein the thermally exfoliated graphite oxide has a surface that has been at least partially functionalized.

Prud'homme, Robert K.↗

Multiphysics Simulation of Moisture-Graphite Oxidation in MHTGR

A small amount of moisture on the ppm level could present in the primary helium coolant under normal operations of High-Temperature Gas-cooled Reactors (HTGRs). One potential safety issue related to HTGRs is the chronic moisture-graphite oxidation, which could affect the integrity of the fuel blocks and reflectors in the reactor core, and the support columns in the hot plenum. However, it is infeasible to perform chronic moisture-graphite oxidation tests under the prototypic high-pressure, high-temperature conditions over a long period of time that is comparable to the full service time, i.e., 36 months for Modular High Temperature Gas-cooled Reactor (MHTGR). As an alternate, accelerated moisture-graphite oxidation tests at the atmospheric pressure and high moisture concentrations have been performed in the literature. Through these accelerated tests, global reaction rate equations have been proposed, which makes it possible to study the moisture-graphite oxidation numerically. This paper is aimed to establish a multiphysics model that can evaluate the moisture-graphite oxidation under MHTGR normal operation conditions. COMSOL Multiphysics was applied to couple the fluid flow, heat and mass transfer, chemical reaction and material structural changes. To reduce the calculation time, the prototypic three-dimensional (3-D) structures were simplified into a two-dimensional (2-D) simulation domain. The performance of four nuclear grades of graphite (IG-110, 2114, PCEA, and NBG-17) over a 36-month service period was then investigated under the most likely prototypic conditions of MHTGR. The simulation results indicate that most oxidation occurs in the three or four bottom fuel blocks due to their higher temperatures. In general, however, only a thin layer of 1 mm into the graphite will be considerably oxidized even for those three or four bottom fuel blocks.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗