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Slides for Oxidation Activities, oxidation rate, penetration/lathing, and strength after oxidation work. Also includes recent and current oxidation studies, background for rate behavior, strength behavior, density profile, and penetration measurements, oxidation resistant graphite coating development, and irradiated and unirradiated graphite oxidation rate behavior.
Effusion steady state pressures time dependence of carbon monoxide and calcium vapors generated during calcium oxide-graphite interaction
A method of preventing oxidation of graphite fireproof material is given. A blend of 1 to 33 weight parts alumina and 3 to 19 parts of K2O + Na2O in 100 parts of SiO2 is pulverized followed by addition of 5 to 160 parts of silicon carbide powder in 100 parts of the mixture. This is thoroughly blended and coated on the surface of graphite fireproof material.
This NEUP project #15-8205 entitled “Experimental Investigation of Forced Convection and Natural Circulation Cooling of a VHTR Core under Normal Operation and Accident Scenarios”, has investigated important phenomena in the safety of Very High Temperature Reactors (VHTRs) using the experimental facilities at City College of New York (CCNY) and Kansas State University (KSU), in collaboration with the Idaho State University (ISU) and Idaho National Laboratory (INL). The main objectives of this project were to investigate the forced convection and bypass flow phenomena, natural circulation flow and heat transfer, and graphite oxidation due to air ingress which could occur in a Very High Temperature Reactor (VHTR) with a prismatic core. High pressure/high temperature experiments have been conducted to obtain data that could be used for validation of VHTR design and safety analysis codes. The focus of these experiments was on the generation of benchmark data for design and off-design heat transfer for forced and natural circulation in a VHTR core. This work has built on the previous NEUP project #11-3218 which investigated forced convection and flow laminarization phenomena in a prismatic core of a VHTR and natural circulation of a pure gas under Pressurized Conduction Cooldown (PCC) and Depressurized Conduction Cooldown (DCC) conditions. Under each Task, extensive literature reviews on natural circulation, bypass flow, air ingress and graphite oxidation phenomena were conducted. In Task 1, scaling analyses were conducted by Idaho State University followed by design and construction of experimental facilities needed to conduct both bypass flow and natural circulation experiments at CCNY. Natural circulation experiments were conducted in Task 2 to investigate the air ingress phenomena, and bypass flow phenomena in Task 3, both at CCNY. In Task 4, radiation heat transfer and graphite oxidation tests were performed at Kansas State University. The experimental data were then analyzed to obtain quantitative results on natural circulation of pure gases and gas mixtures under DCC conditions, bypass flow rates, radiation heat transfer and graphite oxidation. In addition, CFD and Direct Numerical Simulations were conducted by INL and CCNY to investigate the flow laminarization phenomenon in strongly heated gas flows. The scaling analyses have shown that the key nondimensional numbers and parameters all have acceptable distortion levels principally because the CCNY facility’s test sections have representative cooling channel dimensions and are using either helium or a scalable gas such as nitrogen at representative state conditions. The natural circulation experiments involving helium and nitrogen gas mixtures at CCNY have elucidated the effect of nitrogen (simulating air) ingress into a lower plenum on the onset of natural circulation, mass flow rates and heat transfer coefficients under different power input levels in the riser section. Also, the transport of nitrogen from the lower plenum to upper plenum due to natural circulation was quantified for the first time. Nusselt number correlations for the heat transfer coefficient under natural circulation as a function of Reynolds and Prandtl numbers was also developed. The experiments at KSU revealed that prior to the onset of natural circulationin a VHTR core. This work has built on the previous NEUP project #11-3218 which investigated forced convection and flow laminarization phenomena in a prismatic core of a VHTR and natural circulation of a pure gas under Pressurized Conduction Cooldown (PCC) and Depressurized Conduction Cooldown (DCC) conditions. Under each Task, extensive literature reviews on natural circulation, bypass flow, air ingress and graphite oxidation phenomena were conducted. In Task 1, scaling analyses were conducted by Idaho State University followed by design and construction of experimental facilities needed to conduct both bypass flow and natural circulation experiments at CCNY. Natural circulation experiments were conducted in Task 2 to investigate the air ingress phenomena, and bypass flow phenomena in Task 3, both at CCNY. In Task 4, radiation heat transfer and graphite oxidation tests were performed at Kansas State University. The experimental data were then analyzed to obtain quantitative results on natural circulation of pure gases and gas mixtures under DCC conditions, bypass flow rates, radiation heat transfer and graphite oxidation. In addition, CFD and Direct Numerical Simulations were conducted by INL and CCNY to investigate the flow laminarization phenomenon in strongly heated gas flows. The scaling analyses have shown that the key nondimensional numbers and parameters all have acceptable distortion levels principally because the CCNY facility’s test sections have representative cooling channel dimensions and are using either helium or a scalable gas such as nitrogen at representative state conditions.The natural circulation experiments involving helium and nitrogen gas mixtures at CCNY have elucidated the effect of nitrogen (simulating air) ingress into a lower plenum on the onset of natural circulation, mass flow rates and heat transfer coefficients under different power input levels in the riser section. Also, the transport of nitrogen from the lower plenum to upper plenum due to natural circulation was quantified for the first time. Nusselt number correlations for the heat transfer coefficient under natural circulation as a function of Reynolds and Prandtl numbers was also developed. The experiments at KSU revealed that prior to the onset of natural circulation(ONC), molecular diffusion plays a significant role in air-ingress, however, at higher temperatures convection currents may be influencing air ingress and in-turn ONC times. Bypass flow experiments faced difficulties in the measurement of gas velocity in the main channel due to the failure of a high temperature Hot Wire Anemometer probe, so an energy balance method was instead employed to estimate the flow distribution between the main and bypass flow channels. In the graphite oxidation experiments conducted at KSU, oxidation was found to increase the thermal diffusivity of nuclear grade graphite. This change is believed to be driven by oxidation decreasing graphite sample density rather than raising the thermal conductivity. Oxidation was also shown to greatly alter graphite emissivity. If large amounts of impurities have built up within the graphite over time and have significantly increased its effective ash content, then air ingress is likely to severely inhibit the radiative heat transfer abilities of the graphite due to the formation of low emissivity, ash layers on its surface. However, if the purity of the graphite at the time of the air ingress is still close to that of its virgin specifications, the oxidation induced roughening of the graphite’s outer surface would have the effect of slightly raising its emissivity. The flow laminarization phenomenon was investigated by INL by examining the results of Direct Numerical Simulations of previous experiments, and by CCNY conducting its own DNS simulations using DOE’s Nek5000 code
Thermal oxidation of nuclear graphite components is highly undesirable because it can cause structural and property degradation that negatively affect a reactor's intended operation. In this work, the body of knowledge of nuclear graphite oxidation is highlighted, including when O 2 , H 2 O, and/or CO 2 are the oxidant. Oxidation conditions relevant to high-temperature gas-cooled reactors (i.e., when oxidation could occur either as an acute or chronic phenomenon) are emphasized. Here, the objective is to summarize graphite oxidation data in a practical and accessible way to inform future research and regulatory requirements. Although each grade of nuclear graphite is different, the oxidation mechanism has underlying commonalities. Although oxidation behavior is grade dependent, the general temperature dependence is well described by a sequence of elementary steps which become rate limiting. Because the regime transition temperature depends on sample microstructure, size, and oxidant supply rate, extrapolating results beyond the experimental range should be done cautiously. Gravimetric oxidation rate measurements generally replicate well. However, caution must be exercised when rates are estimated by other methods or for samples that deviate significantly in size. Air oxidation data for IG-110, NBG-18, and PCEA graphite is critically reviewed to emphasize this point. Despite the amount of experimental data, gaps remain. Sample size and shape effects are not fully explained. Data on the oxidant penetration depth are insufficient. Analytical assessments demonstrate that lower temperature oxidation does not necessarily imply that oxidation is uniform throughout the bulk. Oxidation occurs faster at higher temperature but is more localized to the exposed surface. Paradoxically, at equal mass loss percentage, low temperature oxidation leads to greater property degradation than at high temperature. The isolated effect of oxidation is important; however, a gap remains in the systematic understanding of any potential effect of neutron irradiation on graphite structure and reactivity.
Torsion effusion method for studying reaction of graphite with thorium and zirconium oxides, discussing thermodynamic properties of thorium carbide
For chemisorption and oxidation on Pt/HOPG (highly-orientated pyrolytic) graphite, reflectance Fourier Transform Infrared (FTIR)-microspectrometry reveals a variable state and reactivity for CO. Even for model surface science systems, where surface heterogeneity is minimal, surface diffusion may be too slow relative to the reaction rate to avoid segregation of reactants into surface islands under steady-state conditions. Thus in CO oxidation on Pt (where the relevant surface diffusion coefficients are such that D sub O less than D sub CO) then reactant CO islands exists at the perimeters of which the surface reaction is thought to occur. Furthermore CO can chemisorb on metals in linear and bridge forms to extents which vary with precise faces predominantly exposed coverage, etc. Infrared has long been used to probe the nature of adsorbed CO on model film and heterogeneous surfaces, but it may now be that FTIR-microspectrometry will allow the state of this adsorbate and reactant to be investigated with a spatial resolution of 4.4 microns on model (and real) catalytic surfaces.
Air-ingress following a depressurized loss-of-forced-cooling (DLOFC) event is a challenging, multiphysics safety scenario for High-Temperature Gas-Cooled Reactors (HTGRs), involving coupled gas composition transport, buoyancy-driven flow redistribution, graphite oxidation, and structural heat-up. Despite its importance — air ingress is a key scenario identified in the PIRT process for the HTGRs — existing system-level safety codes have lacked the integrated capability to simulate the complete event sequence with high confidence. This report documents the development, validation, and demonstration of three new capabilities in the SAM code to address this gap: (1) a multi-component gas mixture flow model with binary diffusion to track the helium-air composition and its effect on system density and flow; (2) a 0-D graphite oxidation model based on the Roes correlation, including oxygen consumption and exothermic heat release; and (3) an isentropic critical flow model for accurate representation of primary system depressurization through a break. These capabilities are validated against two benchmark experiments. The NSTF heavy-gas ingress experiment validates the multi-component flow model: SAM correctly reproduces the rapid buoyancydriven flow stagnation and subsequent natural circulation recovery driven by composition-dependent density changes. The NACOK graphite oxidation experiment validates the oxidation model: SAM predicts a bottom-level graphite weight loss of 25%, in close agreement with the measured 24%, and reproduces the strong axial nonuniformity and block-geometry dependence of oxidation, at a level comparable to the SPECTRA and TINTE codes. The validated capabilities are then exercised together in an integrated, reactor-scale simulation of a DLOFC air-ingress transient in a simplified HTR-PM pebble-bed reactor. In a single calculation spanning approximately 8 days, SAM reproduces the complete accident sequence: rapid depressurization, densityand diffusion-driven air ingress over ˜15 hours, onset of buoyancy-driven natural circulation, exothermic graphite oxidation with a peak fuel temperature at ˜62 hours, and eventual passive cooldown. These results demonstrate that SAM now provides the nuclear community with a preliminarily validated, modern systemlevel tool for HTGR air-ingress safety analysis, filling a recognized capability gap. Future extensions to broaden species tracking, improve oxidation chemistry, and refine the reactor model are discussed.
A gas storage cylinder or gas storage cylinder liner, formed from a polymer composite, containing at least one polymer and a modified graphite oxide material, which is a thermally exfoliated graphite oxide with a surface area of from about 300 m(exp 2)/g to 2600 m(exp 2)2/g.
A magnetic sorbent based on exfoliated graphite modified with magnesium ferrite has been prepared by impregnating oxidized graphite in a mixed solution of FeCl{sub 3} and Mg(NO{sub 3}){sub 2}, followed by heat treatment of the impregnated oxidized graphite in air. X-ray diffraction and Mössbauer spectroscopy results demonstrate that the structure of the magnesium ferrite is an inverse spinel with a degree of inversion of 0.59. The saturation magnetization of the magnesium ferrite-containing exfoliated graphite is 16.1 emu/g, whereas its oil sorption capacity is as high as 54 g/g. Compaction of the exfoliated graphite to a density of 0.03 g/cm{sup 3} reduced its sorption capacity to 26 g/g. Further increasing the density of the material led to a considerable decrease in its sorption capacity.
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.
The influence of three fission products Sr, Eu, and I on the oxidation of IG-110 nuclear graphite was studied in the temperature range of 400 to 1000 °C. Sr and Eu were introduced as chlorides, and I was introduced as NaI. The temperature dependence of both CO 2 and CO production during the graphite oxidation measured with mass spectroscopy and infrared spectrometry shows that the introduction of these three compounds to graphite significantly decreases the onset temperature for the oxidation of graphite. Among the three compounds, NaI is the most active towards the oxidation reaction, characterized by a significant decrease of the onset temperature from approximately 650 to 400 °C before and after its introduction to graphite. Separate measurements of CO 2 and CO concentration at varying temperatures enable the calculation of the activation energy for the formation of CO 2 and CO. The activation energies for the oxidation of pure and fission product-impregnated graphite samples decrease in the following order: standard IG-110 graphite, EuCl 3 -impregnated IG-110, SrCl 2 -impregnated IG-110, and NaI-impregnated IG-110. This trend indicates that the three compounds catalyze the oxidation of graphite at temperatures relevant to the operation of high-temperature gas-cooled reactors. Furthermore, it is found that the three compounds can also affect the molar ratio of reaction products CO 2 and CO, and the rates of the graphite oxidation. At temperatures higher than about 850 °C, the impregnated samples exhibit lower CO 2 : CO ratios than the pure graphite. Different from EuCl 3 and NaI, the introduction of SrCl 2 decreases the graphite oxidation rates at temperatures higher than about 770 °C. Their catalytic mechanism can be understood based on a redox cycle of the intermediate active species, promoting the dissociation of molecular oxygen and transfer to the carbon.
In an all-van der Waals heterostructure, the active layer, gate dielectrics and gate electrodes are assembled from two-dimensional crystals that have a low density of atomic defects. This design allows two-dimensional electron systems with very low disorder to be created, particularly in heterostructures where the active layer also has intrinsically low disorder, such as crystalline graphene layers or metal dichalcogenide heterobilayers. A key missing ingredient has been nanoscale electrostatic control, with existing methods for fabricated local gates typically introducing unwanted contamination. Here we describe a resist-free local anodic oxidation process for patterning sub-100 nm features in graphite gates, and their subsequent integration into an all-van der Waals heterostructure. We define a quantum point contact in the fractional quantum Hall regime as a benchmark device and observe signatures of chiral Luttinger liquid behaviour, indicating an absence of extrinsic scattering centres in the vicinity of the point contact. In the integer quantum Hall regime, we demonstrate in situ control of the edge confinement potential, a key requirement for the precision control of chiral edge states. In conclusion, this technique may enable the fabrication of devices capable of single anyon control and coherent edge-state interferometry in the fractional quantum Hall regime.
Doped activated microwave expanded graphite oxide materials and doped monolayer graphene materials, and methods of making these materials. The materials exhibit increased capacitance relative to undoped activated microwave expanded graphite oxide and monolayer graphene. The materials are suitable for use in, for example, ultracapacitors.
Symmetric cells provide complementary means to probe electrochemical processes in lithium-ion batteries. Here, positive and negative electrodes harvested from conventional oxide/graphite cells are cross-paired, and the assembled reference-electrode-bearing symmetric cells are cycled/aged. For graphite symmetric cells, the electrode potentials and impedances remain nearly constant during calendar aging and the parasitic currents are typically small. However, at higher cell voltages when the “positive” graphite potential exceeds 1.0 V vs. Li/Li + , the capacity loss is higher, indicating that even a mild (but prolonged) overdischarge can damage the SEI. For the layered-oxide symmetric cells there are strong parasitic currents and a persistent slide of the electrode potential over time during calendar aging. Significant cell impedance rise, especially at higher hold voltages, is also observed. Curiously, the impedance rise in the “negative” oxide electrode, which experiences potentials below 4.0 V vs. Li/Li + , is greater than in the “positive” oxide electrode that experiences much higher potentials. We postulate that electrolyte oxidation is responsible for the behavior of these oxide symmetric cells, as it supplies electrons (that bind more Li + into the cathode, causing the potential slide) and protons (that contribute to impedance rise). Furthermore, these insights can guide the development of future lithium-ion cell chemistries.
The aim of this research was to fabricate YBa{sub 2}Cu{sub 3}O{sub 7−δ} (YBCO) superconductor composite with graphene oxide nanosheets and to study the effect of the graphene oxide nanosheets on YBCO superconductor properties. For this purpose, the samples of pure superconductor and superconductor composite with 0.001, 0.01, and 0.1 wt.% graphene oxide were synthesized. First, graphite oxide was made by Hummer’s chemical method; after that, graphene oxide nanosheets were produced by bath-keeper ultrasonic. Then, different amounts of graphene oxide were added to the process of superconductor fabrication, which was made by solid-state reaction method. The samples were characterized and studied by Meissner effect test, XRD analysis, FESEM imaging, EDX measurement, and ac magnetic susceptibility. The critical current density (J{sub c}) of samples was measured by four probes method. The results showed that by increasing the weight ratio of graphene oxide, J{sub c} and T{sub c} decrease.
The contributions of individual resin components to total resin weight loss in 600 F air aged Celion 6000/PMR-15 polyimide composites were determined from the overall resin weight loss in the composite by chemically separating the PMR-15 matrix resin into its monomeric components. The individual resin components were also analyzed by spectroscopic techniques in order to elucidate curing and degradation mechanisms of the PMR-15 matrix resin. The isothermal weight loss of the individual resin components during prolonged 600 F thermo-oxidative aging of the composite was correlated to the changes observed in the Fourier Transform infrared spectra and Fourier Transform nuclear magnetic resonance spectra of the individual resin components. The correlation was used to identify the molecular site of the thermo-oxidative changes in PMR-15 polyimide matrix resin during 600 F curing the prolonged 600 F thermo-oxidative aging.
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