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A brief overview of current and planned applications of graphite/polyimide composites is presented. A short discussion of technical problems delaying the application of graphite polyimide composites in aerospace structures and near-term solutions to these problems are also included.
The Nobel Prize winning discovery of the Buckuball (C60) in 1985 at Rice University by a group including Dr. Richard Smalley led to the whole new class of carbon allotropes including fullerenes and nanotubes. Especially interesting from many viewpoints are single-walled carbon nanotubes, which structurally are like a single graphitic sheet wrapped around a cylinder and capped at the ends. This cylinders have diameter as small as 0.5 - 2 nm (1/100,000th the diameter of a human hair) and are as long as 0.1 - 1 mm. Nanotubes are really individual molecules and believed to be defect-free, leading to high tensile strength despite their low density. Additionally, these fibers exhibit electrical conductivity as high as copper, thermal conductivity as high as diamond, strength 100 times higher than steel at one-sixth the weight, and high strain to failure. Thus it is believed that developments in the field of nanotechnology will lead to stronger and lighter composite materials for next generation spacecraft. Lack of a bulk method of production is the primary reason nanotubes are not used widely today. Toward this goal JSC nanotube team is exploring three distinct production techniques: laser ablation, arc discharge and chemical vapor deposition (CVD, in collaboration with Rice University). In laser ablation technique high-power laser impinges on the piece of carbon containing small amount of catalyst, and nanotubes self-assemble from the resulting carbon vapor. In arc generator similar vapor is created in arc discharge between carbon electrodes with catalyst. In CVD method nanotubes grow at much lower temperature on small catalyst particles from carbon-containing feedstock gas (methane or carbon monoxide). As of now, laser ablation produces cleanest material, but mass yield is rather small. Arc discharge produces grams of material, but purity is low. CVD technique is still in baby steps, but preliminary results look promising, as well as perspective of scaling the process up. We are also working on necessary purification of nanotubes. Applications of nanotubes are in such various fields as lightweight composites, molecular electronics, energy storage (electrodes in Li ion batteries), flat panel displays, conductive polymers, etc. JSC nanotube team is focused on development of lightweight materials. We work on the injection thermoset epoxies reinforced with nanotubes. Early results show good wetting of nanotube surface with epoxy, which is very important. More research will be possible as more nanotubes become available.
Nanomaterials are part of an industrial revolution to develop lightweight but strong materials for a variety of purposes. Single-wall carbon nanotubes are an important member of this class of materials. They structurally resemble rolled-up graphite sheets, usually with one end capped; individually they are about 1 nm in diameter and several microns long, but they often pack tightly together to form rods or ropes of microscopic sizes. Carbon nanotubes possess unique electrical, mechanical, and thermal properties and have many potential applications in the electronics, computer, and aerospace industries. Unprocessed nanotubes are very light and could become airborne and potentially reach the lungs. Because the toxicity of nanotubes in the lung is not known, their pulmonary toxicity was investigated. The three products studied were made by different methods and contained different types and amounts of residual catalytic metals. Mice were intratracheally instilled with 0, 0.1, or 0.5 mg of carbon nanotubes, a carbon black negative control, or a quartz positive control and euthanized 7 d or 90 d after the single treatment for histopathological study of the lungs. All nanotube products induced dose-dependent epithelioid granulomas and, in some cases, interstitial inflammation in the animals of the 7-d groups. These lesions persisted and were more pronounced in the 90-d groups; the lungs of some animals also revealed peribronchial inflammation and necrosis that had extended into the alveolar septa. The lungs of mice treated with carbon black were normal, whereas those treated with high-dose quartz revealed mild to moderate inflammation. These results show that, for the test conditions described here and on an equal-weight basis, if carbon nanotubes reach the lungs, they are much more toxic than carbon black and can be more toxic than quartz, which is considered a serious occupational health hazard in chronic inhalation exposures.
The reprocessing of HTGR spent fuels is in favor of the sustainable development of nuclear energy to realize the maximal use of nuclear resource and the minimum disposal of nuclear waste. The head-end of HTGR spent fuels reprocessing is different from that of the LWR spent fuels reprocessing because of the difference of spent fuel structure. The dismantling of the graphite spent fuel element and the highly effective dissolution of fuel kernel is the most difficult process in the head end of the reprocessing. Recently, some work on the head-end has been done in China. First, the electrochemical method with nitrate salt as electrolyte was studied to disintegrate the graphite matrix from HTGR fuel elements and release the coated fuel particles, to provide an option for the head-end technology of reprocessing. The results show that the graphite matrix can be effectively separated from the coated particle without any damage to the SiC layer. Secondly, the microwave-assisted heating was applied to dissolve the UO{sub 2} kernel from the crashed coated fuel particles. The ceramic UO{sub 2} as the solute has a good ability to absorb the microwave energy. The results of UO{sub 2} kernel dissolution from crushed coated particles by microwave heating show that the total dissolution percentage of UO{sub 2} is more than 99.99% after 3 times cross-flow dissolution with the following parameters: 8 mol/L HNO{sub 3}, temperature 100 Celsius degrees, initial ratio of solid to liquid 1.2 g/ml. (authors)
10B isotope doped p-type diamond epilayer grown by chemical vapor deposition on (110) oriented type IIa diamond single crystal substrate was subjected to neutron transmutation at a fluence of 2.4 9 1020 thermal and 2.4 9 1020 fast neutrons. After neutron irradiation, the epilayer and the diamond substrate were laser annealed using Nd YAG laser irradiation with wave length, 266 nm and energy, 150 mJ per pulse. The neutron irradiated diamond epilayer and the substrate were characterized before and after laser annealing using different techniques. The characterization techniques include optical microscopy, secondary ion mass spectrometry, X-ray diffraction, Raman, photoluminescence and Fourier Transform Infrared spectroscopy, and electrical sheet conductance measurement. The results indicate that the structure of the irradiation induced amorphous epilayer changes to disordered graphite upon laser annealing. The irradiated substrate retains the (110) crystalline structure with neutron irradiation induced defects.
Four grades of nuclear graphite with various microstructures were subjected to accelerated oxidation tests in helium with traces of moisture and hydrogen in order to evaluate the effects of chronic oxidation on graphite components in high temperature gas cooled reactors. Kinetic analysis showed that the Langmuir-Hinshelwood (LH) model cannot consistently reproduce all results. In particular, at high temperatures and water partial pressures oxidation was always faster than the LH model predicts, with stronger deviations for superfine grain graphite than for medium grain grades. It was also found empirically that the apparent reaction order for water has a sigmoid-type variation with temperature which follows the integral Boltzmann distribution function. This suggests that the apparent activation with temperature of graphite reactive sites that causes deviations from the LH model is rooted in specific structural and electronic properties of surface sites on graphite. A semi-global kinetic model was proposed, whereby the classical LH model was modified with a temperature-dependent reaction order for water. The new Boltzmann-enhanced model (BLH) was shown to consistently predict experimental oxidation rates over large ranges of temperature (800-1100 oC) and partial pressures of water (3-1200 Pa) and hydrogen (0-300 Pa), not only for the four grades of graphite but also for the historic grade H-451. The BLH model offers as more reliable input for modeling the chemical environment effects during the life-time operation of new grades of graphite in advanced nuclear reactors operating at high and very high temperatures.
Microreactors have great potential to decrease capital costs and construction timelines, reducing the barriers to implementing advanced nuclear reactor technologies. However, the lower power output of these microreactors introduces economic challenges if the operation and maintenance costs cannot be reduced sufficiently. Many microreactor concepts use graphite materials for in-core moderator and structural purposes, which will require periodic inspection or, ideally, in situ structural health monitoring. This work describes an initial evaluation of the feasibility of leveraging graphite’s semiconducting properties to perform electrical impedance tomography (EIT) for defect localization. First, a study was performed to identify the best methods for bonding electrical contacts to minimize the effects of contact resistance that interfere with impedance measurements of the graphite. After determining the best bonding approach, electrodes were attached to multiple graphite components with varying geometries (e.g., simple block and more representative microreactor hexagonal block). In parallel, finite element analysis approaches were developed and implemented to analyze the impact of defects and contact resistances and to inform an iterative inverse model for reconstructing the conductivity distribution. The results of this study show that defect localization in graphite components is possible using EIT if a sufficient number of electrodes (to improve spatial resolution) can be bonded using a technique with very low contact resistance and those contact resistances remain stable during reactor operation. If the reactor core and vessel design do not allow electrodes to be bonded during reactor operation, then it may be possible to detach/reattach electrodes between reactor operation and outages if a suitable mechanical connection that offers repeatable contact resistance can be identified. Alternatively, future work could focus on identifying contacts that can survive the harsh reactor operating environment so that contacts do not need to be removed.
Spiral Notch Torsion Test (SNTT) was developed recently to measure the intrinsic fracture toughness (KIC) of structural materials. The SNTT system operates by applying pure torsion to uniform cylindrical specimens with a notch line that spirals around the specimen at a 45 pitch. The KIC values and the associated energy release rate are obtained with the aid of a three-dimensional finite-element evaluation. The SNTT method is uniquely suitable for testing a wide variety of structural materials, including others such as ceramics, graphite, concrete, polymeric composites, and for bi-material interface fracture toughness evaluation. The SNTT test results for these structural materials and polymeric composite are demonstrated in this paper. These results demonstrated that SNTT has great potential in structural materials and polymeric composites testing, which can provide useful information for design and fabrication of structural components.
Experimental scattering results using a microwave analog technique are described. Artificially constructed axially symmetric spheres with a graphite-like fine-layered composite structure and anisotropic refractive indices were employed to aid high-precision measurements of forward scattering under stable conditions (temperature, physical dimensions, electronic conditions) and to facilitate studies of the extinction and polarization of light by graphite particles in interstellar space. A theoretical approximation utilizing Mie theory for spheres with suitable orientation-dependent refractive indices is applied to account for changes in the complex forward-scattering amplitudes and phase in response to target orientation. The methods are extended to the full range of scattering angles, from the forward direction continuously to about 165 deg and at 180 deg. Agreement between experiment and prediction is close when the symmetry axis is parallel to the polarization.
One of the biggest challenges facing NASA's deep space exploration goals is structural mass. A long duration transit vehicle on a journey to Mars, for example, requires a large internal volume for cargo, supplies and crew support. As with all space structures, a large pressure vessel is not enough. The vehicle also requires thermal, micro-meteoroid, and radiation protection, a navigation and control system, a propulsion system, and a power system, etc. As vehicles get larger, their associated systems also get larger and more complex. These vehicles require larger lift capacities and force the mission to become extremely costly. In order to build large volume habitable vehicles, with only minimal increases in launch volume and mass, NASA is developing lightweight structures. Lightweight structures are made from non-metallic materials including graphite composites and high strength fabrics and could provide similar or better structural capability than metals, but with significant launch volume and mass savings. Fabric structures specifically, have been worked by NASA off and on since its inception, but most notably in the 1990's with the TransHAB program. These TransHAB developed structures use a layered material approach to form a pressure vessel with integrated thermal and micro-meteoroid and orbital debris (MMOD) protection. The flexible fabrics allow the vessel to be packed in a small volume during launch and expand into a much larger volume once in orbit. NASA and Bigelow Aerospace recently installed the first human-rated inflatable module on the International Space Station (ISS), known as the Bigelow Expandable Activity Module (BEAM) in May of 2016. The module provides a similar internal volume to that of an Orbital ATK Cygnus cargo vehicle, but with a 77% launch volume savings. As lightweight structures are developed, testing methods are vital to understanding their behavior and validating analytical models. Common techniques can be applied to fabric materials, such as tensile testing, fatigue testing, and shear testing, but common measurement techniques cannot be used on fabric. Measuring strain in a material and during a test is a critical parameter for an engineer to monitor the structure during the test and correlate to an analytical model. The ability to measure strain in fabric structures is a challenge for NASA. Foil strain gauges, for example, are commonplace on metallic structures testing, but are extremely difficult to interface with a fabric substrate. New strain measuring techniques need to be developed for use with fabric structures. This paper investigates options for measuring strain in fabric structures for both ground testing and in-space structural health monitoring. It evaluates current commercially available options and outlines development work underway to build custom measurement solutions for NASA's fabric structures.
This report details the initial comparison of mechanical strength properties between the cylindrical nuclear-grade graphite specimens irradiated in the second Advanced Graphite Creep (AGC-2) experiment with the established baseline, or unirradiated, mechanical properties compiled in the Baseline Graphite Characterization program. The overall comparative analysis will describe the development of an appropriate test protocol for irradiated specimens, the execution of the mechanical tests on the AGC-2 sample population, and will further discuss the data in terms of developing an accurate irradiated property distribution in the limited amount of irradiated data by leveraging the considerably larger property datasets being captured in the Baseline Graphite Characterization program. Integrating information on the inherent variability in nuclear-grade graphite with more complete datasets is one of the goals of the VHTR Graphite Materials program. Between “sister” specimens, or specimens with the same geometry machined from the same sub-block of graphite from which the irradiated AGC specimens were extracted, and the Baseline datasets, a comprehensive body of data will exist that can provide both a direct and indirect indication of the full irradiated property distributions that can be expected of irradiated nuclear-grade graphite while in service in a VHTR system. While the most critical data will remain the actual irradiated property measurements, expansion of this data into accurate distributions based on the inherent variability in graphite properties will be a crucial step in qualifying graphite for nuclear use as a structural material in a VHTR environment.
Since the reaction rate and cost for cathodic catalyst in polymer electrolyte membrane fuel cells are obstacles for commercialization, the high-performance catalyst for oxygen reduction reaction is necessary. The Ni encapsulated with N-doped graphitic carbon (Ni@NGC) prepared with ethylenediamine and carbon black is employed as an efficient support for the oxygen reduction reaction. Characterizations show that the Ni@NGC has a large surface area and mesoporous structure that is suitable to the support for the Pt catalyst. The catalyst structure is identified and the size of Pt nanoparticles distributed in the narrow range of 2–3 nm. Four different nitrogen species are doped properly into graphitic carbon structure. The Pt/Ni@NGC shows higher performance than the commercial Pt/C catalyst in an acidic electrolyte. The mass activity of the Pt/Ni@NGC in fuel cell tests exhibits over 1.5 times higher than that of commercial Pt/C catalyst. The Pt/Ni@NGC catalyst at low Pt loading exhibits 47% higher maximum power density than the Pt/C catalyst under H2-air atmosphere. These results indicate that the Ni@NGC as a support is significantly beneficial to improving activity.
A cylindrical shell skirt structure was subjected to a design and analysis study using a wide variety of structural materials and concepts. The design loading, axial compression, and torsion is representative of that expected on a typical space tug skirt section. Structural concepts evaluated included honeycomb sandwich, truss, isogrid, and skin/stringer/frame. The materials considered included a wide variety of structural metals as well as glass, graphite, and boron-reinforced composites. Honeycomb sandwich with aluminum faceskins, honeycomb sandwich with graphite/epoxy faceskins, and aluminum truss with fiberglass meteoroid protection layers were the designs selected for further evaluation. Procurement of materials required for fabrication is reported and the structural test plan and fabrication drawings are included. Construction of the graphite/epoxy faceskins, chem mill of the aluminum faceskins, chem mill of aluminum truss components, and fabrication of the graphite/epoxy honeycomb sandwich development panel is also reported.
A graphite component in a nuclear reactor core is subjected to variety of stresses and can experience degradation during normal and off-normal operation. Understanding how a graphite component will behave in service is essential to ensuring core structural stability and safe reactor operation. This report summarizes a graphite modeling tool currently under development at Idaho National Laboratory. The model incorporates several of the anticipated stresses during service and includes the effects of oxidation and irradiation prior to turnaround. This tool is intended to be used to help assess the design of graphite components by utilizing design code rules found in Section III, Division 5 of the American Society of Mechanical Engineering Boiler and Pressure Vessel Code. Specifically, the tool uses the methodologies found within the Full and Simplified assessments from Article HHA-3000 to verify that a graphite component has an acceptably low probability of failure.
Highlights: • S, B hertroatoms were successfully doped into g-C{sub 3}N{sub 4} by thermal treatment. • S, B heteroatoms effectively change the intrinsic electronic structure of g-C{sub 3}N{sub 4}. • The SBCN shows much higher photocatalytic activity than CN, SCN and BCN. • The SBCN has high photocatalytic stability and reusability. - Abstract: As a metal-free visible light photocatalyst, the photocatalytic performance of graphitic carbon nitride (g-C{sub 3}N{sub 4}) is limited. To improve the activity of g-C{sub 3}N{sub 4}, we herein report a binary S, B co-doped g-C{sub 3}N{sub 4} (SBCN) by thermally treating the precursor mixture of thiourea, melamine and boron oxide. Characterization results show the obtained SBCN has ultrathin sheet-like morphology and these doped heteroatoms are uniform distributed in the sample. Compared to the pristine g-C{sub 3}N{sub 4}, the SBCN has a small band gap with additional absorption in visible light region, decreased photoluminescence emission and electric resistance and enhanced photocurrent response. These advantages endue SBCN with excellent photocatalytic activity for degradation of organic dyes, and its reaction rate is 6.5 times higher than that of the g-C{sub 3}N{sub 4}. Moreover, the successive cycles demonstrate that this SBCN possesses a superior stability and reusability. Finally, we propose a possible photocatalytic mechanism based on the band structure and mainly active species.
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.
Solid-state carbon materials, such as graphite and graphene, are at the forefront of materials research because of their unique electronic, vibrational, and mechanical properties, leading to a broad range of potential and realized applications. One key application is their role as basic structural units of carbon fiber (CF), a lightweight alternative to steel. In CF, a delicate relationship exists between ultimate material strength and the atomic-scale density of defects contained at the inter- and intra-subunit levels. Computational studies provide insight into the stability of various types of defects that can form in these systems and connect with experimental observables such as bandgap and spectroscopic measurements. Therefore, the literature contains many computational studies that focus on changes induced by defects, including vacancies and Dienes transformations (Stone-Wales and Thrower defects). However, wide-ranging methods and cell sizes have been used, and property-specific information is often lacking. Furthermore, this review summarizes key literature findings, paying particular attention to changes in the electronic, vibrational, and mechanical properties induced by defects in graphitic materials relevant to CF.
The purpose of this work is to develop thermographic inspection methods and standards for use in evaluating structural composites and aerospace hardware. Qualification techniques and calibration methods are investigated to standardize the thermographic method for use in the field. Along with the inspections of test standards structural hardware, support hardware is designed and fabricated to aid in the thermographic process. Also, a standard operating procedure is developed for performing inspections with the Bales Thermal Image Processor (TIP). Inspections are performed on a broad range of structural composites. These materials include graphite/epoxies, graphite/cyanide-ester, graphite/silicon-carbide, graphite phenolic and Kevlar/epoxy. Also metal honeycomb (titanium and aluminum faceplates over an aluminum honeycomb core) structures are investigated. Various structural shapes are investigated and the thickness of the structures vary from as few as 3 plies to as many as 80 plies. Special emphasis is placed on characterizing defects in attachment holes and bondlines, in addition to those resulting from impact damage and the inclusion of foreign matter. Image processing through statistical analysis and digital filtering is investigated to enhance the quality and quantify the NDE thermal images when necessary.