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At least 343 records · Page 19

Specimen geometry effects on graphite/PMR-15 composites during thermo-oxidative aging

Studies were conducted to establish the effects of specimen geometry on the thermo-oxidative stability and the mechanical properties retention of unidirectional Celion 12000 graphite fiber reinforced PMR-15 polyimide composites. Weight loss, flexural strength and interlaminar shear strength are measured at isothermal aging times as long as 1639 hr at a temperature of 316 C for three different specimen geometries. It is found that the three different types of specimen surfaces exhibit different values of weight loss/unit area. The mechanical properties retention is also found to be dependent on geometry for these composites. The interlaminar shear strength decreases significantly over the complete range of aging times. The flexural strength retention starts showing geometric dependency after about 1000 hr of aging at 316 C. Weight loss fluxes, associated with the three different types of exposed surfaces, are calculated and used to develop an empirical mathematical model for predicting the weight loss behavior of unidirectional composites of arbitrary geometries. Data are presented comparing experimentally determined weight loss with weight loss values predicted using the empirical model.

Bowles, K. J.↗

Creep Forming of Carbon-Reinforced Ceramic-Matrix Composites

A set of lecture slides describes an investigation of creep forming as a means of imparting desired curvatures to initially flat stock plates of carbon-reinforced ceramic-matrix composite (C-CMC) materials. The investigation is apparently part of a continuing effort to develop improved means of applying small CCMC repair patches to reinforced carbon-carbon leading edges of aerospace vehicles (e.g., space shuttles) prior to re-entry into the atmosphere of the Earth. According to one of the slides, creep forming would be an intermediate step in a process that would yield a fully densified, finished C-CMC part having a desired size and shape (the other steps would include preliminary machining, finish machining, densification by chemical vapor infiltration, and final coating). The investigation included experiments in which C-CMC disks were creep-formed by heating them to unspecified high temperatures for time intervals of the order of 1 hour while they were clamped into single- and double-curvature graphite molds. The creep-formed disks were coated with an oxidation- protection material, then subjected to arc-jet tests, in which the disks exhibited no deterioration after exposure to high-temperature test conditions lasting 490 seconds.

Vaughn, Wallace L.↗

High efficiency electrolytes for high voltage battery systems

Disclosed herein are embodiments of an electrolyte that is stable and efficient at high voltages. The electrolyte can be used in combination with certain cathodes that exhibit poor activity at such high voltages with other types of electrolytes and can further be used in combination with a variety of anodes. In some embodiments, the electrolyte can be used in battery systems comprising a lithium cobalt oxide cathode and lithium metal anodes, silicon anodes, silicon/graphite composite anodes, graphite anodes, and the like.

Ren, Xiaodi↗

HRTEM and EFTEM Observations of Matrix in the Oxidized CV3 Chondrite ALH 84028: Implications for the Origins of Matrix Olivines

The determination of the nature, distribution, and origin of organic material in carbonaceous chondrites is fundamental to understanding early solar nebular conditions and the origin of life. Using a variety of extraction techniques, followed by detailed chemical analysis, an extensive suite of organic compounds has been identified in carbonaceous chondrites. These data have provided key information on the diversity and isotopic composition of the organic component in chondrites. However, one disadvantage of extraction techniques is that all information regarding the spatial distribution of the organics on a fine scale is lost. This is especially important for the insoluble macromolecular carbon, which constitutes approximately 70% of the carbon in carbonaceous chondrites such as Murchison. The distribution and mineralogical associations may provide important constraints on the possible origins of the carbonaceous material. Our previous studies of the CV3 chondrites Allende and Vigarano have demonstrated that energy filtered transmission electron microscopy (EFTEM), combined with high resolution TEM (HRTEM) are powerful tools for the in situ characterization of insoluble organic matter in carbonaceous chondrites. In this study, we have used SEM and TEM techniques to characterize the matrix mineralogy of the CV3 chondrite ALH 84028 and examine the distribution and mineralogical associations of carbon. We are especially interested in establishing whether the occurrence of poorly graphitized carbon (PGC), observed in Allende matrix olivines, is common to all oxidized CV3 chondrites or is a unique feature of Allende.

Abreu, Neyda M.↗

Correlations of norbornenyl crosslinked polyimide resin structures with resin thermo-oxidative stability, resin glass transition temperature and composite initial mechanical properties

PMR (polymerization of monomeric reactants) methodology was used to prepare 70 different polyimide oligomeric resins and 30 different unidirectional graphite fiber/polyimide composites. Monomeric composition as well as chain length between sites of crosslinks were varied to examine their effects on resin thermo-oxidative stability and glass transition temperature (Tg) of the cured/postcured resins. A linear correlation of decreasing 316 C resin weight loss/surface area versus (1) decreasing aliphatic content, or (2) increasing benzylic/aliphatic content stoichiometry ratio over a wide range of resin compositions was observed. An almost linear correlation of Tg versus molecular distance between the crosslinks was also observed. An attempt was made to correlate Tg with initial composite mechanical properties (flexural strength and interlaminar shear strength). However, the scatter in mechanical strength data prevented obtaining a clear correlation. Instead, only a range of composite mechanical properties was obtained at 25, 288, and 316 C. Perhaps more importantly, what did become apparent during the correlation study was (1) the PMR methodology could be used to prepare composites from resins containing a wide variety of monomer modifications, (2) that these composites almost invariably provided satisfactory initial mechanical properties as long as the resins formulated exhibited satisfactory processing flow, and (3) that PMR resins exhibited predictable rates of 316 C weight loss/surface area based on their benzylic/aliphatic stoichiometery ratio.

Alston, William B.↗

An evaluation of candidate oxidation resistant materials for space applications in LEO

Ground based testing of materials considered for polyimide (Kapton) solar array blanket protection and graphite-epoxy stroctural member protection was performed in an RF plasma asher. Protective coatings on Kapton from various commercial sources and from NASA Lewis Research Center were exposed to the air plasma; and mass loss per unit area was measured for each sample. All samples evaluated provided some protection to the underlying surface, but metal-oxide-fluoropolymer coatings provided the best protection by exhibiting very little degradation after 47 hr of asher exposure. Mica paint was evaluated as a protective coating for graphite-epoxy structural members. Mica appeared to be resistant to attack by atomic oxygen, but only offered limited protection as a paint. this is believed to be due to the paint vehicle ashing underneath the mica leaving unattached mica flakes lying on the surface. The protective coatings on Kapton evaluated so far are promising but further research on protection of graphite-epoxy support structures is needed.

Rutledge, Sharon↗

Structural studies on carbon materials for advanced space technology. Part 1: Structure and oxidation behavior of some carbon/carbon composite materials

The microstructure and some microstructural effects of oxidation have been investigated for laminar carbon fiber cloth/cloth binder matrix composite materials. It was found that cloth wave is important in determining the macrostructure of the composites X-ray diffraction analysis showed that the composites were more graphitic than the constituent fiber phases, indicating a graphitic binder matrix phase. Various tests which were conducted to investigate specific properties of the material are described. It was learned that under the moderate temperature and oxidant flow conditions studied, C-700, 730 materials exhibit superior oxidation resistance primarily because of the inhibiting influence of the graphitized binder matrix.

Fischbach, D. B.↗

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↗

Rheological characterization of addition polyimide matrix resins and prepregs

Although graphite-reinforced polyimide matrix composites offer outstanding specific strength and stiffness, together with high thermal oxidative stability, processing problems connected with their rheological behavior remain to be addressed. The present rheological studies on neat polyimide resin systems encountered outgassing during cure. A staging technique has been developed which can successfully handle polyimide samples, and novel methods were applied to generate rheological curves for graphite-reinforced prepregs. The commercial graphite/polyimide systems studied were PRM 15, LARC 160, and V378A.

Maximovich, M. G.↗

Mechanical behavior analysis using small-size graphite disc compression testing with digital image correlation methods

The ASTM International Standard Test Method for Tensile Stress-Strain of Carbon and Graphite (ASTM C749) requires dog-bone shaped specimens. Unfortunately, specimen sizes required in ASTM C749 are much too large for irradiation within a test reactor and are incompatible with irradiation capsule volumes, molten salt degradation facilities, or oxidation apparatus. The ASTM International Standard Test Method for Tensile Strength Estimate by Disc Compression of Manufactured Graphite (ASTM D8289) was developed as an alternative that provides a means for testing tensile properties using smaller specimens when geometric constraints are present. However, the important stress–strain relation throughout the test loading history that could be recorded using ASTM C749 is lost by using ASTM D8289 because of the difficulties involved with using traditional strain gauges or extensometers on such a small specimen. In this work, a digital image correlation (DIC) method, which uses a full-field noncontact surface displacement measurement technique, was applied along with the ASTM D8289 splitting tensile test on eight small samples of graphite grade Mersen 2114 to track their deformation during compressive loading. Initial results showed that the DIC technique can measure the surface displacement/strain on these small (Ø6 × 3 mm) graphite specimens with high accuracy and good repeatability, indicating that the DIC technique, combined with the small-disc splitting tensile test in ASTM D8289, can capture the strain evolution in the test. In conclusion, further comparison of measured strains with analytical and numerical simulation results provides additional understanding of the mechanical behaviour of this nuclear graphite material in complex stress states.

36 MATERIALS SCIENCE↗

Heterogeneous Combustion of Porous Graphite Particles in Microgravity

Recent theoretical investigations on graphite particle combustion have employed several levels of heterogeneous reaction models, ranging from global to elementary models, to describe the oxidation of carbon to gaseous products. Unlike the counterpart homogeneous reaction models, these heterogeneous reaction models are not well developed because of the difficulties associated with decoupling the physical characteristics of the solid (e.g. surface area taking part in combustion) from the chemical kinetic data. This is certainly true for porous graphite particle combustion, where heterogeneous and homogeneous reactions occur within the pores and play an important role in the overall oxidation process. As a result, there are considerable uncertainties of physical phenomena predicted using different heterogeneous kinetic models available in the literature. A good example, discussed later in this paper, is the predicted critical particle size below which the mass burning rate becomes exponentially small. The main goal of this study is to understand the basic mechanism controlling such rapid changes in burning rates, by developing a model where physical contributions are decoupled from chemical rate constants in a consistent manner. Another important goal of the proposed study is to develop a truly intrinsic, detailed heterogeneous reaction model for porous graphite combustion at high-temperatures, and to derive a systematically reduced heterogeneous reaction model in terms of the elementary reaction rate constants of the detailed model. The validation of chemical kinetic models describing the heterogeneous and homogeneous combustion in and around a spherically symmetric porous graphite particle can be considerably simplified by experimental measurements obtained under microgravity conditions. A vital component of this study is to conduct such supporting experiments on particle burning rate and surface temperature using NASA microgravity facilities, in close coordination with the theoretical effort. The basic understanding obtained and models developed as part of this project will be useful for optimal design of coal combustion devices. These models can also be extended to investigate the role of heterogeneous chemistry on pollutant formation pathways in combustion devices. The theoretical approach developed here, with pore diffusion effects decoupled from the chemical effects, can also be extended to understand the heterogeneous combustion of other porous fuels, for example, combustion of magnesium in a CO2 environment for propulsion in the Martian atmosphere.

Chelliah, Harsha K.↗

A control oriented comprehensive degradation model for battery energy storage system life prediction

In order to ensure that stationary battery energy storage systems (BESSs) provide reliable energy buffering, both for power quality and economic purposes, the degradation must be considered. Cell degradation involves various side reactions and is highly dependent on its operating conditions. To accurately track cell degradation and predict its impact on battery behavior, a comprehensive physics-based degradation model based on an electrolyte phase-enhanced single particle (SP) model is developed. Key degradation physics, namely solid electrolyte interphase (SEI) layer formation and growth, Li plating on the graphite anode, and Mn dissolution on cathode of nickel-cobalt-manganese oxide (NMC622) are considered. The model is validated against experimental capacity data. The results reveal that the deposition rate of both SEI layer and Li metal increase as the charge voltage increases. At the cathode side, the solvent oxidation rate determines the Mn dissolution rate. As a result, the volume fraction of NMC622 in the cathode continually decreases at a gradually increasing rate.

25 ENERGY STORAGE↗

Upcycling Polyethylene Waste Into Advanced Carbon Materials Used for Energy Storage Applications

Upcycling plastic into advanced carbons, such as graphite and graphene, offers attractive options to manage waste streams by converting the plastic into carbon electrode materials for energy storage devices. However, polyethylene (PE) is notoriously difficult to upcycle because it decomposes into light gases at approximately 350-400 °C which prevents processing it at higher temperatures to convert it into advanced carbons. This work addresses this challenge by oxidatively functionalizing PE between 300-330 C which stabilizes it for higher temperature processing into graphite & graphene. In addition, the graphite & graphene are tested as lithium-ion battery or supercapacitor electrodes where their electrochemical performances outperform commercial materials.

graphene↗

Upcycling Polyethylene Waste Into Advanced Carbon Materials Used for Energy Storage Applications

Upcycling plastic into advanced carbons, such as graphite and graphene, offers attractive options to manage waste streams by converting the plastic into carbon electrode materials for energy storage devices. However, polyethylene (PE) is notoriously difficult to upcycle because it decomposes into light gases at approximately 350-400 °C which prevents processing it at higher temperatures to convert it into advanced carbons. This work addresses this challenge by oxidatively functionalizing PE between 300-330 C which stabilizes it for higher temperature processing into graphite & graphene. In addition, the graphite & graphene are tested as lithium-ion battery or supercapacitor electrodes where their electrochemical performances outperform commercial materials.

graphene↗

Carbon isotopes in bulk carbonaceous chondrites

The chemical and physical processes involved in the formation of the solar system are examined. Primitive matter has been found on a microscopic scale in a variety of meteorites: fragments of small solar system bodies that were never part of a large planet. This primitive matter has, in most cases, been identified by the presence of anomalous abundances of some isotopes of the chemical elements. Of particular interest for carbon isotope studies are the primitive meteorites known as carbonaceous chondrites. Using a selective oxidation technique to sort out the carbon contained in different chemical forms (graphite, carbonates, and organic matter), four carbonaceous chondrites are analyzed. The presence of the (13) C-rich component was confirmed and additional carbon components with different, but characteristic, isotopic signatures were resolved.

Halbout, J.↗

Phosphorus-containing imide resins - Modification by elastomers

The syntheses and general features of addition-type maleimide resins based on bis(m-aminophenyl)phosphine oxide and tris(m-aminophenyl)phosphine oxide have been reported previously. These resins have been used to fabricate graphite cloth laminates having excellent flame resistance. These composites did not burn even in pure oxygen. However, these resins were somewhat brittle. This paper reports the modification of these phosphorus-containing resins by an amine-terminated butadiene-acrylonitrile copolymer (ATBN) and a perfluoroalkylene diaromatic amine elastomer (3F). An approximately two-fold increase in short beam shear strength and flexural strength was observed at 7 percent ATBN concentration. The tensile, flexural, and shear strengths were reduced when 18 percent ATBN was used. Anaerobic char yields of the resins at 800 C and the limiting oxygen indexes of the laminates decreased with increasing ATBN concentration. The perfluorodiamine (3F) was used with both imide resins at 6.4 percent concentration. The shear strength was doubled in the case of the bisimide with no loss of flammability characteristics. The modified trisimide laminate also had improved properties over the unmodified one. The dynamic mechanical analysis of a four-ply laminate indicated a glass transition temperature above 300 C. Scanning electron micrographs of the ATBN modified imide resins were also recorded.

Varma, I. K.↗

High-Temperature Treatments For Polyimide/Graphite Composite

Combination of inert-gas heat treatment and coating with material impermeable by oxygen proposed to increase thermo-oxidative and high-temperature structural stabilities of composite materials made of graphite fibers in matrices of PMR-15 polyimide. Proposal directed toward development of lightweight matrix/fiber composites for use in aircraft engines, wherein composites exposed to maximum operating temperatures between 371 and 427 degrees C.

Bowles, Kenneth J.↗