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At least 793 records · Page 44

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NASA NTRS1991

Delamination behavior of quasi-isotropic graphite epoxy laminates subjected to tension and torsion loads

Sixteen and thirty-two ply quasi-isotropic laminates fabricated from AS4/3501-6 were subjected to pure tension, simultaneous tension and torsion, and torsion fatigue. Layups tested were (45 sub n/-45 sub n/0 sub n/90 sub n) sub s, with n = 2 or 4. A torsion damage pattern consisting of a localized matrix crack and delaminations was characterized, and the measured torsional stiffnesses were compared with calculated values. It was found that a combination of tension and torsion led to failure at smaller loads than either type of deformation acting alone. Further work is required to determine the exact form of the failure criterion.

Hinkley, J. A.↗

DOE OSTI2023

The Effects of Silicon and Niobium Concentration on the Solidification Behavior and Microstructure of Cast Monel Alloys

Cast Monel alloys are used in applications requiring a combination of good mechanical properties and excellent resistance to corrosion. Despite prevalent industrial use, relatively few studies have been conducted to investigate the relationships between composition, solidification behavior, and microstructure. Given that these alloys are used in the cast and welded conditions, these factors have a significant influence over the material properties. Here, in this work, microstructural characterization, electron probe microanalysis, X-ray diffraction, and differential scanning calorimetry were used to study how changes in Si and Nb concentrations affected the solidification path and microstructure of Monel alloys. It was found that increasing Nb concentration stabilized higher amounts of MC carbides and suppressed graphite formation during solidification. It was also found that the high nominal concentration and segregation of Si to the liquid led to the formation of Ni 31 Si 12 and other silicides via terminal eutectic reactions at the end of solidification. A pseudo-binary solidification diagram was constructed using experimental data and was applied to predict the mass fraction of solidified eutectic as a function of composition. The modeled microstructures were found to be in good agreement with experimentally measured phase fractions.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Oak Ridge National Laboratory Official TM Cover: Development and Qualification of Tungsten Reference Materials for LA-ICP-MS

Reference materials have been developed to provide areal density measurements of tungsten that is deposited on graphite when using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). Several reference materials of varying areal densities have been produced using a magnetron sputtering, thin film deposition technique. With multiple reference materials that have varying areal densities, a calibration curve has been developed for translating the detector response of an ICP-MS into a quantitative measurement. These results provide the opportunity to make calibrated comparisons across graphite samples that were exposed to tungsten transport experiments for nuclear fusion research. In addition, these methods may be applied to provide individual areal density measurements for the five unique isotopes of tungsten. It is found that areal density measurements via LA-ICP-MS agree with characterization for the same samples when using the more traditional Rutherford backscattering ion beam technique. Qualification of these reference materials was completed using ion beam laboratories at the University of Tennessee, Knoxville and Massachusetts Institute of Technology, and Sandia National Laboratory.

36 MATERIALS SCIENCE↗

NASA NTRS1983

Fire- and heat-resistant laminating resins based on maleimido-substituted aromatic cyclotriphosphazenes

A novel class of flame- and heat-resistant polymers has been synthesized by the thermal polymerization of maleimido-substituted aromatic cyclotriphosphazenes. The polymer obtained from tris-(aminophenoxy)tris(maleimidophenoxy)cyclotriphosphazene has good thermal stability and is noteworthy for its high char yield, viz., 82 percent at 800 C in nitrogen and 81 percent at 700 C in air. Graphite-fabric laminates prepared with this polymer did not burn in pure oxygen, even at 300 C, and were tested for mechanical properties. Hexakis(4-maleimidophenoxy)cyclotriphosphazene and some fluorine-containing monomers have also been synthesized. The structures of these cyclic phosphazene precursors and polymers were characterized by FT IR spectrophotometry, H-1 NMR, F-19 NMR, and P-31 solid-state magic angle spinning NMR spectroscopy, and mass spectrometry. The curing behavior of the polymer precursors and the thermal stabilities of the polymers were evaluated by differential scanning calorimetry (DSC) and thermogravimetric analyses (TGA).

Kumar, D.↗

DOE OSTI2010

An experimental test plan for the characterization of molten salt thermochemical properties in heat transport systems

Molten salts are considered within the Very High Temperature Reactor program as heat transfer media because of their intrinsically favorable thermo-physical properties at temperatures starting from 300 C and extending up to 1200 C. In this context two main applications of molten salt are considered, both involving fluoride-based materials: as primary coolants for a heterogeneous fuel reactor core and as secondary heat transport medium to a helium power cycle for electricity generation or other processing plants, such as hydrogen production. The reference design concept here considered is the Advanced High Temperature Reactor (AHTR), which is a large passively safe reactor that uses solid graphite-matrix coated-particle fuel (similar to that used in gas-cooled reactors) and a molten salt primary and secondary coolant with peak temperatures between 700 and 1000 C, depending upon the application. However, the considerations included in this report apply to any high temperature system employing fluoride salts as heat transfer fluid, including intermediate heat exchangers for gas-cooled reactor concepts and homogenous molten salt concepts, and extending also to fast reactors, accelerator-driven systems and fusion energy systems. The purpose of this report is to identify the technical issues related to the thermo-physical and thermo-chemical properties of the molten salts that would require experimental characterization in order to proceed with a credible design of heat transfer systems and their subsequent safety evaluation and licensing. In particular, the report outlines an experimental R&D test plan that would have to be incorporated as part of the design and operation of an engineering scaled facility aimed at validating molten salt heat transfer components, such as Intermediate Heat Exchangers. This report builds on a previous review of thermo-physical properties and thermo-chemical characteristics of candidate molten salt coolants that was generated as part of the same project [1]. However, this work focuses on two materials: the LiF-BeF2 eutectic (67 and 33 mol%, respectively, also known as flibe) as primary coolant and the LiF-NaF-KF eutectic (46.5, 11.5, and 52 mol%, respectively, also known as flinak) as secondary heat transport fluid. At first common issues are identified, involving the preparation and purification of the materials as well as the development of suitable diagnostics. Than issues specific to each material and its application are considered, with focus on the compatibility with structural materials and the extension of the existing properties database.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Characterization of Surface Free Energy of Composite Electrodes for Lithium-Ion Batteries

One critical step in lithium-ion battery manufacturing process is the electrolyte wetting step, which usually takes up to several days at elevated temperatures, posing a distinctive bottleneck in the manufacturing process especially for large-size cells. The electrode wettability depends on both the surface tension of electrolyte and the surface free energy of electrodes. This work reports a systematic study on the characterization of surface free energy of battery electrodes and the correlation between surface free energy and electrode processing. It shows that, when switching manufacturing from conventional solvent based processing to aqueous processing, the polar component of surface free energy increases 74.1% for NMC532 electrodes and 48.2% for A12 graphite electrodes. The results provide valuable guidance for electrode processing to optimize the electrolyte wetting process, helping lower processing costs and enable higher product quality and throughput.

25 ENERGY STORAGE↗

NASA NTRS1998

Study Methods to Standardize Thermography NDE

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 various graphite/epoxies, graphite/cyanide-ester, graphite/silicon-carbide, graphite phenolic and Keviar/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.

Walker, James L.↗

NASA NTRS1998

Study Methods to Standardize Thermography NDE

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.

Walker, James L.↗

DOE OSTI2012

Mixed Convection in the VHTR in the Event of a LOFA

The US Department of Energy, Office of Nuclear Energy (DOE-NE) is supporting the development of a very high temperature reactor (VHTR) concept as the primary focus of it next generation nuclear power plant (NGNP) program. The VHTR is cooled by forcing helium downwards through the core into the lower plenum and out the hot duct. In the event that the coolant circulators are lost, the driving pressure drop across the core will reduce to zero and there will be the opportunity for natural circulation to occur. During the time that the circulators are powering down, the heat transfer in the core from the graphite blocks to the helium coolant will transform from turbulent forced convection to mixed convection, where buoyancy effects become important, to free or natural convection, where buoyancy is dominant. Analysis of the nature of the forced, mixed and free convection is best done using computational fluid dynamic (CFD) software that can provide fine details of the flow and heat transfer. However, CFD analysis involves approximations in the results because of the finite nature of the spatial and temporal discretizations required, the inexact nature of the turbulence models that are used and the finite precision of the computers employed. Therefore, it is necessary to validate the CFD computations. Validation is accomplished by comparing results from specific CFD computations to experimental data that have been taken specifically for the purpose of validation and that are related to the physical phenomena in question. The present report examines the flow and heat transfer parameters (dimensionless numbers) that characterize the flow and reports ranges for their values based on specific CFD studies performed for the VHTR.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2015

The functionalization and characterization of multi-walled carbon nanotubes (MWCNTs)

Functionalization is the process of introducing chemical functional groups on the surface of the material. In this study, a multi-walled carbon nanotube (MWCNTs) was functionalized by oxidation treatment using concentrated nitric acid. The functionalized and pristine MWCNTs were analyzed by using Fourier Transform Infrared Spectroscopy (FT-IR) and X-Ray Diffraction (XRD). The XRD patterns exhibit the graphitic properties for all samples. Besides, the XRD results also demonstrate that the percent of crystallinity of MWCNTs increases as the duration of acid treatment increases. The percent of crystallinity increases from 66% to 80% when the pristine MWCNT treated for 12 hours with additional 12 hours reflux process with nitric acid. The IR spectrum for the 12 hours-treated MWCNTs shows the formation of carboxyl functional group. Additional 12 hours reflux process with nitric acid on the 12 hours-treated MWCNTs have shown the loss of existing carboxyl group and only hydroxyl group formed.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

NASA NTRS2000

Experimental and Numerical Characterization of a Cylindrical Blackbody Cavity

During hypersonic flight, high temperatures and high heat fluxes are generated on the surfaces of vehicles. The Flight Loads Laboratory (FLL) at Dryden Flight Research Center (DFRC) is equipped with a calibration furnace, capable of calibrating heat flux gages up to 1100kW per square meters, and temperature sensors up to 2600 C. One heating configuration of the calibration furnace is a cylindrical blackbody cavity. Throughout the blackbody there are temperature gradients due to various boundary conditions. These boundary conditions include resistance heating, radiant heat transfer, and conduction to water-cooled electrodes. Also, an inert gas is purged through the graphite blackbody to prevent it from oxidizing. Consequently, the various modes of heat transfer present during operation of the blackbody cavity must be well understood in order to produce accurate heat flux gage and temperature sensor calibrations for use in ground testing or flight testing of hypersonic vehicles. The first step towards understanding the heat transfer in the blackbody cavity was to perform experiments at 1100 C, with and without outer surface insulation, while taking detailed temperature measurements inside the blackbody cavity. Steady state thermal models of the blackbody cavity were then developed. These models included detailed thermal analysis using commercial thermal analysis software. Conduction, radiation, and convection were considered in the thermal models for two cases: one with the outside of the blackbody cavity insulated and the second without insulation. This paper describes the experimental and numerical efforts used to characterize the steady state operation of the blackbody cavity. It describes the analysis of the test measurements, the boundary conditions used in the numerical models, and how the models were calibrated to fit the experimental data. Effects of various uncertainties, such as material properties, and convection are discussed.Initial thermal models predicted temperatures in the deepest part of the blackbody cavity within 7 C of the measured value and produced trends comparable to the experimental data, throughout the models. Adjustment of the boundary conditions, which were included in the thermal models, produced good agreement with measured temperatures. Free and forced convection of the purge gas inside the blackbody was found to be insignificant.

Abdelmessih, Amanie N.↗

DOE OSTI2018

Solution-Based, Template-Assisted Realization of Large-Scale Graphitic ZnO

With a honeycomb single-atomic-layer structure similar to those of graphene and hexagonal boron nitride (hBN), the graphitic phase of ZnO (gZnO) have been predicted to offer many advantages for engineering, including high-temperature stability in ambient conditions and great potential in heterostructure applications. However, there is little experimental data about this hexagonal phase due to the difficulty of synthesizing large-area gZnO for characterization and applications. In this work, we demonstrate a solution-based approach to realize gZnO nanoflakes with thicknesses down to a monolayer and sizes up to 20 mum. X-ray photoelectron spectroscopy, X-ray absorption near-edge spectroscopy, photoluminescence, atomic force microscopy, and electron microscopy characterizations are conducted on synthesized gZnO samples. Measurements show significant changes to the electronic band structure compared to its bulk phase, including an increase of the band gap to 4.8 eV. The gZnO nanosheets also exhibit excellent stability at temperatures as high as 800 °C in ambient environment. This wide band gap layered material provides us with a platform for harsh environment electronic devices, deep ultraviolet optical applications, and a practical alternative for hBN. As a result, our synthesis method may also be applied to achieve other types of 2D oxides.

36 MATERIALS SCIENCE↗

DOE OSTI2011

Oxidation and disorder in few-layered graphene induced by the electron-beam irradiation

Structural changes caused by an electron beam with the high irradiation energy of 5 MeV were investigated in few-layered graphene. Both the original and the irradiated few-layered graphene were characterized by x-ray diffraction, Raman spectroscopy, and x-ray photoelectron spectroscopy. It was found that a typical diffraction peak of graphene oxide emerged and this may be attributed to a partial oxidation in few-layered graphene which was induced by the irradiation. In addition, the graphitic structure of few-layered graphene was found to be disordered according to the increased intensity ratio of D to G band.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2017

Understanding Function and Performance of Carbon Additives in Lead-Acid Batteries

While the low cost and strong safety record of lead-acid batteries make them an appealing option compared to lithium-ion technologies for stationary storage, they can be rapidly degraded by the extended periods of high rate, partial state-of-charge operation required in such applications. Degradation occurs primarily through a process called hard sulfation, where large PbSO 4 crystals are formed on the negative battery plates, hindering charge acceptance and reducing battery capacity. Various researchers have found that the addition of some forms of excess carbon to the negative active mass in lead-acid batteries can mitigate hard sulfation, but the mechanism through which this is accomplished is unclear. In this work, the effect of carbon composition and morphology was explored by characterizing four discrete types of carbon additives, then evaluating their effect when added to the negative electrodes within a traditional valve-regulated lead-acid battery design. The cycle life for the carbon modified cells was significantly larger than an unmodified control, with cells containing a mixture of graphitic carbon and carbon black yielding the greatest improvement. The carbons also impacted other electrochemical aspects of the battery (e.g., float current, capacity, etc.) as well as physical characteristics of the negative active mass, such as the specific surface area.

25 ENERGY STORAGE↗

DOE OSTI2012

Millimeter-Wave Thermal Analysis Development and Application to GEN IV Reactor Materials

New millimeter-wave thermal analysis instrumentation has been developed and studied for characterization of materials required for diverse fuel and structural needs in high temperature reactor environments such as the Next Generation Nuclear Plant (NGNP). A two-receiver 137 GHz system with orthogonal polarizations for anisotropic resolution of material properties has been implemented at MIT. The system was tested with graphite and silicon carbide specimens at temperatures up to 1300 ºC inside an electric furnace. The analytic and hardware basis for active millimeter-wave radiometry of reactor materials at high temperature has been established. Real-time, non contact measurement sensitivity to anisotropic surface emissivity and submillimeter surface displacement was demonstrated. The 137 GHz emissivity of reactor grade graphite (NBG17) from SGL Group was found to be low, ~ 5 %, in the 500 – 1200 °C range and increases by a factor of 2 to 4 with small linear grooves simulating fracturing. The low graphite emissivity would make millimeter-wave active radiometry a sensitive diagnostic of graphite changes due to environmentally induced stress fracturing, swelling, or corrosion. The silicon carbide tested from Ortek, Inc. was found to have a much higher emissivity at 137 GHz of ~90% Thin coatings of silicon carbide on reactor grade graphite supplied by SGL Group were found to be mostly transparent to millimeter-waves, increasing the 137 GHz emissivity of the coated reactor grade graphite to about ~14% at 1250 ºC.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

NASA NTRS1980

Creep-rupture of polymer-matrix composites

An accelerated characterization method for resin matrix composites is reviewed. Methods for determining modulus and strength master curves are given. Creep rupture analytical models are discussed as applied to polymers and polymer matrix composites. Comparisons between creep rupture experiments and analytical models are presented. The time dependent creep rupture process in graphite epoxy laminates is examined as a function of temperature and stress level.

Brinson, H. F.↗

NASA NTRS2016

A Raman Study of Carbonates and Organic Contents in Five CM Chondrites

Carbonates comprise the second most abundant class of carbon-bearing phases in carbonaceous chondrites after organic matter (approximately 2 wt.%), followed by other C-bearing phases such as diamond, silicon carbide, and graphite. Therefore, understanding the abundances of carbonates and the associated organic matter provide critical insight into the genesis of major carbonaceous components in chondritic materials. Carbonates in CM chondrites mostly occur as calcite (of varying composition) and dolomite. Properly performed, Raman spectroscopy provides a non-destructive technique for characterizing meteorite mineralogy and organic chemistry. It is sensitive to many carbonaceous phases, allows the differentiation of organic from inorganic materials, and the interpretation of their spatial distribution. Here, with the use of Raman spectroscopy, we determine the structure of the insoluble organic matter (IOM) in the matrix and carbonate phases in five CM chondrites: Jbilet Winselwan, Murchison, Nogoya, Santa Cruz, and Wisconsin Range (WIS) 91600, and interpret the relative timing of carbonate precipitation and the extent of the associated alteration events.

Chan, Q. H. S.↗

NASA NTRS2003

Studies on Hot-Melt Prepregging of PMR-II-50 Polyimide Resin with Graphite Fibers

A Second generation PMR (in situ Polymerization of Monomer Reactants) polyimide resin, PMR-II-50, has been considered for high temperature and high stiffness space propulsion composites applications for its improved high temperature performance. As part of composite processing optimization, two commercial prepregging methods: solution vs. hot-melt processes were investigated with M40J fabrics from Toray. In a previous study a systematic chemical, physical, thermal and mechanical characterization of these composites indicated that poor resin-fiber interfacial wetting, especially for the hot-melt process, resulted in poor composite quality. In order to improve the interfacial wetting, optimization of the resin viscosity and process variables were attempted in a commercial hot-melt prepregging line. In addition to presenting the results from the prepreg quality optimization trials, the combined effects of the prepregging method and two different composite cure methods, i.e., hot press vs. autoclave on composite quality and properties are discussed.

Shin, E. Eugene↗