Analyzing carbon fiber structures observed by helium ion microscopy and their mechanical properties
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Low electronic conductivities and improper morphologies of anode electrodes greatly limit the reaction area, catalyst utilization and efficiency in proton exchange membrane water electrolyzers. In this study, conductive sublayers with different conductivities and morphologies were introduced into anode electrodes in membrane-based water electrolyzers. In-situ and ex-situ investigation results showed that conductive sublayers (Au mesh and carbon nanotube (CNT) film) augmented the sheet conductivity of anode electrodes by up to 4000 times (from 2000 to 0.5 ohm square -1 ), and the ohmic resistance of water electrolyzers was reduced to 1/3 when inserting conductive sublayers. In addition, CNT film provided a higher electrochemical active area than Au mesh, because of favorable morphologies (large porosity and surface area) of CNT fibers on CNT films. Therefore, the current density of water splitting was increased by 3 times (from 4.55 mA cm -2 to 14.83 mA cm -2 ) at 2.5 V compared to a conventional anode electrode. Visualizations on bubble dynamics showed improved performances with conductive sublayers; this was mainly due to greatly increased number of reaction sites, highly spread reaction area (from 50 to 1000 um), and reduced activation overpotential. Therefore, a balance between high electronic conductivity and nanoporous morphology is essential to the anode electrode for larger reaction sites and areas in highly efficient water electrolyzers.
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This work provides a summary of selected experimental capabilities being developed to support nonnuclear testing and demonstration of technology in support of microreactors under the U.S. Department of Energy’s (DOE’s) Microreactor Program. Major capabilities include the Single Primary Heat Extraction and Removal Emulator (SPHERE) and the Microreactor Agile Non-nuclear Experimental Test Bed (MAGNET). The SPHERE facility allows for controlled testing of the steady-state and transient heat rejection capabilities of a single heat pipe using electrical heaters that simulate nuclear heating. The facility is capable of monitoring axial temperature profiles along the heat pipe and surrounding test articles during startup, steady-state operation, and transients. Instrumentation includes noncontact infrared thermal imaging, surface thermocouples, spatially distributed fiber optic temperature and strain sensors, electrical power meters, and a water-cooled, gas-gap calorimeter for quantifying heat rejection from the heat pipe. The facility can be operated under both vacuum and inert-gas conditions. The MAGNET facility is a large-scale, 250-kW electrically heated microreactor test bed to enable nonnuclear experimental evaluation of a variety of microreactor concepts. It can be supplied to electrically heat a scaled section of a microreactor and further test the capabilities of heat rejection systems. The initial MAGNET experiments will support technology maturation and reduce uncertainty and risk associated with the design, operation, and deployment of monolithic heat pipe–based reactors. However, this test bed can broadly be applied to multiple microreactor concepts to evaluate a wide range of thermal-hydraulic and structural phenomena such as interface coupling with power conversion units and other collocated systems. MAGNET can evaluate integral thermomechanical effects during electrical heating of an array of heat pipes in a larger test article. Examples of initial testing will include thermal stresses in the monolith and the impact of debonding of a heat pipe from the core block and how that failure could impact surrounding heat pipes, i.e., understanding the potential for cascading failure. This work also discusses some modeling capabilities that can support experiment design, analysis, and interpretation, including the heat pipe code Sockeye and a comparison of thermal-structural simulations performed using ABAQUS and STAR-CCM+.
Compressive properties and weight saving of metals reinforced on surface with resin bonded fibers
Manufacturing development studies have been conducted to provide information on the fabrication and handling characteristics of a number of candidate multilayer insulation systems. The application of these complex, lightweight insulation systems to large-scale, flight-type cryogenic tankage and other structures has of necessity required the development of new methods, processes, and tooling concepts. Results of some of the studies that have contributed to the advancement of cryogenic technology are presented. The insulation systems that are of primary importance for future application are those using the sliced foam spacers, the net type spacers, the glass fiber paper spacers, and the Superfloc system which consists of tufts of dacron fibers flocked on the surface of the radiation shields.
Analytical trade studies are presented that consider passive TPS configurations using the following material categories: (1) reuseable surface insulation - surface-coated rigidized ceramic fiber; (2) low density charring ablators; and (3) carbon-carbon and high density ablators for leading edge areas. Emphasized are effects on TPS weight by variations in entry trajectories and material thermal characteristics.
Studies conducted with addition-type polyimides are reviewed with emphasis on the development of the Polymerization of Monomer Reactants (PMR) approach, in which PMR occurs on the surface of the reinforcing fibers.
A review is presented of studies conducted with addition-cured polyimides, giving particular attention to an improved method involving in situ polymerization of monomer reactants (PMR) on the surface of the reinforcing fibers. The studies show that the PMR approach provides a powerful method for fabricating high performance polymer matrix composites. Significant advantages of the PMR approach are related to the superior high temperature properties of the obtained material, lower cost, greater safety, and processing versatility.
It is found that the mechanical properties of fibrous refractory composite insulation (FRCI) can be improved if a higher calcination temperature is used before final processing. The results also reveal that a higher density FRCI containing 60 wt pct aluminoborosilicate fibers will exhibit minimal surface recession at 1480 C in a convective-heating environment. Another finding is that the material performance in the convective-heating environment is limited by the coating and the temperature capability of its emittance agent. A table is included giving the coating compositions used with the composite insulation and tested in the convectively heated environment at a surface temperature of 1480 C.
This program was directed primarily to the development of the negative (Cr3+/Cr2+) electrode for the NASA chromous/ferric Redox battery. The investigation of the effects of substrate processing and gold/lead catalyzation parameters on electrochemical performance were continued. In addition, the effects of reactant cross-mixing, acidity level, and temperature were examined for both Redox couples. Finally, the performance of optimized electrodes was tested in system hardware (1/3 square foot single cell). The major findings are discussed: (1) The recommended processing temperature for the carbon felt, as a substrate for the negative electrode, is 1650 to 1750 C, (2) The recommended gold catalyzation procedure is essentially the published NASA procedure (NASA TM-82724, Nov. 1981) based on deposition from aqueous methanol solution, with the imposition of a few controls such as temperature (25 C) and precatalyzation pH of the felt (7), (3) Experimental observations of the gold catalyzation process and subsequent electron microscopy indicate that the gold is deposited from the colloidal state, induced by contact of the solution with the carbon felt, (4) Electrodeposited lead appears to be present as a thin uniform layer over the entire surface of the carbon fibers, rather than an discrete particles, and (5) Cross-mixing of reactants (Fe-2+ in negative electrode solution or Cr-3+ in the positive electrode solution) did not appear to produce significant interference at either electrode.
In the experimental phase of the present study of the interlaminar fracture behavior of a randomly oriented short fiber sheet molding compound (SMC) composite, the double cantilever beam fracture test is used to evaluate the mode I interlaminar fracture toughness of different composite thicknesses. In the analytical phase of this work, a geometrically nonlinear analysis is introduced in order to account for large deflections and nonlinear load deflection curves in the evaluation of interlaminar fracture toughness. For the SMC-R50 material studied, interlaminar toughness is an order of magnitude higher than that of unreinforced neat resin, due to unusual damage mechanisms ahead of the crack tip, together with significant fiber bridging across crack surfaces. Composite thickness effects on interlaminar fracture are noted to be appreciable, and a detailed discussion is given on the influence of SMC microstructure.
A series of graphite fiber/PMR-15 polyimide composites were subjected to isothermal aging at 350 C in flowing air (100 cc/min and 1000 cc/min) over a 520 hr time period. The graphite fibers were analyzed by ISS/SIMS techniques before composite fabrication. Fibers exposed at the surface of the composite due to the isothermal aging process were also analyzed by the ISS/SIMS method. Component and composite weight less studies were also conducted for similarly exposed materials. Optical micrograph investigations of composites to follow the progress of the thermo-oxidative process were also conducted. Flexural and interlaminar shear strengths of the imaged and aged composites were measured. The relationship of component and composite properties as they relate to the thermo-oxidative behavior of the materials was discussed.
Water-cooled optical probe measures temperature of nearby radiating object. Intended primarily for use in silicon-growing furnace for measuring and controlling temperatures of silicon ribbon, meniscus, cartridge surfaces, heaters, or other parts. Cooling water and flushing gas cool fiber-optic probe and keep it clean. Fiber passes thermal radiation from observed surface to measuring instrument.
Ti-15-3 reinforced with SCS-6 silicon carbide fibers, in five different layups, was tested at 650 C to determine monotonic and fatigue strengths, basic mechanical properties, and damage initiation and progression. The elevated temperature results were compared to those obtained at room temperature. Analytical predictions were made of the monotonic stress-strain response as well as cyclic stress-strain hysteresis. The fiber reinforcement was found to significantly increase the static and fatigue strengths of the laminates over that of the matrix material at elevated temperature while the increase was insignificant at room temperature. Initial damage, in either the fibers or the matrix, was partitioned as a function of the life and applied strain range in the constituents. High strains and short lives resulted in multiple fiber failure with no signs of matrix fatigue cracking. Low strains and long lives resulted in extensive matrix cracking and no fiber breaks away from the fracture surface. At 650 C the matrix was too weak to cause fiber-matrix interface failure prior to matrix yielding. Laminate fatigue lives were hypothesized to be a function of the 0 deg fiber stress. More scatter was found in the 0 deg fiber stress vs. high temperature fatigue life data than for the room temperature data. An initial unloading modulus that was greater than the initial loading modulus was observed in the elevated temperature fatigue tests.
Halogenated CBr(sub x)I(sub y) (1 less than y/x less than 10) was made by exposing graphite materials with interplanar spacing in the 3.35 to 3.41 A range to either pure Br2 or an I2-Br2 mixture, and then to iodine vapor containing a small amount of Br2. The electrical resistivity of this product is from 3 to 6.5 times the pristine value. The presence of a small amount of isoprene rubber in the reaction significantly increased the iodine to bromine ratio in the product. In this reaction, rubber is known to generate HBr and to slowly remove bromine from the vapor. The halogenation generally caused a 22 to 25 percent weight increase. The halogens were found uniformly distributed in the product interior. However, although the surface contains very little iodine, it has high concentrations of bromine and oxygen. It is believed that the high concentrations of bromine and oxygen in this surface cause the halogenated fiber to be more resistant to fluorine attack during subsequent fluorination to fabricate graphite fluoride fibers.
Ti-15-3 reinforced with SCS-6 silicon carbide fibers, in five different layups, was tested at 650 C to determine monotonic and fatigue strengths, basic mechanical properties, and damage initiation and progression. The elevated temperature results were compared to those obtained at room temperature. Analytical predictions were made of the monotonic stress-strain response as well as cyclic stress-strain hysteresis. The fiber reinforcement was found to significantly increase the static and fatigue strengths of the laminates over that of the matrix material at elevated temperature while the increase was insignificant at room temperature. Initial damage, in either the fibers or the matrix, was partitioned as a function of the life and applied strain range in the constituents. High strains and short lives resulted in multiple fiber failure with no signs of matrix fatigue cracking. Low strains and long lives resulted in extensive matrix cracking and no fiber breaks away from the fracture surface. At 650 C the matrix was too weak to cause fiber-matrix interface failure prior to matrix yielding. Laminate fatigue lives were hypothesized to be a function of the 0 deg fiber stress. More scatter was found in the 0 deg fiber stress vs. high temperature fatigue life data than for the room temperature data. An initial unloading modulus that was greater than the initial loading modulus was observed in the elevated temperature fatigue tests.
A finite element-based numerical technique has been developed to simulate damage growth in unidirectional composites. This technique incorporates elastic-plastic analysis, micromechanics analysis, failure criteria, and a node splitting and node force relaxation algorithm to create crack surfaces. Any combination of fiber and matrix properties can be used. One of the salient features of this technique is that damage growth can be simulated without pre-specifying a crack path. In addition, multiple damage mechanisms in the forms of matrix cracking, fiber breakage, fiber-matrix debonding and plastic deformation are capable of occurring simultaneously. The prevailing failure mechanism and the damage (crack) growth direction are dictated by the instantaneous near-tip stress and strain fields. Once the failure mechanism and crack direction are determined, the crack is advanced via the node splitting and node force relaxation algorithm. Simulations of the damage growth process in center-slit boron/aluminum and silicon carbide/titanium unidirectional specimens were performed. The simulation results agreed quite well with the experimental observations.