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NASA NTRS1994

Graphite intercalation compound with iodine as the major intercalate

Halogenated graphite CBr(x)I(y) (I less than y/x less than 10) was made by exposing graphite materials to either pure Br2 or an I2/Br2/HBr mixture to initiate the reaction, and then to iodine vapor containing a small amount of Br2/HBr/IBr to complete the intercalation reaction. Wetting of the graphite materials by the I2/Br2/HBr mixture is needed to start the reaction, and a small amount of Br2/HBr/IBr is needed to complete the charge transfer between iodine and carbon. The interplanar spacings for the graphite materials need to be in the 3.35 to 3.41 A range. The X-ray diffraction data obtained from the halogenated HOPG indicate that the distance between the two carbon layers containing intercalate is 7.25 A. Electrical resistivity of the fiber 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 percent 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 structural damage during subsequent fluorination to fabricate graphite fluoride fibers.

Hung, Ching-Cheh↗

DOE OSTI2022

Printable Fiber Reinforced Cement Composites – Feasibility Study

Additive manufacturing is enabling the manufacturability of structures with previously unattainable complexity or functionality, and there is growing interest in additive manufacturing of “printed” concrete structures. The focus of this Phase 1 Technical Collaboration (TC) project was to evaluate feasibility of printing hybrid cement composite structures reinforced with textile carbon fibers (tCF). This project leverages other (non-IACMI) projects on cement formulation and printing process development, as well as on the production process for tCF. This project’s primary focus was to explore cement composite mix design with textile carbon fibers to be manufactured by MonteFibre (TC partner) and evaluate suitable fiber-matrix interface or sizing for cement composites working with Michelman (TC Partner). This project supports IACMI’s goal of reducing the cost and embodied energy of carbon fiber composites. Cost is one of the fundamental challenges to carbon fiber reinforced cement composites. Cement is an extremely inexpensive material (approximately $\$$0.05/lb). Adding 1 wt% of conventional carbon fiber to cement quadruples its cost. Therefore, the need to use low-cost carbon fiber and ensure that the additional cost of the carbon fiber has a greater cost benefit to the final product. This was the first preliminary evaluation to integrate tCF reinforcement in cement composites, and such potential tCF utilization should significantly reduce materials cost. Cement composite production is energy and emissions intensive, thus by strengthening it less material will be required. Hence, the embodied energy and production time of the resulting structures will be reduced. Additionally, integrating these new materials into additive processes can enable selective use of the material in high load or stress areas. It is noteworthy that past work in this field of fiber reinforced cement composites did not consider the optimization of fiber-matrix interface using suitable sizing. Carbon fiber reinforcement offers potential added benefits of thermal conductivity (which affects cure rate) and flow behavior that could provide opportunities for site specific utilization of carbon fiber on hybrid cement structures (e.g. use the fiber reinforcement on outer surfaces to enhance strength and modulus and then infiltrating the internal structures with conventional concrete). MonteFibre was the industry lead and planned on supplying the tCF for this project. However, during the short Phase-1 duration of this project, MonteFibre was unable to produce tCF for this project due to manufacturing plant being off-line throughout the course of the project. The project team decided to pursue an alternate option which involved demonstrating printable concrete with steel fibers by the ORNL lead, Dr. Brian Post. The University of Tennessee collaboration team focused on evaluating the suitable chemical sizing for carbon fibers working with Michelman and also developed methods for material characterization of cement-based composites to evaluate the material response for compression, shear, flexure, and tension. The two milestones for University of Tennessee, Knoxville were realized related to identification of one sizing suitable for carbon fiber reinforced cement composite and developing data associated with mechanical behavior of unreinforced (neat) and carbon fiber reinforced cement composites. ORNL could not complete the task of carbon fiber reinforced printed cement composites due to the reasons mentioned earlier, but was able to replace tCF with steel fibers to demonstrate the feasibility of printing with fiber reinforced cement composites. The Project team reviewed possible sizing chemistry available in collaboration with Michelman for use on carbon fiber reinforcement in cement composites and concrete applications. Our initial goal was to identify a sizing most promising for formulation with textile carbon fibers (tCF) to deliver excellent mechanical properties in composite material state. Since tCF was not available for this project as originally envisioned, the team continued this task to identify a suitable sizing for carbon fiber applications by applying such sizing to lower cost carbon fibers currently available commercially from Zoltek called Panex fibers. At a future time this can be optimized for textile carbon fibers from Montefibre. The bulk of previous work on carbon fiber reinforced cement has neglected the importance of fiber-matrix adhesion on mechanical properties of the cement composite and identifying this missing link was an important accomplishment for future research. Tensile behavior of fiber reinforced concrete is important to evaluate in order to realize the dream of concrete products that do not need reinforcing steel. Important sample preparation and testing procedures were addressed in this study and it was concluded that substantial improvements in tensile behavior, without compromising compressive strength, and improved ductility can result from the use of carbon fiber reinforcement.

36 MATERIALS SCIENCE↗

NASA NTRS1999

Method of Fabricating Chopped-Fiber Composite Piston

A three-dimensional piston molding is fabricated from a mixture of chopped, carbon tow filaments of variable length, which are prepregged with carbonaceous organic resins and/or pitches and molded by conventional molding processes into a near net shape, to form a carbon-fiber reinforced organic-matrix composite part. Continuous reinforcement in the form of carbon-carbon composite tapes or pieces of fabric can be also laid in the mold before or during the charging of the mold with the chopped-fiber mixture, to enhance the strength in the crown and wrist-pin areas. The molded chopped-fiber reinforced organic-matrix composite parts are then pyrolized in an inert atmosphere, to convert the organic matrix materials to carbon. These pyrolized parts are then densified by reimpregnation with resins or pitches, which are subsequently carbonized. Densification is also accomplished by direct infiltration with carbon by vapor deposition processes. Once the desired density has been achieved, the piston molds are machined to final piston dimensions, and piston ring grooves are added. To prevent oxidation and/or to seal the piston surface or near surface, the chopped-fiber piston is coated with ceramic and/or metallic sealants: and/or coated with a catalyst.

Rivers, H. Kevin↗

NASA NTRS2007

Formation and Growth of Micro and Macro Bubbles on Copper-Graphite Composite Surfaces

Micro scale boiling behavior in the vicinity of graphite micro-fiber tips on the coppergraphite composite boiling surfaces is investigated. It is discovered that a large number of micro bubbles are formed first at the micro scratches and cavities on the copper matrix in pool boiling. In virtue of the non-wetting property of graphite, once the growing micro bubbles touch the graphite tips, the micro bubbles are sucked by the tips and merged into larger micro bubbles sitting on the tips. The micro bubbles grow rapidly and coalesce to form macro bubbles, each of which sitting on several tips. The growth processes of the micro and macro bubbles are analyzed and formulated followed by an analysis of bubble departure on the composite surfaces. Based on these analyses, the enhancement mechanism of the pool boiling heat transfer on the composite surfaces is clearly revealed. Experimental results of pool boiling heat transfer both for water and Freon-113 on the composite surfaces convincingly demonstrate the enhancement effects of the unique structure of Cu-Gr composite surfaces on boiling heat transfer.

Chao, David F.↗

DOE OSTI2023

Next Generation Fiber-Encapsulated Nanoscale Hybrid Materials for Direct Air Capture with Selective Water Rejection

Recently, NOHMs sorbents have been demonstrated to be highly stable and tunable for CO2 capture and have negligible vapor pressure, but their main drawbacks are high viscosity and high gas transfer limitation in their neat bulk phase. This project explored gas-assisted electrospinning processing coupled with promising encapsulation matrices such as Polymers with Intrinsic Microporosity (PIM-1) and polyacrylonitrile (PAN)/organopolysilizane (OPSZ) polymer/ceramic hybrid materials, which were demonstrated to be effective novel carriers for the active NOHMs sorbents. These encapsulation materials were evaluated by their thermal stability, hydrophobicity, permeability, and CO2 selectivity. The manufacturing parameters such as component composition and processing solvent were linked to bulk sorbent properties, e.g., surface area, pore volume, fiber thickness, capture capacity, capture kinetics, etc. These investigations resulted in fundamental knowledge and technical know-how that will be useful for scaling up the nanofiber mat contactor design. The encapsulation materials and design has been shown to not only increase the thermal oxidative stability of the NOHMs, but also yield significantly reduced pressure drop and increased performance of large modular air filters. 70 PAN: 30 OPSZ/NIPEI fibers exhibited the highest capture performance with 1.5 mmol CO2/g∙h kinetics the first hour under 100% CO2 condition, followed by 80 PAN: 20 OPSZ/NIPEI and 90 PAN: 10 OPSZ/NIPEI, while 90 PAN: 10 OPSZ/NIPEI fibers performed the best with 0.25 mmol CO2/g∙h of the initial kinetics under 400 ppm CO2 concentration. All the fabricated fibers demonstrated stable capture performances up to 15 cycles of adsorption and desorption. Using encapsulated NOHMs, the study found that the microwave could help regenerate the capture materials within 20 minutes without chemically degrading the materials. A high-level TEA/LCA study was performed to evaluate the feasibility of this technology at scale. These estimates show that the sorbent cost and environmental impact levels are comparable to other existing technologies. Overall, these findings increase the technological feasibility of using liquid-like, low vapor pressure NOHMs as a next generation sorbent for the direct air capture of CO2.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1981

Benzoic acid degradation of polyacrylonitrile fibers

The reactions of polyacrylonitrile (PAN) fibers in the presence of benzoic acid have been studied. Polyacrylonitrile fibers oxidize more readily in the presence of benzoic acid than in air at temperatures in the range of 170 C. The product decreased in solubility with extent of reaction. Gel permeation chromatography of the soluble fraction showed change in polydispersity. The insoluble product exhibited differences in weight loss as a function of decomposition temperature compared to PAN fibers. Infrared analyses of the fiber product showed absorption peaks similar to air-oxidized PAN. High-energy photoelectron spectral analysis showed a carbon-rich surface which contained oxygen and nitrogen. An air oxidized sample of fiber contained more oxygen at the surface than a fiber treated first with benzoic acid and then air oxidized.

Varma, D. S.↗

NASA NTRS1981

Benzoic acid degradation of polyacrylonitrile fibers

Varma, D. S.↗

NASA NTRS1997

Experimental Characterization and Micromechanical Modeling of Woven Carbon/Copper Composites

The results of an extensive experimental characterization and a preliminary analytical modeling effort for the elastoplastic mechanical behavior of 8-harness satin weave carbon/copper (C/Cu) composites are presented. Previous experimental and modeling investigations of woven composites are discussed, as is the evolution of, and motivation for, the continuing research on C/Cu composites. Experimental results of monotonic and cyclic tension, compression, and Iosipescu shear tests, and combined tension-compression tests, are presented. With regard to the test results, emphasis is placed on the effect of strain gauge size and placement, the effect of alloying the copper matrix to improve fiber-matrix bonding, yield surface characterization, and failure mechanisms. The analytical methodology used in this investigation consists of an extension of the three-dimensional generalized method of cells (GMC-3D) micromechanics model, developed by Aboudi (1994), to include inhomogeneity and plasticity effects on the subcell level. The extension of the model allows prediction of the elastoplastic mechanical response of woven composites, as represented by a true repeating unit cell for the woven composite. The model is used to examine the effects of refining the representative geometry of the composite, altering the composite overall fiber volume fraction, changing the size and placement of the strain gauge with respect to the composite's reinforcement weave, and including porosity within the infiltrated fiber yarns on the in-plane elastoplastic tensile, compressive, and shear response of 8-harness satin C/Cu. The model predictions are also compared with the appropriate monotonic experimental results.

Bednarcyk, Brett A.↗

NASA NTRS2003

Thermomechanical Properties of Interface Modified M40J Carbon/PMR-II-50 Composites

To increase performance and durability of high-temperature composites for potential rocket engine components, it is necessary to optimize wetting and interfacial bonding between high modulus carbon fibers and high-temperature polyimide resins. It has been previously demonstrated that the electro-oxidative shear treatments used by fiber manufacturers are not effective on higher modulus fibers that have fewer edge and defect sites in the surface crystallites. In addition, sizings commercially supplied on most carbon fibers are not compatible with polyimides. In this study, the surface chemistry and energy of high modulus carbon fibers (M40J and M60J, Torray) and typical fluorinated polyimide resins, such as PMR-11-50 were characterized. A continuous desizing system that uses an environmentally friendly chemical- mechanical process was developed for tow level fiber. Composites were fabricated with fibers containing the manufacturer's sizing, desized, and further treated with a reactive finish. Results of room temperature tests show that desizing reduces interface sensitive properties compared to the manufacturer's sizing and that subsequent surface re-treatment with reactive finish increases interface sensitive properties. Properties of thermally aged composites and composites with varying finish concentrations will also be discussed.

Allred, Ronald E.↗

NASA NTRS2003

Thermomechanical Properties of M40J Carbon/PMR-II-50 Composites

To increase performance and durability of high-temperature composites for potential rocket engine components, it is necessary to optimize wetting and interfacial bonding between high modulus carbon fibers and high-temperature polyimide resins. It has been previously demonstrated that the electro-oxidative shear treatments used by fiber manufacturers are not effective on higher modulus fibers that have fewer edge and defect sites in the surface crystallites. In addition, sizings commercially supplies on most carbon fibers are not compatible with polyimides. In this study, the surface chemistry and energy of high modulus carbon fibers (M40J and M60J, Torray) and typical fluorinated polyimide resins, such as PMR-II-50 were characterized. A continuous desizing system that uses an environmentally friendly chemical-mechanical process was developed for tow level fiber. Composites were fabricated with fibers containing the manufacturer's sizing, desized, and further treated with a reactive finish. Results of room temperature tests show that desizing reduces interface sensitive properties compared to the manufacturer's sizing and that subsequent surface re-treatment with reactive finish increases interface sensitive properties. Properties of thermally aged composites and composites with varying finish concentrations are also discussed.

Ronald E. Allred↗

NASA NTRS2006

Micromechanics Modeling of Functionally Graded Interphase Regions in Carbon Nanotube-Polymer Composites

The effective elastic properties of a unidirectional carbon fiber/epoxy lamina in which the carbon fibers are coated with single-walled carbon nanotubes are modeled herein through the use of a multi-scale method involving the molecular dynamics/equivalent continuum and micromechanics methods. The specific lamina representative volume element studied consists of a carbon fiber surrounded by a region of epoxy containing a radially varying concentration of carbon nanotubes which is then embedded in the pure epoxy matrix. The variable concentration of carbon nanotubes surrounding the carbon fiber results in a functionally graded interphase region as the properties of the interphase region vary according to the carbon nanotube volume fraction. Molecular dynamics and equivalent continuum methods are used to assess the local effective properties of the carbon nanotube/epoxy comprising the interphase region. Micromechanics in the form of the Mori-Tanaka method are then applied to obtain the global effective properties of the graded interphase region wherein the carbon nanotubes are randomly oriented. Finally, the multi-layer composite cylinders micromechanics approach is used to obtain the effective lamina properties from the lamina representative volume element. It was found that even very small quantities of carbon nanotubes (0.36% of lamina by volume) coating the surface of the carbon fibers in the lamina can have a significant effect (8% increase) on the transverse properties of the lamina (E22, k23, G23 and G12) with almost no affect on the lamina properties in the fiber direction (E11 and v12).

Seidel, Gary D.↗

NASA NTRS1977

Mechanical behavior and fracture characteristics of off-axis fiber composites. 1: Experimental investigation

The mechanical behavior, fracture surfaces, and fracture modes of unidirectional high-modulus graphite-fiber/epoxy composites subjected to off-axis tensile loads were investigated experimentally. The investigation included the generation of stress-strain-to-fracture data and scanning electron microscope studies of the fractured surfaces. The results led to the identification of fracture modes and distinct fracture surface characteristics for off-axis tensile loading. The results also led to the formulation of critical for identifying and characterizing these fracture modes and their associated fracture surfaces. The results presented and discussed herein were used in the theoretical investigation and comparisons described in Part 2. These results should also provide a good foundation for identifying, characterizing, and quantifying fracture modes in both off-axis and angle-plied laminates.

Sinclair, J. H.↗

NASA NTRS2004

Advanced SiC/SiC Ceramic Composites For Gas-Turbine Engine Components

NASA Glenn Research Center (GRC) is developing a variety of advanced SiC/SiC ceramic composite (ASC) systems that allow these materials to operate for hundreds of hours under stress in air at temperatures approaching 2700 F. These SiC/SiC composite systems are lightweight (approximately 30% metal density) and, in comparison to monolithic ceramics and carbon fiber-reinforced ceramic composites, are able to reliably retain their structural properties for long times under aggressive gas-turbine engine environments. The key for the ASC systems is related first to the NASA development of the Sylramic-iBN Sic fiber, which displays higher thermal stability than any other SiC- based ceramic fibers and possesses an in-situ grown BN surface layer for higher environmental durability. This fiber is simply derived from Sylramic Sic fiber type that is currently produced at ATK COI Ceramics (COIC). Further capability is then derived by using chemical vapor infiltration (CVI) and/or polymer infiltration and pyrolysis (PIP) to form a Sic-based matrix with high creep and rupture resistance as well as high thermal conductivity. The objectives of this study were (1) to optimize the constituents and processing parameters for a Sylramic-iBN fiber reinforced ceramic composite system in which the Sic-based matrix is formed at COIC almost entirely by PIP (full PIP approach), (2) to evaluate the properties of this system in comparison to other 2700 F Sylramic-iBN systems in which the matrix is formed by full CVI and CVI + PIP, and (3) to examine the pros and cons of the full PIP approach for fabricating hot-section engine components. A key goal is the development of a composite system with low porosity, thereby providing high modulus, high matrix cracking strength, high interlaminar strength, and high thermal conductivity, a major property requirement for engine components that will experience high thermal gradients during service. Other key composite property goals are demonstration at high temperatures of high environmental resistance and high creep resistance, which in turn will result in long component life. Data are presented from a variety of laboratory tests on simple two-dimensional panels that examine these properties and compare the performance of the optimized full PIP system with those of the full CVI and CVI + PIP hybrid systems. Underlying mechanisms for performance differences in the various systems are discussed. Remaining issues for further property enhancement and for application of the full PIP approach for engine components are also discussed, as well as on-going approaches at NASA to solve these issues.

H. M. Yun↗

DOE OSTI2024

Simultaneous measurement of temperature and strain by cascaded fiber Bragg grating-silicon Fabry-Perot interferometer sensor

We report a fiber-optic sensor configuration with a cascaded fiber Bragg grating (FBG) and a silicon Fabry-Perot interferometer (FPI) for simultaneous measurement of temperature and strain. The sensor is composed of a 5 mm FBG on a single mode fiber and a 100μm thick silicon FPI attached to the tip of the optical fiber. The FBG is surface mounted on the host structure, and the FPI tip is suspended. Due to the stress-free, cantilever configuration, the silicon FPI is insensitive to strain, but sensitive to temperature with a sensitivity much higher than the FBG due to the large thermo-optic coefficient of silicon. The sensor is tested from room temperature to 100°C with varying strain up to ∼150με. The silicon FPI provides high temperature sensitivity of 89 pm/°C unaffected by strain. Since the FBG is attached to the host structure, it is affected by both thermal and mechanical strain; the sensitivity of these was experimentally obtained 32 pm/°C and 1.09 pm / με, respectively. Interrogated with a broadband light source and a high-speed spectrometer, the sensor shows temperature and strain resolutions of 1.9 × 10 −3 °C and 0.042 με, respectively. Here, due to the small size, enhanced sensitivity, and high resolution, this cascaded FBG-FPI sensor can be used in applications where accurate measurement of temperature and strain is required.

42 ENGINEERING↗

DOE OSTI2022

Fiber-optic sensor packaging assessment and benchmarking for embedded sensing applications

Fiber optic-based sensing for non-destructive evaluation (NDE) and structural health monitoring of various infrastructure and energy assets is an increasingly important sensing scheme. Because of their immunity to electromagnetic interferences, versatility in sensing mechanisms and designs as well as capability for distributed sensing, the fiber optic sensing is of great interest for embedding within infrastructures using advanced manufacturing methods. However, the protection of fiber optic sensors during advanced manufacturing-based embedding is an important aspect for infrastructure monitoring in practice. While successful installation of fiber optic sensors has been accomplished through application of epoxy or adhesives on infrastructure surfaces, there has been only limited investigation of fiber protection packaging schemes which are compatible with in-situ repair techniques such as the metallic cold-spray. With increasing interest and importance of cold spray-based repair processes, the integration of fiber optic sensors simultaneously during the repair is equally important. In this work, we focus our efforts on investigating various types of packaging schemes for their compatibility and integrability on the surfaces of metallic structures such as oil and gas pipelines during an in-situ repair coating. First, we consider sandblasting using silica sand particles of various size for optical fibers on the surface of a metallic coupon as a useful proxy test of sensor packaging stability. Structural damage of packaging is characterized by means of optical microscopy and the optical integrity of embedded fiber optic cables is examined using optical backscatter reflectometry (OBR). In addition, initial investigation of metallic cold-spray embedded fiber optic cables under various packaging on metallic substrates is also considered with early conclusions and future directions.

Fiber-optic sensors, Sensors packaging, Metallic C↗

NASA NTRS1979

Fatigue behavior of SiC reinforced titanium composites

The low cycle axial fatigue properties of 25 and 44 fiber volume percent SiC/Ti(6Al-4V) composites were measured at room temperature and at 650 C. At room temperature, the S-N curves for the composites showed no anticipated improvement over bulk matrix behavior. Although axial and transverse tensile strength results suggest a degradation in SiC fiber strength during composite fabrication, it appears that the poor fatigue life of the composites was caused by a reduced fatigue resistance of the reinforced Ti(6Al-4V) matrix. Microstructural studies indicate that the reduced matrix behavior was due, in part, to the presence of flawed and fractured fibers created near the specimen surfaces by preparation techniques. Another possible contributing factor is the large residual tensile stresses that can exist in fiber-reinforced matrices. These effects, as well as the effects of fatigue testing at high temperature, are discussed.

Bhatt, R. T.↗

NASA NTRS1991

A comparison of experimental observations and numerical predictions for the initiation of fiber microbuckling in notched composite laminates

The results of the present experimental study of fiber microbuckling indicates that free surfaces, ply orientations, and resin-rich regions affect the strain level for the initiation of in-plane fiber microbuckling. Nonlinear matrix constitutive behavior, in conjunction with initial fiber waviness, cause significant reductions of fiber microbuckling initiation strain level; these two factors generate nonlinear global stress-strain responses in the models. The fiber microbuckling initiation strains correlate well with the applied strain associated with asymptotic local shear strains.

Guynn, E. G.↗

NASA NTRS2006

Investigation of Post-Flight Solid Rocket Booster Thermal Protection System

After every Shuttle mission, the Solid Rocket Boosters (SRBs) are recovered and observed for missing material. Most of the SRB is covered with a cork-based thermal protection material (MCC-l). After the most recent shuttle mission, STS-114, the forward section of the booster appeared to have been impacted during flight. The darkened fracture surfaces indicated that this might have occurred early in flight. The scope of the analysis included microscopic observations to assess the degree of heat effects and locate evidence of the impact source as well as chemical analysis of the fracture surfaces and recovered foreign material using Fourier Transform Infrared Spectroscopy and Scanning Electron Microscopy/Energy Dispersive Spectroscopy. The amount of heat effects and presence of soot products on the fracture surface indicated that the material was impacted prior to SRB re-entry into the atmosphere. Fragments of graphite fibers found on these fracture surfaces were traced to slag inside the Solid Rocket Motor (SRM) that forms during flight as the propellant is spent and is ejected throughout the descent of the SRB after separation. The direction of the impact mark matches with the likely trajectory of SRBs tumbling prior to re-entry.

Nelson, Linda A.↗