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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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Studies of fiber-matrix adhesion on compression strength

A study was initiated on the effect of the matrix polymer and the fiber matrix bond strength of carbon fiber polymer matrix composites. The work includes tests with micro-composites, single ply composites, laminates, and multi-axial loaded cylinders. The results obtained thus far indicate that weak fiber-matrix adhesion dramatically reduces 0 degree compression strength. Evidence is also presented that the flaws in the carbon fiber that govern compression strength differ from those that determine fiber tensile strength. Examination of post-failure damage in the single ply tests indicates kink banding at the crack tip.

Bascom, Willard D.↗

Characterization of carbon fibers and fiber-matrix adhesion in composites

The effect of fiber/matrix interactions on the mechanical properties of thermoplastic carbon fiber composites was determined. The experimental approach was a multi-faceted one involving the following areas: characterization of the surface of carbon fibers using X-ray photoelectron spectroscopy (XPS), secondary ion mass spectroscopy (SIMS) and scanning transmission electron microcopy (STEM); determination of the functional groups on carbon fiber surfaces using an elemental tagging scheme - derivatization; determination of the polar and dispersion contribution to the surface energy of carbon fibers by measuring wetting forces in a series of liquids having known polar and dispersion components; and study of the interaction of thermoplastic polymers with carbon surfaces by solution adsorption, STEM and fiber critical length.

Wightman, J. P.↗

Enhancing Composite Toughness Through Hierarchical Interphase Formation

High strength and ductility are highly desired in fiber-reinforced composites, yet achieving both simultaneously remains elusive. A hierarchical architecture is developed utilizing high aspect ratio chemically transformable thermoplastic nanofibers that form covalent bonding with the matrix to toughen the fiber-matrix interphase. The nanoscale fibers are electrospun on the micrometer-scale reinforcing carbon fiber, creating a physically intertwined, randomly oriented scaffold. Unlike conventional covalent bonding of matrix molecules with reinforcing fibers, here, the nanofiber scaffold is utilized - interacting non-covalently with core fiber but bridging covalently with polymer matrix - to create a high volume fraction of immobilized matrix or interphase around core reinforcing elements. This mechanism enables efficient fiber-matrix stress transfer and enhances composite toughness. Molecular dynamics simulation reveals enhancement of the fiber-matrix adhesion facilitated by nanofiber-aided hierarchical bonding with the matrix. The elastic modulus contours of interphase regions obtained from atomic force microscopy clearly indicate the formation of stiffer interphase. These nanoengineered composites exhibit a ≈60% and ≈100% improved in-plane shear strength and toughness, respectively. This approach opens a new avenue for manufacturing toughened high-performance composites.

36 MATERIALS SCIENCE↗

Effects of mercerization and fiber sizing of coir fiber for utilization in polypropylene composites

The use of natural fibers as an alternative to synthetic fibers for reinforcing composites is increasing. However, the poor interfacial adhesion between natural fibers and polymer matrices limits their applications. Several approaches have been considered to improve fiber-matrix adhesion via chemical and/or physical treatment. However, the effectiveness of these treatments varies based on the type of fiber, its source, and its composition. Thus, it is imperative to understand the effectiveness of treatment conditions. In this study, we investigated the influence of alkali treatment and fiber sizing on the chemical, thermal, morphological, and mechanical properties of coir fibers and the interface between coir fiber and polypropylene matrix. Further, it was found that using a 5 wt% sodium hydroxide solution for 6 h at room temperature was the optimal treatment condition that led to an improvement in tensile strength by 58%, tensile modulus by 71%, and elongation at break by 37% compared to untreated fibers, and an increment in interfacial shear strength (IFSS) between coir fibers and polypropylene matrix by 32%. The alkali treatment removed the fiber surface impurities, made the fiber surface rough, and enhanced the fiber crystallinity. Sizing of the alkali-treated fiber led to an improvement in IFSS by 87% with no modification of the fiber’s mechanical properties.

36 MATERIALS SCIENCE↗

TuFF internal WRAP for Rapid Pipeline Repair (TuFF iWRAP)

The goal of “TuFF internal WRAP for Rapid Pipeline Repair” (TuFF iWRAP) program was to develop a novel material system and placement process to fabricate structural pipe within the existing deteriorated pipelines without disruption of gas delivery. The team (University of Delaware – Center for Composite Materials (UD-CCM) and Plitzie Inc.) addressed this challenge by developing a new material feedstock and pipe in pipe (PIP) repair strategy. This allows the potential for significant cost reduction and has minimum operational impact on gas customers. The new robotic based placement design allows discontinuous placement of pipe sections creating a stand-alone structural liner within the legacy pipeline without the need for pipe shutdown. Here, the material is supplied using a tethered material feeding system and is placed and UV cured with the internal Wound Rapid Automated Placement (iWRAP) system. This provides maximum placement efficiency capable of traversing 90 angle bends in 12-inch pipe and overall design customization to meet pipe repair requirements (e.g., variable wall thickness, bridging gaps, etc.). UV-curable fiber reinforced composite material has been optimized to meet structural performance and placement/cure times. Superior strength and fatigue life has been demonstrated by improving fiber-matrix adhesion using new fiber sizing for UV resins. Rapid cure approaches using new liner and resins have been evaluated with industry. The appropriate design of the section joints has been developed and tested. We estimate coating time to be ~100 hours per mile enabling typical pipe repair within 1 week.

03 NATURAL GAS↗

Some features of the fabrication of multilayer fiber composites by explosive welding

The fabrication of multilayer fiber composites by explosive welding is characterized by intense plastic deformation of the matrix material as it fills the spaces between fibers and by high velocity of the collision between matrix layers due to acceleration in the channels between fibers. The plastic deformation of the matrix layers and fiber-matrix friction provide mechanical and thermal activation of the contact surfaces, which contributes to the formation of a bond. An important feature of the process is that the fiber-matrix adhesion strength can be varied over a wide range by varying the parameters of impulsive loading.

Kotov, V. A.↗

Differences in interfacial bond strengths of graphite fiber-epoxy resin composites

The effect of epoxy-size and degree of cure on the interfacial bonding of an epoxy-amine-graphite fiber composite system is examined. The role of the fiber-resin interface in determining the overall mechanical properties of composites is poorly understood. A good interfacial adhesive bond is required to achieve maximum stress transfer to the fibers in composites, but at the same time some form of energy absorbing interfacial interaction is needed to achieve high fracture toughening. The incompatibility of these two processes makes it important to understand the nature and basic factors involved at the fiber-resin interface as stress is applied. The mechanical properties including interlaminar shear values for graphite fiber-resin composites are low compared to glass and boron-resin composites. These differences have been attributed to poor fiber-matrix adhesion. Graphite fibers are commonly subjected to post-treatments including application of organic sizing in order to improve their compatibility with the resin matrix and to protect the fiber tow from damage during processing and lay-up. In such processes, sized graphite fiber tow is impregnated with epoxy resin and then layed-up i nto the appropriate configuration. Following an extended ambient temperature cure, the graphite-resin composite structure is cured at elevated temperature using a programmed temperature sequence to cure and then cool the product.

Needles, H. L.↗

Interface effects in interlaminar fracture of thermoplastic composites

Mode I interlaminar fracture toughness was determined on a series of unidirectional poly(phenylene oxide)/carbon fiber composites using the double cantilever beam test. Initial toughness for growth of a delamination from an insert depends on fiber type, and ranges from 190 to 440 J/sq m, with intermediate modulus fibers tending to give lower values than high-strain fibers. Low toughness values are attributed to poor fiber-matrix adhesion. As a delamination progress down the beam, fiber bridging increases the apparent toughness by up to a factor of 7, depending on the fiber.

Hinkley, J. A.↗

Flexure Test For Off-Axis Unidirectional Composites

Improved flexure test yields data on ply strength of off-axis unidirectional composite material. Rotatable end supports allow ends of specimen to twist freely. End supports apply only vertical loads, making simple three-point bending test. Ply-strength data provide basis for predicting onset of damage in composite structures and serve as measure of fiber-matrix adhesion.

Crews, John H., Jr.↗

The Effects of Fiber Surface Modification and Thermal Aging on Composite Toughness and Its Measurement

A detailed experimental study was conducted to establish the structure-property relationships between elevated temperature aging and fiber-matrix bonding, Mode 2 interlaminar fracture toughness, and failure modes of carbon fiber/PMR-15 composites. The fiber-matrix adhesion was varied by using carbon fibers with different surface treatments. Short beam shear tests were used to quantify the interfacial shear strength afforded by the use of the different fiber surface treatments. The results of the short beam shear tests showed that, for times up to 1000 hr, the aging process caused no changes in the bulk of the three composite materials that would degrade the shear properties of the material. Comparisons between the interlaminar shear strengths (ILSS) measured by the short beam shear tests and the GIIC test results, as measured by the ENF test, indicated that the differences in the surface treatments significantly affected the fracture properties while the effect of the aging process was probably limited to changes at the starter crack tip. The fracture properties changed due to a shift in the fracture from an interfacial failure to a failure within the matrix when the fiber was changed from AU-4 to AS-4 or AS-4G. There appears to be an effect of the fiber/matrix bonding on the thermo-oxidative stability of the composites that were tested. The low bonding afforded by the AU 1 fiber resulted in weight losses about twice those experienced by the AS 1 reinforced composites, the ones with the best TOS.

Bowles, Kenneth J.↗

The Effects of Fiber Surface Modification and Thermal Aging on Composite Toughness And its Measurement

A detailed experimental study was conducted to establish the structure-property relationships between elevated temperature aging and (I) fiber-matrix bonding, (2) Mode II interlaminar fracture toughness, and (3) failure modes of carbon fiber/PMR-15 composites. The fiber-matrix adhesion was varied by using carbon fibers with different surface treatments. Short beam shear tests were used to quantify the interfacial shear strength afforded by the use of the different fiber surface treatments. The results of the short beam shear tests definitely showed that, for aging times up to 1000 hr, the aging process caused no observable changes in the bulk of the three composite materials that---would degrade the shear properties of the material. Comparisons between the interlaminar shear strength (ILSS) measured by the short beam shear tests and the GII c test results, as measured by the ENF test, indicated that the differences in the surface treatments significantly affected the fracture properties while the effect of the aging process was probably limited to changes at the starter crack tip. The fracture properties changed due to a shift in the fracture from an interfacial failure to a failure within the matrix when the fiber was changed from AU-4 to AS-4 or AS-4G. There appears to be an effect of the fiber/matrix bonding on the thermo-oxidative stability of the composites that were tested. The low bonding afforded by the AU-4 fiber resulted in weight losses about twice those experienced by the AS-4 reinforced composites, the ones with the best TOS.

Bowles, Kenneth J.↗

Surface analysis in composite bonding

The role of the interfacial region in determining the bond strength and durability of composite bonds is discussed. The characterization of a variety of carbon fibers including Celion 6000 using both scanning electron microscopy and X-ray photoelectron spectroscopy is discussed. The emphasis is on composite bonding, that is, the adhesive bonding between composites in contrast to fiber-matrix interaction. The primary objective of the research is the characterization of composite surfaces before adhesive bonding and after fracture of bonded specimens. Work done on the analysis of composite samples pretreated in a number of ways prior to bonding is detailed.

Messick, D. L.↗

Designing Physicochemically‐Ordered Interphases for High‐Performance Composites

To enhance the mechanical properties of carbon fiber‐reinforced polymer composites, a physicochemical scaffold is designed incorporating microscopically architected chemically reactive nanofibers that act as a multiscale bridge between the carbon fibers and the matrix. Thermally activated nanofibers leverage their morphologically driven mechanochemical properties to form covalent bonds with adjacent polymer molecules, creating a co‐continuous network that dramatically enhances fiber‐matrix load transfer. By meticulously controlling the nanofiber architecture through variable surface area, functional group availability, and polymer chain alignment effects, the extent of covalent bonding between nanofibers and the matrix is manipulated ultimately resulting in improved carbon fiber‐matrix adhesion. Further, the concept was validated using polyacrylonitrile nanofibers within an acrylonitrile butadiene styrene matrix in a discontinuous carbon fiber‐reinforced composite system. Nanomechanical studies using atomic force microscopy and low‐field nuclear magnetic resonance spectroscopy confirmed immobilized, chemically transferred, and ordered nanostructures at the interphase. The resulting composites demonstrated ≈56% and ≈175% improvements in tensile strength and toughness, respectively, compared to composites without nanofiber. Comprehensive thermal, rheological, and X‐ray scattering analyses, along side all‐atomic molecular dynamics simulations, revealed the fundamental mechanisms behind these improvements in mechanical behavior. The versatility and efficacy of the approach have the potential to address longstanding interphase challenges in the composite industry.

36 MATERIALS SCIENCE↗

Low-Cost, High-Performance Carbon Fiber for Compressed Natural Gas Storage Tanks (Final Technical Report – Down Select Report)

The aim of this project is to reduce the cost of Type IV, carbon fiber (CF) composite overwrap compressed gas storage tanks by reducing the cost of CF and CF composites. The project team worked to reduce the cost of CF by exploring and testing opportunities for a low-cost alternative precursor material for CF production to supplant market-dominant and costly polyacrylonitrile (PAN). Concurrently, the team aimed to reduce the cost of the tanks at the composite level by improving the interfacial adhesion between the fibers and the matrix resin through the incorporation of low-cost nanoparticles recycled from waste materials, which would reduce the volume of costly CF required to achieve the same tank performance. At the end of the first year, the project team selected mesophase pitch as the primary precursor candidate from a field of materials based on the superior mechanical performance and cost-saving potential. During the second year, the team produced CFs derived from mesophase pitch achieving an average tensile strength of 365.6 ksi and average tensile modulus of 40.74 Msi. Facility availability for spinning and converting these fibers at greater scale has hindered scale-up demonstration, but the team has identified opportunities to conduct this work in the near term. Cost modeling shows that these mesophase pitch-derived CFs can be up to 40% less expensive than PAN-derived CFs due to the lower cost of the feedstock material, higher throughput, greater conversion yield, and lower cost spinning method and compared to PAN. Additionally, the team has demonstrated at lab-scale that nanoparticle coating CFs can significantly increase the interfacial shear strength and load transfer efficiency of CFs in a matrix. Single filament pull-out testing showed a 27% average increase in max interfacial shear strength due to this coating. A continuous method of applying these coatings to a tow of CF has been developed for scale-up. 26 m tows of coated CFs were produced using this system and formed into composite ring samples for ASTM ring burst testing. Issues with the testing protocol have limited assessment of these results. A prototype Type IV tank was designed to meet ANSI HGV2 standards, and the design criteria set out by DOE, using the CF properties developed by the team paired with a proprietary resin matrix, a polyamide liner, and aluminum end bosses. The tank weighs 153.1 kg and with a total capacity of 5.8 kg H2 (5.6 kg usable), which yields a gravimetric capacity of 1.17 kWh/kg. Cost modeling predicts that the tank will have a projected cost of $15.73/kWh. Tank performance modeling does not include considerations for fiber-matrix load transfer efficiency improvements offered by nanoparticle coating method.

08 HYDROGEN↗